data_10_18srv286
_audit_creation_date 2018-07-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number '2017/1'
loop_
_audit_author_name
_audit_author_email
_audit_author_address
'Yufit, D.' d.s.yufit@durham.ac.uk
;
Durham University
Chemistry
South Rd.
Durham
DH1 3LE
UK
;
_publ_requested_journal 'Nature'
_publ_section_title
;
Rupturing Aromaticity by Periphery Overcrowding
;
_publ_contact_author_name 'Dmitry Yufit'
_publ_contact_author_address
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
_publ_contact_author_email 'd.s.yufit@durham.ac.uk'
_publ_contact_letter
;
The CIF file contains data for the structure 10 from
the paper
"Rupturing Aromaticity by Periphery Overcrowding"
by P.Saha, A.Mallick, A.T.Turley, A.N. Bismillah, A.Danos, A.P.Monkman,
A-J Avestro, D.S.Yufit and P.R.McGonigal
The paper will be submitted to Nature shortly.
;
loop_
_publ_author_name
_publ_author_address
'Saha, Promeet'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Mallick, Abhijit'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Turley, Andrew T.'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Bismillah, Aisha N.'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Danos, Andrew'
;
Department of Physics
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Monkman, Andrew P.'
;
Department of Physics
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'Avestro, Alyssa-Jennifer'
;
Department of Chemistry
University of York
Heslington
York
YO10 5DD
UK
;
'Yufit, Dmitry S.'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
'McGonigal, Paul R.'
;
Department of Chemistry
Durham University
South Rd.
Durham
DH1 3LE
UK
;
_publ_section_references
;
Dolomanov, O. V., Bourhis, L. J., Gildea, R. J., Howard, J. A. K. & Puschmann,
H. (2009). J. Appl. Cryst. 42, 339--341.
Sheldrick, G. M. (2008). Acta Cryst. A64, 112--122.
Sheldrick, G. M. (2015). Acta Cryst. C71, 3--8.
;
_chemical_name_common ?
_chemical_name_systematic ?
_chemical_formula_moiety 'C43 H28 O'
_chemical_formula_sum 'C43 H28 O'
_chemical_formula_weight 560.65
_chemical_melting_point ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system triclinic
_space_group_IT_number 2
_space_group_name_H-M_alt 'P -1'
_space_group_name_Hall '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 9.3113(6)
_cell_length_b 10.5095(7)
_cell_length_c 16.2093(10)
_cell_angle_alpha 84.875(3)
_cell_angle_beta 80.864(3)
_cell_angle_gamma 75.921(3)
_cell_volume 1516.90(17)
_cell_formula_units_Z 2
_cell_measurement_reflns_used 6168
_cell_measurement_temperature 120.0
_cell_measurement_theta_max 29.08
_cell_measurement_theta_min 2.31
_shelx_estimated_absorpt_T_max 0.996
_shelx_estimated_absorpt_T_min 0.986
_exptl_absorpt_coefficient_mu 0.072
_exptl_absorpt_correction_T_max 1.0000
_exptl_absorpt_correction_T_min 0.8357
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0791 before and 0.0456 after correction.
The Ratio of minimum to maximum transmission is 0.8357.
The \l/2 correction factor is Not present.
;
_exptl_absorpt_special_details ?
_exptl_crystal_colour 'clear colourless'
_exptl_crystal_colour_lustre clear
_exptl_crystal_colour_primary colourless
_exptl_crystal_density_diffrn 1.227
_exptl_crystal_density_meas ?
_exptl_crystal_density_method ?
_exptl_crystal_description irregular
_exptl_crystal_F_000 588
_exptl_crystal_size_max 0.19
_exptl_crystal_size_mid 0.14
_exptl_crystal_size_min 0.06
_exptl_transmission_factor_max ?
_exptl_transmission_factor_min ?
_diffrn_reflns_av_R_equivalents 0.0530
_diffrn_reflns_av_unetI/netI 0.0648
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max 12
_diffrn_reflns_limit_h_min -12
_diffrn_reflns_limit_k_max 13
_diffrn_reflns_limit_k_min -13
_diffrn_reflns_limit_l_max 21
_diffrn_reflns_limit_l_min -21
_diffrn_reflns_number 29340
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full 25.242
_diffrn_reflns_theta_max 27.999
_diffrn_reflns_theta_min 2.278
_diffrn_ambient_temperature 120.0
_diffrn_detector 'Bruker PHOTON 100 CMOS'
_diffrn_detector_area_resol_mean 10.4
_diffrn_detector_type 'CMOS sensor'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device '3-circle diffractometer'
_diffrn_measurement_device_type 'Bruker D8 Venture'
_diffrn_measurement_method '\f and \w scans'
_diffrn_radiation_monochromator 'focusing mirrors'
_diffrn_radiation_probe x-ray
_diffrn_radiation_type MoK\a
_diffrn_radiation_wavelength 0.71073
_diffrn_source 'microfocus sealed X-ray tube'
_diffrn_source_type 'Incoatec I\mS microsource'
_diffrn_standards_number 0
_reflns_Friedel_coverage 0.000
_reflns_Friedel_fraction_full .
_reflns_Friedel_fraction_max .
_reflns_number_gt 4625
_reflns_number_total 7327
_reflns_special_details
;
Reflections were merged by SHELXL according to the crystal
class for the calculation of statistics and refinement.
_reflns_Friedel_fraction is defined as the number of unique
Friedel pairs measured divided by the number that would be
possible theoretically, ignoring centric projections and
systematic absences.
;
_reflns_threshold_expression 'I > 2\s(I)'
_computing.bruker_data_scaling 'SADABS V2012/1 (Bruker AXS Inc.)'
