Self-Assembled Molecular Gear: A 4:1 Complex of Rh(III)Cl Tetraarylporphyrin and Tetra(p-pyridyl)cavitand.
Nakamura, Munechika; Kishimoto, Kazuki; Kobori, Yasuhiro; Abe, Tomoka; Yoza, Kenji; Kobayashi, Kenji; Journal of the American Chemical Society 138 (2016) 12564–12577; doi:10.1021/jacs.6b07284

data_4130833
_publ_section_title
;
 Self-Assembled Molecular Gear: A 4:1 Complex of Rh(III)Cl
 Tetraarylporphyrin and Tetra(p-pyridyl)cavitand.
;
_journal_issue                   38
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12564
_journal_page_last               12577
_journal_paper_doi               10.1021/jacs.6b07284
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C67.5 H55.5 Cl8.5 N5 O3.25 Rh'
_chemical_formula_weight         1392.90
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.0036(9)
_cell_length_b                   25.0036(9)
_cell_length_c                   23.9683(8)
_cell_measurement_temperature    100
_cell_volume                     14984.5(9)
_computing_cell_refinement       'APEX2 v2014.9 (Bruker AXS)'
_computing_data_collection
'Bruker Instrument Service V4.2.2 (Bruker AXS Inc., 2014)'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_molecular_graphics    'XSHELL V6.3.1 (Bruker AXS Inc., 2004)'
_computing_publication_material
'Generate Report V2014.1 (Bruker AXS Inc., 2014)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT (Sheldrick, 2013)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker D8 goniometer'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multilayered conforcal mirror'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0521
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            51713
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.304
_diffrn_source                   'micro focus sealed tube'
_diffrn_source_type              'INCOATEC I\mS'
_exptl_absorpt_coefficient_mu    0.575
_exptl_absorpt_correction_T_max  0.961
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       plate
_exptl_crystal_F_000             5688
_exptl_crystal_size_max          0.272
_exptl_crystal_size_mid          0.152
_exptl_crystal_size_min          0.069
_refine_diff_density_max         1.546
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.160
_refine_ls_abs_structure_details
;
 Flack x determined using 4612 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     853
_refine_ls_number_reflns         13248
_refine_ls_number_restraints     1507
_refine_ls_restrained_S_all      1.109
_refine_ls_R_factor_all          0.1006
_refine_ls_R_factor_gt           0.0837
_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^)+(0.1569P)^2^+91.5361P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2300
_refine_ls_wR_factor_ref         0.2459
_reflns_Friedel_coverage         0.949
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                11021
_reflns_number_total             13248
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b07284_si_002.cif
_cod_data_source_block           b
_cod_original_cell_volume        14984.5(12)
_cod_original_formula_sum        'C67.50 H55.50 Cl8.50 N5 O3.25 Rh'
_cod_database_code               4130833
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.859
_shelx_estimated_absorpt_t_max   0.961
_shelx_res_checksum              7310
_shelx_hkl_checksum              5746