Compression of a Flapping Mechanophore Accompanied by Thermal Void Collapse in a Crystalline Phase.
Yamakado, Takuya; Otsubo, Kazuya; Osuka, Atsuhiro; Saito, Shohei; Journal of the American Chemical Society 140 (2018) 6245–6248; doi:10.1021/jacs.8b03833

data_4132424
_publ_section_title
;
 Compression of a Flapping Mechanophore Accompanied by Thermal Void
 Collapse in a Crystalline Phase.
;
_journal_issue                   20
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6245
_journal_page_last               6248
_journal_paper_doi               10.1021/jacs.8b03833
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C52 H52 Si4, 0.3(C H2 Cl2)'
_chemical_formula_sum            'C52.3 H52.6 Cl0.6 Si4'
_chemical_formula_weight         814.77
_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
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                106.0212(17)
_cell_angle_beta                 92.4568(18)
_cell_angle_gamma                96.7633(18)
_cell_formula_units_Z            2
_cell_length_a                   9.7656(11)
_cell_length_b                   16.3229(17)
_cell_length_c                   16.4044(17)
_cell_measurement_reflns_used    5143
_cell_measurement_temperature    90
_cell_measurement_theta_max      28.31
_cell_measurement_theta_min      2.33
_cell_volume                     2488.1(5)
_computing_cell_refinement       'APEX2 (Bruker AXS, 2006)'
_computing_data_collection       'APEX2 (Bruker AXS, 2006)'
_computing_data_reduction        'SAINT (Bruker AXS, 2004)'
_computing_molecular_graphics    'XSHEL (Bruker AXS,2002)'
_computing_publication_material  'XCIF (Bruker AXS, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.972
_diffrn_measurement_device_type  'Bruker APEXII CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_unetI/netI     0.0465
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.972
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17157
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.972
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.504
_diffrn_reflns_theta_min         1.310
_exptl_absorpt_coefficient_mu    0.183
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.889
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.088
_exptl_crystal_description       prism
_exptl_crystal_F_000             865
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.402
_refine_diff_density_min         -0.407
_refine_diff_density_rms         0.051
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     561
_refine_ls_number_reflns         12233
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0526
_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^)+(0.0408P)^2^+1.7492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1142
_refine_ls_wR_factor_ref         0.1263
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9085
_reflns_number_total             12233
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b03833_si_007.cif
_cod_data_source_block           71107TY_0m_a
_cod_original_formula_sum        'C52.30 H52.60 Cl0.60 Si4'
_cod_database_code               4132424
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.964
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              98586
_shelx_hkl_checksum              4403