_computing_cell_refinement 'SAINT V8.38A (Bruker AXS, 2016)'
_computing_data_collection 'APEX3 v.2017.3_0 (Bruker AXS, 2017)'
_computing_data_reduction 'SAINT v8.38A (Bruker AXS, 2016)'
_computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material 'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement 'ShelXL (Sheldrick, 2015)'
_computing_structure_solution 'XS (Sheldrick, 2008)'
_refine_diff_density_max 0.242
_refine_diff_density_min -0.261
_refine_diff_density_rms 0.047
_refine_ls_extinction_coef .
_refine_ls_extinction_method none
_refine_ls_goodness_of_fit_ref 1.034
_refine_ls_hydrogen_treatment constr
_refine_ls_matrix_type full
_refine_ls_number_parameters 397
_refine_ls_number_reflns 7327
_refine_ls_number_restraints 0
_refine_ls_R_factor_all 0.0960
_refine_ls_R_factor_gt 0.0489
_refine_ls_restrained_S_all 1.034
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme calc
_refine_ls_wR_factor_gt 0.1018
_refine_ls_wR_factor_ref 0.1168
_refine_special_details ?
_olex2_refinement_description
;
1. Fixed Uiso
At 1.2 times of:
All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
C22(H22), C23(H23), C24(H24), C25(H25), C26(H26), C32(H32), C33(H33),
C34(H34), C35(H35), C36(H36), C42(H42), C43(H43), C44(H44), C45(H45), C48(H48),
C49(H49), C50(H50), C51(H51), C62(H62), C63(H63), C64(H64), C65(H65),
C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76)
;
_atom_sites_solution_hydrogens geom
_atom_sites_solution_primary direct
_atom_sites_solution_secondary ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.37744(13) 0.46154(10) 0.30489(7) 0.0364(3) Uani 1 1 d . . . . .
C1 C 0.33676(16) 0.37003(14) 0.28412(9) 0.0249(3) Uani 1 1 d . . . . .
C2 C 0.26371(16) 0.36756(14) 0.20785(9) 0.0225(3) Uani 1 1 d . . . . .
C3 C 0.34685(15) 0.29323(13) 0.14607(9) 0.0207(3) Uani 1 1 d . . . . .
C4 C 0.50652(15) 0.22837(13) 0.15363(9) 0.0215(3) Uani 1 1 d . . . . .
C5 C 0.54708(16) 0.15287(14) 0.22423(9) 0.0224(3) Uani 1 1 d . . . . .
C6 C 0.43508(16) 0.13380(14) 0.29797(9) 0.0234(3) Uani 1 1 d . . . . .
C7 C 0.33857(17) 0.23985(14) 0.33153(9) 0.0240(3) Uani 1 1 d . . . . .
C21 C 0.09942(16) 0.42461(14) 0.22042(9) 0.0231(3) Uani 1 1 d . . . . .
C22 C 0.04221(18) 0.54931(15) 0.25105(9) 0.0278(4) Uani 1 1 d . . . . .
H22 H 0.108341 0.601876 0.258785 0.033 Uiso 1 1 calc R . . . .
C23 C -0.11093(19) 0.59687(16) 0.27029(10) 0.0345(4) Uani 1 1 d . . . . .
H23 H -0.149425 0.682761 0.289947 0.041 Uiso 1 1 calc R . . . .
C24 C -0.20781(19) 0.52024(17) 0.26104(10) 0.0367(4) Uani 1 1 d . . . . .
H24 H -0.312567 0.552611 0.275553 0.044 Uiso 1 1 calc R . . . .
C25 C -0.15266(17) 0.39679(16) 0.23078(10) 0.0337(4) Uani 1 1 d . . . . .
H25 H -0.219556 0.344391 0.224037 0.040 Uiso 1 1 calc R . . . .
C26 C -0.00014(17) 0.34890(15) 0.21018(10) 0.0282(4) Uani 1 1 d . . . . .
H26 H 0.037155 0.263949 0.188935 0.034 Uiso 1 1 calc R . . . .
C31 C 0.29049(15) 0.26872(14) 0.06929(9) 0.0210(3) Uani 1 1 d . . . . .
C32 C 0.20447(15) 0.36898(14) 0.02355(9) 0.0235(3) Uani 1 1 d . . . . .
H32 H 0.168318 0.453627 0.045373 0.028 Uiso 1 1 calc R . . . .
C33 C 0.17113(16) 0.34674(15) -0.05316(9) 0.0268(3) Uani 1 1 d . . . . .
H33 H 0.113428 0.416236 -0.084078 0.032 Uiso 1 1 calc R . . . .
C34 C 0.22166(16) 0.22332(15) -0.08510(10) 0.0281(4) Uani 1 1 d . . . . .
H34 H 0.201292 0.208537 -0.138588 0.034 Uiso 1 1 calc R . . . .
C35 C 0.30180(16) 0.12190(15) -0.03876(10) 0.0257(3) Uani 1 1 d . . . . .
H35 H 0.333377 0.036337 -0.059536 0.031 Uiso 1 1 calc R . . . .
C36 C 0.33633(15) 0.14421(14) 0.03772(9) 0.0228(3) Uani 1 1 d . . . . .
H36 H 0.391899 0.073825 0.069029 0.027 Uiso 1 1 calc R . . . .
C41 C 0.62002(15) 0.24325(13) 0.08290(9) 0.0216(3) Uani 1 1 d . . . . .
C42 C 0.58472(16) 0.32690(14) 0.01252(9) 0.0240(3) Uani 1 1 d . . . . .
H42 H 0.486109 0.379874 0.013131 0.029 Uiso 1 1 calc R . . . .
C43 C 0.68804(17) 0.33413(15) -0.05661(10) 0.0282(4) Uani 1 1 d . . . . .
