Conversion of 12-Membered D3- and L3-CoIII3CdII3 Metallorings into a 24-Membered D3L3-CoIII6CdII6 Metalloring
Hayashi, Daiki; Yoshinari, Nobuto; Konno, Takumi; Chemical Communications  (2018) –; doi:10.1039/C8CC09121H

data_7122744
_publ_section_title
;
 Conversion of 12-Membered D3- and L3-CoIII3CdII3 Metallorings into a
 24-Membered D3L3-CoIII6CdII6 Metalloring
;
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C8CC09121H
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H60 Cd3 Co3 I3 N6 O12 S6, 9(O)'
_chemical_formula_sum            'C36 H60 Cd3 Co3 I3 N6 O21 S6'
_chemical_formula_weight         1999.95
_space_group_crystal_system      orthorhombic
_space_group_IT_number           20
_space_group_name_Hall           'C 2c 2'
_space_group_name_H-M_alt        'C 2 2 21'
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-11-16 deposited with the CCDC.
2018-12-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.2149(7)
_cell_length_b                   25.0212(15)
_cell_length_c                   22.9649(16)
_cell_measurement_reflns_used    21850
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      3.04
_cell_volume                     6444.2(7)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'Mercury 3.10'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku R-AXIS VII'
_diffrn_measurement_method       \w
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0267
_diffrn_reflns_av_unetI/netI     0.0247
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25665
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.044
_diffrn_source                   'Rigaku FR-E SuperBright'
_exptl_absorpt_coefficient_mu    3.427
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7481
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    2.061
_exptl_crystal_description       block
_exptl_crystal_F_000             3864
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.030
_refine_diff_density_max         2.648
_refine_diff_density_min         -2.144
_refine_diff_density_rms         0.111
_refine_ls_abs_structure_details
;
 Flack x determined using 3128 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     346
_refine_ls_number_reflns         7380
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0317
_refine_ls_R_factor_gt           0.0310
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0298P)^2^+33.1997P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0744
_refine_ls_wR_factor_ref         0.0749
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.995
_reflns_number_gt                7241
_reflns_number_total             7380
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09121h2.cif
_cod_data_source_block           L3-1I
_cod_database_code               7122744
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.726
_shelx_estimated_absorpt_t_max   0.904
_shelx_res_checksum              53984