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_7123630
_publ_section_title
;
 Anisotropic elasticity and plasticity of organic crystal
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC03542G
_journal_year                    2019
_chemical_absolute_configuration rmad
_chemical_formula_moiety         'C27 H44 O, 2(C27 H46 O)'
_chemical_formula_sum            'C81 H136 O3'
_chemical_formula_weight         1157.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           5
_space_group_name_Hall           'C 2y'
_space_group_name_H-M_alt        'C 1 2 1'
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-11-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-11-19 deposited with the CCDC.    2019-06-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 95.942(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.6899(9)
_cell_length_b                   6.3426(2)
_cell_length_c                   54.772(2)
_cell_measurement_reflns_used    9981
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      65.05
_cell_measurement_theta_min      3.75
_cell_volume                     8185.6(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      173.0
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0357
_diffrn_reflns_av_unetI/netI     0.0515
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       63
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            32087
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        63.000
_diffrn_reflns_theta_max         63.000
_diffrn_reflns_theta_min         3.245
_exptl_absorpt_coefficient_mu    0.405
_exptl_absorpt_correction_T_max  0.0624
_exptl_absorpt_correction_T_min  0.0059
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1527 before and 0.0747 after correction.
The Ratio of minimum to maximum transmission is 0.0946.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.940
_exptl_crystal_description       needle
_exptl_crystal_F_000             2584
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_platon_squeeze_details
;
TITL 161102vd3_0m_a.res in C2
CELL   23.6899    6.3426   54.7720     90.00     95.94     90.00
SPGR C2
C101 0.946 0.037 0.656 !       2.19 eA-3
C102 0.638 0.266 0.339 !       2.07 eA-3
C103 0.900 0.136 0.654 !       1.96 eA-3
C104 0.954 0.507 0.653 !       1.80 eA-3
C105 0.992 0.106 0.649 !       1.79 eA-3
C106 0.594 0.302 0.336 !       1.63 eA-3
C107 0.535 0.456 0.316 !       1.60 eA-3
C108 0.079 0.187 0.361 !       1.57 eA-3
C109 0.540 0.191 0.336 !       1.52 eA-3
C110 0.348 0.498 0.660 !       1.51 eA-3
C111 0.094 0.392 0.335 !       1.46 eA-3
C112 0.397 0.493 0.664 !       1.44 eA-3
C113 0.006 0.334 0.656 !       1.39 eA-3
C114 0.846 0.501 0.656 !       1.35 eA-3
C115 0.433 0.328 0.648 !       1.30 eA-3
C116 0.486 0.251 0.688 !       1.28 eA-3
C117 0.495 0.317 0.351 !       1.20 eA-3
C118 0.486 0.380 0.648 !       1.11 eA-3
C119 0.493 0.068 0.351 !       0.87 eA-3
C120 0.077 0.364 0.362 !       0.84 eA-3
Q121 0.449 0.500 0.405 !       0.67 eA-3
Q122 0.456 0.051 0.040 !       0.61 eA-3
Q123 0.540 0.510 0.581 !       0.59 eA-3
;
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.254
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details
;
 Flack x determined using 4000 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.12(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     783
_refine_ls_number_reflns         13059
_refine_ls_number_restraints     706
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.1062
_refine_ls_R_factor_gt           0.0983
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1652P)^2^+1.3395P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2418
_refine_ls_wR_factor_ref         0.2496
_reflns_Friedel_coverage         0.803
_reflns_Friedel_fraction_full    0.978
_reflns_Friedel_fraction_max     0.978
_reflns_number_gt                11090
_reflns_number_total             13059
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9cc03542g5.cif
_cod_data_source_block           161102vd3_0m_sq
_cod_database_code               7123630
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C26B-C25B = C27B-C25B
 1.58 with sigma of 0.02
 C26-C25
 1.58 with sigma of 0.02
 O1-H1
 0.85 with sigma of 0.02
 O2-H2
 0.85 with sigma of 0.02
 O3-H3
 0.85 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C26) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
4. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5.a Ternary CH refined with riding coordinates:
 C3(H3C), C14(H14), C17(H17), C20(H20), C25(H25), C3B(H3B), C8B(H8B), C9B(H9B),
  C14B(H14B), C17B(H17B), C20B(H20B), C25B(H25B), C3A(H3A), C8A(H8A), C9A(H9A),
 C14A(H14A), C17A(H17A), C20A(H20A), C25A(H25A)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C9(H9C,H9D), C11(H11E,H11F), C12(H12E,
 H12F), C15(H15E,H15F), C16(H16E,H16F), C22(H22E,H22F), C23(H23E,H23F),
 C24(H24E,H24F), C1B(H1BA,H1BB), C2B(H2BA,H2BB), C4B(H4BA,H4BB), C7B(H7BA,H7BB),
  C11B(H11A,H11B), C12B(H12A,H12B), C15B(H15A,H15B), C16B(H16A,H16B), C22B(H22A,
 H22B), C23B(H23A,H23B), C24B(H24A,H24B), C1A(H1AA,H1AB), C2A(H2AA,H2AB),
 C4A(H4AA,H4AB), C7A(H7AA,H7AB), C11A(H11C,H11D), C12A(H12C,H12D), C15A(H15C,
 H15D), C16A(H16C,H16D), C22A(H22C,H22D), C23A(H23C,H23D), C24A(H24C,H24D)
5.c Aromatic/amide H refined with riding coordinates:
 C6(H6), C7(H7), C6B(H6B), C6A(H6A)
5.d X=CH2 refined with riding coordinates:
 C19(H19G,H19H)
5.e Idealised Me refined as rotating group:
 C18(H18G,H18H,H18I), C21(H21G,H21H,H21I), C26(H26G,H26H,H26I), C27(H27G,H27H,
 H27I), C18B(H18A,H18B,H18C), C19B(H19A,H19B,H19C), C21B(H21A,H21B,H21C),
 C26B(H26A,H26B,H26C), C27B(H27A,H27B,H27C), C18A(H18D,H18E,H18F), C19A(H19D,
 H19E,H19F), C21A(H21D,H21E,H21F), C26A(H26D,H26E,H26F), C27A(H27D,H27E,H27F)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'