H43 H 0.660441 0.389687 -0.103832 0.034 Uiso 1 1 calc R . . . .
C44 C 0.83412(17) 0.25963(15) -0.05752(10) 0.0314(4) Uani 1 1 d . . . . .
H44 H 0.905771 0.262324 -0.106021 0.038 Uiso 1 1 calc R . . . .
C45 C 0.87417(17) 0.18270(15) 0.01144(10) 0.0298(4) Uani 1 1 d . . . . .
H45 H 0.974983 0.134822 0.010804 0.036 Uiso 1 1 calc R . . . .
C46 C 0.77009(16) 0.17250(14) 0.08339(9) 0.0237(3) Uani 1 1 d . . . . .
C47 C 0.81314(16) 0.09471(14) 0.15800(10) 0.0246(3) Uani 1 1 d . . . . .
C48 C 0.96282(17) 0.02831(15) 0.16366(11) 0.0307(4) Uani 1 1 d . . . . .
H48 H 1.036830 0.029117 0.116092 0.037 Uiso 1 1 calc R . . . .
C49 C 1.00334(18) -0.03706(16) 0.23616(11) 0.0355(4) Uani 1 1 d . . . . .
H49 H 1.104281 -0.082737 0.238226 0.043 Uiso 1 1 calc R . . . .
C50 C 0.89718(18) -0.03688(16) 0.30691(11) 0.0358(4) Uani 1 1 d . . . . .
H50 H 0.926143 -0.079694 0.357855 0.043 Uiso 1 1 calc R . . . .
C51 C 0.75038(18) 0.02528(15) 0.30303(10) 0.0306(4) Uani 1 1 d . . . . .
H51 H 0.678609 0.024903 0.351707 0.037 Uiso 1 1 calc R . . . .
C52 C 0.70385(16) 0.08961(14) 0.22842(10) 0.0241(3) Uani 1 1 d . . . . .
C61 C 0.43133(16) -0.00382(14) 0.32853(9) 0.0246(3) Uani 1 1 d . . . . .
C62 C 0.44292(16) -0.09710(15) 0.27094(10) 0.0276(4) Uani 1 1 d . . . . .
H62 H 0.454870 -0.072632 0.212856 0.033 Uiso 1 1 calc R . . . .
C63 C 0.43736(17) -0.22544(15) 0.29668(11) 0.0338(4) Uani 1 1 d . . . . .
H63 H 0.442905 -0.287532 0.256460 0.041 Uiso 1 1 calc R . . . .
C64 C 0.42376(18) -0.26283(16) 0.38084(12) 0.0390(4) Uani 1 1 d . . . . .
H64 H 0.421580 -0.351034 0.398640 0.047 Uiso 1 1 calc R . . . .
C65 C 0.41331(19) -0.17137(16) 0.43924(11) 0.0384(4) Uani 1 1 d . . . . .
H65 H 0.404644 -0.196998 0.497187 0.046 Uiso 1 1 calc R . . . .
C66 C 0.41548(17) -0.04227(15) 0.41325(10) 0.0317(4) Uani 1 1 d . . . . .
H66 H 0.406063 0.020437 0.453689 0.038 Uiso 1 1 calc R . . . .
C71 C 0.21077(17) 0.24451(15) 0.40023(9) 0.0276(4) Uani 1 1 d . . . . .
C72 C 0.10417(18) 0.17220(17) 0.39858(10) 0.0349(4) Uani 1 1 d . . . . .
H72 H 0.116183 0.114175 0.354976 0.042 Uiso 1 1 calc R . . . .
C73 C -0.0189(2) 0.18441(19) 0.45999(11) 0.0447(5) Uani 1 1 d . . . . .
H73 H -0.090711 0.134311 0.458706 0.054 Uiso 1 1 calc R . . . .
C74 C -0.0376(2) 0.26888(19) 0.52296(11) 0.0473(5) Uani 1 1 d . . . . .
H74 H -0.122476 0.277452 0.565027 0.057 Uiso 1 1 calc R . . . .
C75 C 0.0667(2) 0.34089(19) 0.52488(11) 0.0466(5) Uani 1 1 d . . . . .
H75 H 0.053909 0.398742 0.568660 0.056 Uiso 1 1 calc R . . . .
C76 C 0.1901(2) 0.32986(16) 0.46361(10) 0.0359(4) Uani 1 1 d . . . . .
