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_4515443
_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         'I2, 2(C30 H32 O6)'
_chemical_formula_sum            'C60 H64 I2 O12'
_chemical_formula_weight         1230.91
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2018-06-24
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.18 svn.r3501 for OlexSys, GUI svn.r5488)
;
_cell_angle_alpha                82.119(4)
_cell_angle_beta                 84.605(4)
_cell_angle_gamma                86.509(4)
_cell_formula_units_Z            1
_cell_length_a                   7.9875(15)
_cell_length_b                   11.333(2)
_cell_length_c                   15.342(3)
_cell_measurement_reflns_used    1315
_cell_measurement_temperature    273
_cell_measurement_theta_max      22.762
_cell_measurement_theta_min      2.399
_cell_volume                     1368.0(4)
_computing_cell_refinement       'SAINT v6.45A (Bruker, 2003)'
_computing_data_reduction        'SAINT v6.45A (Bruker, 2003)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      273.0
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_device_type  'CCD Area Detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_unetI/netI     0.1059
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7793
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.82
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.212
_exptl_absorpt_correction_T_max  0.9880
_exptl_absorpt_correction_T_min  0.609369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS v.2.10 (Bruker,2003) was used for absorption correction.
R(int) was 0.0584 before and 0.0294 after correction.
The Ratio of minimum to maximum transmission is 0.6094.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            'clear light gray'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    gray
_exptl_crystal_density_diffrn    1.494
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             626
_exptl_crystal_size_max          0.01
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.336
_refine_diff_density_min         -0.848
_refine_diff_density_rms         0.239
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     340
_refine_ls_number_reflns         5415
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1311
_refine_ls_R_factor_gt           0.0962
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1463P)^2^+13.2792P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2634
_refine_ls_wR_factor_ref         0.2916
_reflns_number_gt                3770
_reflns_number_total             5415
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            am8b20108_si_003.cif
_cod_data_source_block           ca146m
_cod_original_cell_volume        1367.9(5)
_cod_database_code               4515443
_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. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C18(H18A,H18B), C28(H28A,H28B)
3.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C10(H10), C13(H13), C14(H14), C15(H15), C19(H19), C22(H22), C29(H29),
 C33(H33), C1(H1)
3.c Idealised Me refined as rotating group:
 C30(H30A,H30B,H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,
 H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C)
;
_olex2_submission_special_instructions 'No special instructions were received'