Anisotropic elasticity and plasticity of organic crystal
Wang, Jian-Rong; Li, Meiqi; Yu, Qihui; Zhang, Zaiyong; Zhu, Bingqing; Qin, Wenming; Mei, Xuefeng; Chemical Communications  (2019) –; doi:10.1039/C9CC03542G

data_7123631
_publ_section_title
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 Anisotropic elasticity and plasticity of organic crystal
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03542G
_journal_year                    2019
_chemical_formula_moiety         '2(C28 H44 O), C27 H46 O'
_chemical_formula_sum            'C83 H134 O3'
_chemical_formula_weight         1179.89
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2018-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-11-19 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.4109(3)
_cell_length_b                   33.5378(14)
_cell_length_c                   35.2624(14)
_cell_measurement_reflns_used    8849
_cell_measurement_temperature    173
_cell_measurement_theta_max      20.74
_cell_measurement_theta_min      2.31
_cell_volume                     7581.7(6)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0713
_diffrn_reflns_av_unetI/netI     0.0732
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            56930
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.997
_diffrn_reflns_theta_max         24.997
_diffrn_reflns_theta_min         1.676
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0942 before and 0.0717 after correction. The Ratio of minimum to maximum transmission is 0.7690. The \l/2 correction factor is 0.0015.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.034
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2624
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     794
_refine_ls_number_reflns         13325
_refine_ls_number_restraints     617
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0659
_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^)+(0.0935P)^2^+2.5009P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1617
_refine_ls_wR_factor_ref         0.1912
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                8721
_reflns_number_total             13325
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03542g5.cif
_cod_data_source_block           mo_2015111_0m
_cod_database_code               7123631
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.986
_olex2_refinement_description
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1. Twinned data refinement
 Scales: 0(3)
 1(3)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, {H27g,H27h,H27i} of C27B, {H26g,H26h,H26i} of C26B, {H26d,
  H26e,H26f} of C26A, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups, {H27a,H27b,H27c} of C27, {H26a,H26b,H26c} of C26, {H21a,
  H21b,H21c} of C21, {H18a,H18b,H18c} of C18, {H27d,H27e,H27f} of C27A, {H19a,
  H19b,H19c} of C19, {H18d,H18e,H18f} of C18A, {H21d,H21e,H21f} of C21A, {H28a,
  H28b,H28c} of C28A, {H28d,H28e,H28f} of C28B, {H18g,H18h,H18i} of C18B, {H21g,
  H21h,H21i} of C21B
3. Restrained distances
 O2-H2 = O3-H3
 0.82 with sigma of 0.01
 O3-H3 = O2-H2
 0.82 with sigma of 0.01
4. Rigid bond restraints
 C25A, C27A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C25B, C27B
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C28B, C27B, C25B, C26B, C27A, C26A, C25A, C28A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C24B, C25B
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
5. Uiso/Uaniso restraints and constraints
C25A \\sim C27A: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
C25B \\sim C27B: within 2A with sigma of 0.02 and sigma for terminal atoms of
0.04
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C24B \\sim C25B: within 2A with sigma of 0.005 and sigma for terminal atoms of
0.01
Uanis(C28B) \\sim Ueq, Uanis(C27B) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C28B) \\sim Ueq, Uanis(C27B) \\sim Ueq, Uanis(C26B) \\sim Ueq,
Uanis(C27A) \\sim Ueq, Uanis(C26A) \\sim Ueq, Uanis(C25A) \\sim Ueq,
Uanis(C28A) \\sim Ueq, Uanis(C25B) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
6.a Ternary CH refined with riding coordinates:
 C25A(H25A), C24B(H24d), C3A(H3Aa), C14A(H14A), C17A(H17A), C20A(H20A),
 C24A(H24c), C3B(H3B), C14B(H14B), C17B(H17B), C20B(H20B), C3(H3a), C8(H8),
 C14(H14), C17(H17), C20(H20), C25(H25), C9(H9), C25B(H25B)
6.b Secondary CH2 refined with riding coordinates:
 C2A(H2Aa,H2Ab), C9A(H9Aa,H9Ab), C11A(H11c,H11d), C12A(H12c,H12d), C12B(H12e,
 H12f), C11B(H11e,H11f), C2B(H2Ba,H2Bb), C23(H23a,H23b), C16(H16a,H16b),
 C15(H15a,H15b), C2(H2a,H2b), C1(H1a,H1b), C4A(H4Aa,H4Ab), C1A(H1Aa,H1Ab),
 C16A(H16c,H16d), C15A(H15c,H15d), C4B(H4Ba,H4Bb), C9B(H9Ba,H9Bb), C15B(H15e,
 H15f), C16B(H16e,H16f), C1B(H1Ba,H1Bb), C4(H4a,H4b), C7(H7a,H7b), C22(H22a,
 H22b), C24(H24a,H24b), C11(H11a,H11b), C12(H12a,H12b)
6.c Aromatic/amide H refined with riding coordinates:
 C22B(H22d), C23B(H23d), C6A(H6A), C7A(H7Aa), C22A(H22c), C23A(H23c), C6B(H6B),
  C7B(H7Ba), C6(H6)
6.d X=CH2 refined with riding coordinates:
 C19B(H19f,H19g), C19A(H19d,H19e)
6.e Idealised Me refined as rotating group:
 C26A(H26d,H26e,H26f), C28A(H28a,H28b,H28c), C28B(H28d,H28e,H28f), C27(H27a,
 H27b,H27c), C26(H26a,H26b,H26c), C21(H21a,H21b,H21c), C21A(H21d,H21e,H21f),
 C18A(H18d,H18e,H18f), C18B(H18g,H18h,H18i), C21B(H21g,H21h,H21i), C19(H19a,
 H19b,H19c), C18(H18a,H18b,H18c), C27B(H27g,H27h,H27i), C26B(H26g,H26h,H26i),
 C27A(H27d,H27e,H27f)
6.f Idealised tetrahedral OH refined as rotating group:
 O1(H1), O2(H2), O3(H3)
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_olex2_submission_special_instructions 'No special instructions were received'