H76 H 0.260813 0.381012 0.465041 0.043 Uiso 1 1 calc R . . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
O1 0.0472(7) 0.0259(6) 0.0414(7) -0.0051(5) -0.0148(6) -0.0124(5)
C1 0.0235(8) 0.0220(8) 0.0282(8) -0.0066(7) -0.0027(6) -0.0021(6)
C2 0.0245(8) 0.0179(7) 0.0257(8) -0.0007(6) -0.0056(6) -0.0050(6)
C3 0.0190(7) 0.0175(7) 0.0260(8) 0.0006(6) -0.0046(6) -0.0048(6)
C4 0.0194(8) 0.0172(7) 0.0294(8) -0.0061(6) -0.0052(6) -0.0045(6)
C5 0.0217(8) 0.0179(7) 0.0290(8) -0.0043(6) -0.0051(6) -0.0052(6)
C6 0.0233(8) 0.0231(8) 0.0258(8) -0.0004(6) -0.0096(6) -0.0057(6)
C7 0.0260(8) 0.0241(8) 0.0245(8) -0.0027(6) -0.0087(6) -0.0069(7)
C21 0.0246(8) 0.0221(8) 0.0201(8) -0.0012(6) -0.0032(6) -0.0006(6)
C22 0.0339(9) 0.0239(8) 0.0241(8) -0.0052(6) -0.0073(7) -0.0007(7)
C23 0.0397(10) 0.0300(9) 0.0275(9) -0.0103(7) -0.0086(7) 0.0097(8)
C24 0.0250(9) 0.0432(10) 0.0350(10) -0.0069(8) -0.0032(7) 0.0062(8)
C25 0.0229(9) 0.0362(10) 0.0398(10) -0.0056(8) -0.0003(7) -0.0042(7)
C26 0.0251(8) 0.0237(8) 0.0334(9) -0.0040(7) -0.0008(7) -0.0023(7)
C31 0.0150(7) 0.0227(8) 0.0254(8) -0.0040(6) -0.0007(6) -0.0048(6)
C32 0.0180(8) 0.0208(8) 0.0308(9) -0.0042(6) -0.0026(6) -0.0025(6)
C33 0.0196(8) 0.0291(9) 0.0308(9) -0.0005(7) -0.0064(6) -0.0025(6)
C34 0.0205(8) 0.0354(9) 0.0305(9) -0.0080(7) -0.0064(7) -0.0066(7)
C35 0.0180(8) 0.0245(8) 0.0357(9) -0.0107(7) -0.0033(6) -0.0040(6)
C36 0.0162(7) 0.0220(8) 0.0303(8) -0.0019(6) -0.0040(6) -0.0040(6)
C41 0.0178(7) 0.0167(7) 0.0317(8) -0.0063(6) -0.0040(6) -0.0045(6)
C42 0.0195(8) 0.0193(8) 0.0333(9) -0.0022(6) -0.0040(6) -0.0041(6)
C43 0.0269(9) 0.0249(8) 0.0336(9) 0.0015(7) -0.0052(7) -0.0081(7)
C44 0.0270(9) 0.0294(9) 0.0361(9) -0.0009(7) 0.0027(7) -0.0080(7)
C45 0.0193(8) 0.0252(8) 0.0432(10) -0.0028(7) -0.0015(7) -0.0034(6)
C46 0.0193(8) 0.0183(7) 0.0351(9) -0.0040(6) -0.0049(6) -0.0060(6)
C47 0.0212(8) 0.0195(8) 0.0358(9) -0.0043(7) -0.0074(7) -0.0065(6)
C48 0.0235(8) 0.0253(8) 0.0445(10) -0.0048(7) -0.0083(7) -0.0044(7)
C49 0.0227(9) 0.0296(9) 0.0565(12) -0.0019(8) -0.0171(8) -0.0034(7)
C50 0.0334(10) 0.0306(9) 0.0472(11) 0.0063(8) -0.0220(8) -0.0076(8)
C51 0.0290(9) 0.0287(9) 0.0373(9) 0.0014(7) -0.0107(7) -0.0103(7)
C52 0.0225(8) 0.0184(8) 0.0344(9) -0.0031(6) -0.0108(7) -0.0058(6)
C61 0.0202(8) 0.0219(8) 0.0311(9) -0.0005(7) -0.0053(6) -0.0027(6)
C62 0.0211(8) 0.0261(8) 0.0344(9) -0.0030(7) -0.0029(7) -0.0033(6)
C63 0.0269(9) 0.0240(9) 0.0498(11) -0.0075(8) -0.0036(8) -0.0037(7)
C64 0.0313(10) 0.0236(9) 0.0574(12) 0.0033(8) 0.0001(8) -0.0039(7)
C65 0.0372(10) 0.0331(10) 0.0394(10) 0.0077(8) -0.0013(8) -0.0035(8)
C66 0.0316(9) 0.0272(9) 0.0346(9) -0.0015(7) -0.0051(7) -0.0037(7)
C71 0.0318(9) 0.0241(8) 0.0236(8) 0.0002(7) -0.0070(7) 0.0015(7)
C72 0.0309(9) 0.0373(10) 0.0346(10) -0.0036(8) -0.0013(7) -0.0056(8)
C73 0.0361(11) 0.0473(11) 0.0445(11) 0.0052(9) 0.0023(8) -0.0056(9)
C74 0.0430(11) 0.0505(12) 0.0323(10) 0.0082(9) 0.0061(8) 0.0087(10)
C75 0.0633(14) 0.0406(11) 0.0232(9) -0.0021(8) -0.0037(9) 0.0110(10)
C76 0.0470(11) 0.0301(9) 0.0265(9) -0.0034(7) -0.0072(8) 0.0008(8)
_geom_special_details
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.2071(17) . ?
C1 C2 1.508(2) . ?
C1 C7 1.506(2) . ?
C2 C3 1.346(2) . ?
C2 C21 1.489(2) . ?
C3 C4 1.4966(19) . ?
C3 C31 1.490(2) . ?
C4 C5 1.382(2) . ?
C4 C41 1.456(2) . ?
C5 C6 1.490(2) . ?
C5 C52 1.459(2) . ?
C6 C7 1.346(2) . ?
C6 C61 1.493(2) . ?
C7 C71 1.490(2) . ?
C21 C22 1.393(2) . ?
C21 C26 1.397(2) . ?
C22 H22 0.9500 . ?
C22 C23 1.386(2) . ?
C23 H23 0.9500 . ?
C23 C24 1.379(2) . ?
C24 H24 0.9500 . ?
C24 C25 1.377(2) . ?
C25 H25 0.9500 . ?
C25 C26 1.383(2) . ?
C26 H26 0.9500 . ?
C31 C32 1.3928(19) . ?
C31 C36 1.391(2) . ?
C32 H32 0.9500 . ?
C32 C33 1.381(2) . ?
C33 H33 0.9500 . ?
C33 C34 1.385(2) . ?
C34 H34 0.9500 . ?
C34 C35 1.380(2) . ?
C35 H35 0.9500 . ?
