Semi-Rigid Molecular-Clip-Based Molecular Crystal Gearshift.
Wu, Jia-Rui; Li, Bao; Zhang, Jiang-Wei; Yang, Ying-Wei; ACS applied materials & interfaces 11 (2019) 998–1003; doi:10.1021/acsami.8b20108

data_4515445
_publ_section_title
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 Semi-Rigid Molecular-Clip-Based Molecular Crystal Gearshift.
;
_journal_issue                   1
_journal_name_full               'ACS applied materials &amp; interfaces'
_journal_page_first              998
_journal_page_last               1003
_journal_paper_doi               10.1021/acsami.8b20108
_journal_volume                  11
_journal_year                    2019
_chemical_formula_moiety         'C30 H32 O6, 2(H2 O)'
_chemical_formula_sum            'C30 H36 O8'
_chemical_formula_weight         524.59
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-06-29
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 109.243(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4791(17)
_cell_length_b                   13.0125(13)
_cell_length_c                   16.8365(17)
_cell_measurement_reflns_used    8936
_cell_measurement_temperature    196(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.95
_cell_volume                     2994.9(6)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      196.4
_diffrn_detector_area_resol_mean 16.0971
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0682
_diffrn_reflns_av_unetI/netI     0.0572
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29456
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.499
_diffrn_reflns_theta_min         2.953
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.084
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.980
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            ad
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.416
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.160
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         6031
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.160
_refine_ls_R_factor_all          0.1009
_refine_ls_R_factor_gt           0.0717
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1424
_refine_ls_wR_factor_ref         0.1824
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3544
_reflns_number_total             6031
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            am8b20108_si_004.cif
_cod_data_source_block           dmo
_cod_database_code               4515445
_shelx_shelxl_version_number     2018/3
_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, All O(H,H) groups
2. Restrained distances
 O17-O18
 2.5 with sigma of 0.02
3.a Free rotating group:
 O17(H17A,H17B), O18(H18A,H18B)
3.b Secondary CH2 refined with riding coordinates:
 C12(H12A,H12B), C11(H11A,H11B)
3.c Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C17(H17), C5(H5), C15(H15), C3(H3), C1(H1), C26(H26), C2(H2),
 C24(H24)
3.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C28(H28A,H28B,H28C), C19(H19A,H19B,
 H19C), C29(H29A,H29B,H29C), C30(H30A,H30B,H30C)
;