C35 C36 1.382(2) . ?
C36 H36 0.9500 . ?
C41 C42 1.408(2) . ?
C41 C46 1.4151(19) . ?
C42 H42 0.9500 . ?
C42 C43 1.366(2) . ?
C43 H43 0.9500 . ?
C43 C44 1.393(2) . ?
C44 H44 0.9500 . ?
C44 C45 1.366(2) . ?
C45 H45 0.9500 . ?
C45 C46 1.407(2) . ?
C46 C47 1.452(2) . ?
C47 C48 1.412(2) . ?
C47 C52 1.410(2) . ?
C48 H48 0.9500 . ?
C48 C49 1.366(2) . ?
C49 H49 0.9500 . ?
C49 C50 1.390(2) . ?
C50 H50 0.9500 . ?
C50 C51 1.373(2) . ?
C51 H51 0.9500 . ?
C51 C52 1.409(2) . ?
C61 C62 1.387(2) . ?
C61 C66 1.391(2) . ?
C62 H62 0.9500 . ?
C62 C63 1.387(2) . ?
C63 H63 0.9500 . ?
C63 C64 1.380(2) . ?
C64 H64 0.9500 . ?
C64 C65 1.385(2) . ?
C65 H65 0.9500 . ?
C65 C66 1.388(2) . ?
C66 H66 0.9500 . ?
C71 C72 1.394(2) . ?
C71 C76 1.384(2) . ?
C72 H72 0.9500 . ?
C72 C73 1.382(2) . ?
C73 H73 0.9500 . ?
C73 C74 1.375(3) . ?
C74 H74 0.9500 . ?
C74 C75 1.374(3) . ?
C75 H75 0.9500 . ?
C75 C76 1.383(2) . ?
C76 H76 0.9500 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 C1 C2 126.32(14) . . ?
O1 C1 C7 127.27(14) . . ?
C7 C1 C2 106.29(12) . . ?
C3 C2 C1 116.35(13) . . ?
C3 C2 C21 128.67(13) . . ?
C21 C2 C1 113.50(12) . . ?
C2 C3 C4 119.14(13) . . ?
C2 C3 C31 124.38(13) . . ?
C31 C3 C4 116.48(12) . . ?
C5 C4 C3 121.87(13) . . ?
C5 C4 C41 119.99(13) . . ?
C41 C4 C3 118.12(13) . . ?
C4 C5 C6 122.05(13) . . ?
C4 C5 C52 120.06(13) . . ?
C52 C5 C6 117.89(13) . . ?
C5 C6 C61 117.73(13) . . ?
C7 C6 C5 119.05(13) . . ?
C7 C6 C61 123.15(14) . . ?
C6 C7 C1 116.88(13) . . ?
C6 C7 C71 128.49(14) . . ?
C71 C7 C1 113.38(12) . . ?
C22 C21 C2 120.38(13) . . ?
C22 C21 C26 118.80(14) . . ?
C26 C21 C2 120.48(13) . . ?
C21 C22 H22 119.9 . . ?
C23 C22 C21 120.17(15) . . ?
C23 C22 H22 119.9 . . ?
C22 C23 H23 119.8 . . ?
C24 C23 C22 120.38(15) . . ?
C24 C23 H23 119.8 . . ?
C23 C24 H24 120.0 . . ?
C25 C24 C23 120.00(15) . . ?
C25 C24 H24 120.0 . . ?
C24 C25 H25 119.9 . . ?
C24 C25 C26 120.18(16) . . ?
C26 C25 H25 119.9 . . ?
C21 C26 H26 119.8 . . ?
C25 C26 C21 120.45(14) . . ?
C25 C26 H26 119.8 . . ?
C32 C31 C3 122.24(13) . . ?
C36 C31 C3 119.02(13) . . ?
C36 C31 C32 118.47(13) . . ?
C31 C32 H32 119.6 . . ?
C33 C32 C31 120.75(14) . . ?
C33 C32 H32 119.6 . . ?
C32 C33 H33 119.9 . . ?
C32 C33 C34 120.12(14) . . ?
C34 C33 H33 119.9 . . ?
C33 C34 H34 120.2 . . ?
C35 C34 C33 119.61(14) . . ?
C35 C34 H34 120.2 . . ?
C34 C35 H35 119.8 . . ?
C34 C35 C36 120.33(14) . . ?
C36 C35 H35 119.8 . . ?
C31 C36 H36 119.7 . . ?
C35 C36 C31 120.63(14) . . ?
C35 C36 H36 119.7 . . ?
C42 C41 C4 121.60(12) . . ?
C42 C41 C46 118.19(13) . . ?
C46 C41 C4 120.21(13) . . ?
C41 C42 H42 119.0 . . ?
C43 C42 C41 121.94(13) . . ?
C43 C42 H42 119.0 . . ?
C42 C43 H43 120.2 . . ?
C42 C43 C44 119.66(15) . . ?
C44 C43 H43 120.2 . . ?
C43 C44 H44 120.1 . . ?
C45 C44 C43 119.89(15) . . ?
C45 C44 H44 120.1 . . ?
C44 C45 H45 119.1 . . ?
C44 C45 C46 121.76(14) . . ?
C46 C45 H45 119.1 . . ?
C41 C46 C47 119.60(13) . . ?
C45 C46 C41 118.37(14) . . ?
C45 C46 C47 122.01(13) . . ?
C48 C47 C46 121.98(14) . . ?
C52 C47 C46 119.28(13) . . ?
C52 C47 C48 118.68(14) . . ?
C47 C48 H48 119.3 . . ?
C49 C48 C47 121.33(15) . . ?
C49 C48 H48 119.3 . . ?
C48 C49 H49 119.9 . . ?
C48 C49 C50 120.12(15) . . ?
C50 C49 H49 119.9 . . ?
C49 C50 H50 120.1 . . ?
C51 C50 C49 119.88(15) . . ?
C51 C50 H50 120.1 . . ?
C50 C51 H51 119.3 . . ?
C50 C51 C52 121.43(16) . . ?
C52 C51 H51 119.3 . . ?
C47 C52 C5 120.41(13) . . ?
C51 C52 C5 121.14(14) . . ?
C51 C52 C47 118.43(13) . . ?
C62 C61 C6 119.28(13) . . ?
C62 C61 C66 118.40(14) . . ?
C66 C61 C6 122.32(14) . . ?
C61 C62 H62 119.4 . . ?
C63 C62 C61 121.15(15) . . ?
C63 C62 H62 119.4 . . ?
C62 C63 H63 120.1 . . ?
C64 C63 C62 119.89(16) . . ?
C64 C63 H63 120.1 . . ?
C63 C64 H64 120.1 . . ?
C63 C64 C65 119.79(16) . . ?
C65 C64 H64 120.1 . . ?
C64 C65 H65 120.0 . . ?
C64 C65 C66 120.09(16) . . ?
C66 C65 H65 120.0 . . ?
C61 C66 H66 119.7 . . ?
C65 C66 C61 120.65(16) . . ?
C65 C66 H66 119.7 . . ?
C72 C71 C7 121.22(14) . . ?
C76 C71 C7 119.68(15) . . ?
C76 C71 C72 118.90(15) . . ?
C71 C72 H72 119.8 . . ?
C73 C72 C71 120.38(16) . . ?
C73 C72 H72 119.8 . . ?
C72 C73 H73 119.9 . . ?
C74 C73 C72 120.15(18) . . ?
C74 C73 H73 119.9 . . ?
C73 C74 H74 120.1 . . ?
C75 C74 C73 119.83(17) . . ?
C75 C74 H74 120.1 . . ?
C74 C75 H75 119.7 . . ?
C74 C75 C76 120.56(17) . . ?
C76 C75 H75 119.7 . . ?
C71 C76 H76 119.9 . . ?
C75 C76 C71 120.16(17) . . ?
C75 C76 H76 119.9 . . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C1 C2 C3 C4 -4.9(2) . . . . ?
C1 C2 C3 C31 174.39(13) . . . . ?
C1 C2 C21 C22 52.24(18) . . . . ?
C1 C2 C21 C26 -120.95(15) . . . . ?
C1 C7 C6 C5 8.5(2) . . . . ?
C1 C7 C6 C61 -168.57(13) . . . . ?
C1 C7 C71 C72 116.22(16) . . . . ?
C1 C7 C71 C76 -58.54(18) . . . . ?
C2 C1 C7 C6 72.14(16) . . . . ?
C2 C1 C7 C71 -96.20(14) . . . . ?
C2 C3 C4 C5 51.38(19) . . . . ?
C2 C3 C4 C41 -130.48(14) . . . . ?
C2 C3 C31 C32 45.3(2) . . . . ?
C2 C3 C31 C36 -140.77(15) . . . . ?
C3 C2 C1 O1 109.28(18) . . . . ?
C3 C2 C1 C7 -74.56(16) . . . . ?
C3 C2 C21 C22 -142.29(16) . . . . ?
C3 C2 C21 C26 44.5(2) . . . . ?
C3 C4 C5 C6 -1.4(2) . . . . ?
C3 C4 C5 C52 178.99(13) . . . . ?
C4 C3 C2 C21 -170.03(13) . . . . ?
C4 C3 C31 C32 -135.43(14) . . . . ?
C4 C3 C31 C36 38.55(18) . . . . ?
C4 C5 C6 C7 -51.4(2) . . . . ?
C4 C5 C6 C61 125.80(15) . . . . ?
C5 C4 C3 C31 -127.97(14) . . . . ?
C5 C6 C7 C71 174.76(14) . . . . ?
C5 C6 C61 C62 -42.76(19) . . . . ?
C5 C6 C61 C66 137.70(15) . . . . ?
C6 C5 C4 C41 -179.55(13) . . . . ?
C6 C7 C1 O1 -111.74(18) . . . . ?
C6 C7 C71 C72 -50.5(2) . . . . ?
C6 C7 C71 C76 134.78(16) . . . . ?
C7 C1 C2 C21 92.82(14) . . . . ?
C7 C6 C5 C52 128.17(15) . . . . ?
C7 C6 C61 C62 134.33(16) . . . . ?
C7 C6 C61 C66 -45.2(2) . . . . ?
C21 C2 C1 O1 -83.35(19) . . . . ?
C21 C2 C3 C31 9.3(2) . . . . ?
C31 C3 C4 C41 50.17(17) . . . . ?
C41 C4 C5 C52 0.9(2) . . . . ?
C52 C5 C6 C61 -54.62(18) . . . . ?
C61 C6 C7 C71 -2.3(2) . . . . ?
C71 C7 C1 O1 79.92(19) . . . . ?
_olex2_submission_special_instructions 'No special instructions were received'
_iucr_refine_instructions_details
;
TITL 18srv286 in P-1 #2
REM reset to P-1 #2
CELL 0.71073 9.3113 10.5095 16.2093 84.8752 80.8635 75.9212
ZERR 2 0.0006 0.0007 0.001 0.0026 0.0025 0.0025
LATT 1
SFAC C H O
UNIT 86 56 2
L.S. 9
PLAN 5
SIZE 0.06 0.14 0.19
TEMP -153.15
CONF C3 C2 C1 O1
CONF C3 C2 C1 C7
CONF C21 C2 C1 O1
CONF C7 C1 C2 C21
CONF C1 C2 C3 C4
CONF C4 C3 C2 C21
CONF C1 C2 C3 C31
CONF C21 C2 C3 C31
CONF C2 C3 C4 C5
CONF C5 C4 C3 C31
CONF C2 C3 C4 C41
CONF C31 C3 C4 C41
CONF C3 C4 C5 C6
CONF C6 C5 C4 C41
CONF C3 C4 C5 C52
CONF C41 C4 C5 C52
CONF C4 C5 C6 C7
CONF C7 C6 C5 C52
CONF C4 C5 C6 C61
CONF C52 C5 C6 C61
CONF C1 C7 C6 C5
CONF C1 C7 C6 C61
CONF C5 C6 C7 C71
CONF C61 C6 C7 C71
CONF C6 C7 C1 O1
CONF C2 C1 C7 C6
CONF C71 C7 C1 O1
CONF C2 C1 C7 C71
CONF C1 C2 C21 C22
CONF C3 C2 C21 C22
CONF C1 C2 C21 C26
CONF C3 C2 C21 C26
CONF C2 C3 C31 C32
CONF C4 C3 C31 C32
CONF C2 C3 C31 C36
CONF C4 C3 C31 C36
CONF C5 C6 C61 C62
CONF C7 C6 C61 C62
CONF C5 C6 C61 C66
CONF C7 C6 C61 C66
CONF C1 C7 C71 C72
CONF C6 C7 C71 C72
CONF C1 C7 C71 C76
CONF C6 C7 C71 C76
BOND $h
fmap 2 53
acta
OMIT -2 56
OMIT 0 1 0
WGHT 0.05 0.2
FVAR 0.24308
REM
REM
REM
O1 3 0.37744 0.46154 0.30489 11.00000 0.04725 0.02593 0.04142 =
-0.00509 -0.01484 -0.01239
C1 1 0.33676 0.37003 0.28412 11.00000 0.02353 0.02200 0.02820 =
-0.00657 -0.00271 -0.00215
C2 1 0.26371 0.36756 0.20785 11.00000 0.02448 0.01791 0.02568 =
-0.00072 -0.00560 -0.00498
C3 1 0.34685 0.29323 0.14607 11.00000 0.01902 0.01751 0.02599 =
0.00062 -0.00455 -0.00476
C4 1 0.50652 0.22837 0.15363 11.00000 0.01936 0.01719 0.02945 =
-0.00609 -0.00515 -0.00447
C5 1 0.54708 0.15287 0.22423 11.00000 0.02174 0.01786 0.02901 =
-0.00430 -0.00511 -0.00521
C6 1 0.43508 0.13380 0.29797 11.00000 0.02328 0.02309 0.02576 =
-0.00045 -0.00956 -0.00568
C7 1 0.33857 0.23986 0.33153 11.00000 0.02601 0.02406 0.02454 =
-0.00271 -0.00868 -0.00694
C21 1 0.09942 0.42461 0.22042 11.00000 0.02458 0.02214 0.02009 =
-0.00123 -0.00323 -0.00061
C22 1 0.04221 0.54931 0.25105 11.00000 0.03388 0.02395 0.02412 =
-0.00523 -0.00732 -0.00075
AFIX 43
H22 2 0.10834 0.60188 0.25878 11.00000 -1.20000
AFIX 0
C23 1 -0.11094 0.59687 0.27029 11.00000 0.03967 0.02997 0.02747 =
-0.01029 -0.00863 0.00966
AFIX 43
H23 2 -0.14943 0.68276 0.28995 11.00000 -1.20000
AFIX 0
C24 1 -0.20781 0.52024 0.26105 11.00000 0.02496 0.04318 0.03496 =
-0.00689 -0.00318 0.00620
AFIX 43
H24 2 -0.31257 0.55261 0.27555 11.00000 -1.20000
AFIX 0
C25 1 -0.15266 0.39679 0.23078 11.00000 0.02295 0.03616 0.03976 =
-0.00562 -0.00025 -0.00415
AFIX 43
H25 2 -0.21956 0.34439 0.22404 11.00000 -1.20000
AFIX 0
C26 1 -0.00014 0.34890 0.21019 11.00000 0.02509 0.02366 0.03344 =
-0.00396 -0.00076 -0.00234
AFIX 43
H26 2 0.03716 0.26395 0.18893 11.00000 -1.20000
AFIX 0
C31 1 0.29049 0.26872 0.06929 11.00000 0.01495 0.02270 0.02536 =
-0.00403 -0.00069 -0.00480
C32 1 0.20447 0.36898 0.02355 11.00000 0.01800 0.02078 0.03083 =
-0.00421 -0.00255 -0.00248
AFIX 43
H32 2 0.16832 0.45363 0.04537 11.00000 -1.20000
AFIX 0
C33 1 0.17113 0.34674 -0.05316 11.00000 0.01957 0.02905 0.03082 =
-0.00049 -0.00645 -0.00253
AFIX 43
H33 2 0.11343 0.41624 -0.08408 11.00000 -1.20000
AFIX 0
C34 1 0.22166 0.22332 -0.08510 11.00000 0.02049 0.03536 0.03055 =
-0.00805 -0.00638 -0.00659
AFIX 43
H34 2 0.20129 0.20854 -0.13859 11.00000 -1.20000
AFIX 0
C35 1 0.30180 0.12190 -0.03876 11.00000 0.01796 0.02451 0.03570 =
-0.01065 -0.00333 -0.00396
AFIX 43
H35 2 0.33338 0.03634 -0.05954 11.00000 -1.20000
AFIX 0
C36 1 0.33633 0.14421 0.03772 11.00000 0.01624 0.02197 0.03032 =
-0.00195 -0.00401 -0.00399
AFIX 43
H36 2 0.39190 0.07383 0.06903 11.00000 -1.20000
AFIX 0
C41 1 0.62003 0.24325 0.08290 11.00000 0.01780 0.01673 0.03166 =
-0.00630 -0.00402 -0.00452
C42 1 0.58472 0.32690 0.01252 11.00000 0.01952 0.01927 0.03326 =
-0.00218 -0.00396 -0.00412
AFIX 43
H42 2 0.48611 0.37987 0.01313 11.00000 -1.20000
AFIX 0
C43 1 0.68804 0.33414 -0.05661 11.00000 0.02687 0.02493 0.03361 =
0.00152 -0.00515 -0.00807
AFIX 43
H43 2 0.66044 0.38969 -0.10383 11.00000 -1.20000
AFIX 0
C44 1 0.83412 0.25964 -0.05752 11.00000 0.02697 0.02943 0.03613 =
-0.00088 0.00272 -0.00804
AFIX 43
H44 2 0.90577 0.26232 -0.10602 11.00000 -1.20000
AFIX 0
C45 1 0.87417 0.18271 0.01144 11.00000 0.01927 0.02522 0.04323 =
-0.00275 -0.00149 -0.00341
AFIX 43
H45 2 0.97498 0.13482 0.01080 11.00000 -1.20000
AFIX 0
C46 1 0.77009 0.17250 0.08339 11.00000 0.01927 0.01832 0.03515 =
-0.00401 -0.00491 -0.00601
C47 1 0.81314 0.09471 0.15800 11.00000 0.02118 0.01955 0.03578 =
-0.00433 -0.00744 -0.00653
C48 1 0.96282 0.02831 0.16366 11.00000 0.02345 0.02527 0.04448 =
-0.00484 -0.00826 -0.00436
AFIX 43
H48 2 1.03683 0.02912 0.11609 11.00000 -1.20000
AFIX 0
C49 1 1.00334 -0.03706 0.23616 11.00000 0.02273 0.02958 0.05654 =
-0.00188 -0.01708 -0.00341
AFIX 43
H49 2 1.10428 -0.08274 0.23823 11.00000 -1.20000
AFIX 0
C50 1 0.89718 -0.03688 0.30691 11.00000 0.03344 0.03063 0.04722 =
0.00625 -0.02198 -0.00762
AFIX 43
H50 2 0.92614 -0.07969 0.35785 11.00000 -1.20000
AFIX 0
C51 1 0.75038 0.02528 0.30303 11.00000 0.02901 0.02868 0.03730 =
0.00138 -0.01068 -0.01032
AFIX 43
H51 2 0.67861 0.02490 0.35171 11.00000 -1.20000
AFIX 0
C52 1 0.70385 0.08961 0.22842 11.00000 0.02245 0.01843 0.03440 =
-0.00313 -0.01083 -0.00576
C61 1 0.43133 -0.00382 0.32853 11.00000 0.02017 0.02193 0.03108 =
-0.00047 -0.00532 -0.00275
C62 1 0.44292 -0.09710 0.27094 11.00000 0.02108 0.02609 0.03445 =
-0.00305 -0.00288 -0.00325
AFIX 43
H62 2 0.45487 -0.07263 0.21286 11.00000 -1.20000
AFIX 0
C63 1 0.43736 -0.22544 0.29668 11.00000 0.02692 0.02404 0.04981 =
-0.00747 -0.00358 -0.00374
AFIX 43
H63 2 0.44290 -0.28753 0.25646 11.00000 -1.20000
AFIX 0
C64 1 0.42376 -0.26283 0.38084 11.00000 0.03132 0.02361 0.05744 =
0.00328 0.00008 -0.00386
AFIX 43
H64 2 0.42158 -0.35103 0.39864 11.00000 -1.20000
AFIX 0
C65 1 0.41331 -0.17137 0.43925 11.00000 0.03715 0.03305 0.03936 =
0.00771 -0.00130 -0.00352
AFIX 43
H65 2 0.40464 -0.19700 0.49719 11.00000 -1.20000
AFIX 0
C66 1 0.41548 -0.04227 0.41325 11.00000 0.03157 0.02721 0.03464 =
-0.00145 -0.00514 -0.00367
AFIX 43
H66 2 0.40606 0.02044 0.45369 11.00000 -1.20000
AFIX 0
C71 1 0.21077 0.24451 0.40023 11.00000 0.03183 0.02409 0.02359 =
0.00020 -0.00699 0.00146
C72 1 0.10417 0.17219 0.39858 11.00000 0.03093 0.03725 0.03457 =
-0.00358 -0.00131 -0.00558
AFIX 43
H72 2 0.11618 0.11418 0.35498 11.00000 -1.20000
AFIX 0
C73 1 -0.01889 0.18441 0.45999 11.00000 0.03615 0.04729 0.04445 =
0.00520 0.00231 -0.00565
AFIX 43
H73 2 -0.09071 0.13431 0.45871 11.00000 -1.20000
AFIX 0
C74 1 -0.03763 0.26888 0.52296 11.00000 0.04301 0.05049 0.03231 =
0.00817 0.00608 0.00866
AFIX 43
H74 2 -0.12248 0.27745 0.56503 11.00000 -1.20000
AFIX 0
C75 1 0.06666 0.34089 0.52488 11.00000 0.06327 0.04060 0.02321 =
-0.00206 -0.00371 0.01104
AFIX 43
H75 2 0.05391 0.39874 0.56866 11.00000 -1.20000
AFIX 0
C76 1 0.19009 0.32986 0.46360 11.00000 0.04695 0.03013 0.02647 =
-0.00339 -0.00724 0.00078
AFIX 43
H76 2 0.26081 0.38101 0.46504 11.00000 -1.20000
AFIX 0
HKLF 4
END
;