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_7122745
_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         'C24 H40 Cd2 Cl2 Co2 N4 O9 S4, 14.5(O)'
_chemical_formula_sum            'C24 H71 Cd2 Cl2 Co2 N4 O23.5 S4'
_chemical_formula_weight         1333.64
_space_group_crystal_system      tetragonal
_space_group_IT_number           92
_space_group_name_Hall           'P 4abw 2nw'
_space_group_name_H-M_alt        'P 41 21 2'
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 2'
_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            8
_cell_length_a                   17.911(3)
_cell_length_b                   17.911(3)
_cell_length_c                   31.795(3)
_cell_measurement_reflns_used    32591
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.98
_cell_volume                     10200(3)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0443
_diffrn_reflns_av_unetI/netI     0.0337
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            75431
_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         27.455
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'Rigaku FR-E SuperBright'
_exptl_absorpt_coefficient_mu    1.806
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5754
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.737
_exptl_crystal_description       block
_exptl_crystal_F_000             5432
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.591
_refine_diff_density_min         -0.550
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details
;
 Flack x determined using 4428 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         11652
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0449
_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^)+(0.0721P)^2^+13.4765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1239
_refine_ls_wR_factor_ref         0.1261
_reflns_Friedel_coverage         0.778
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                11068
_reflns_number_total             11652
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09121h2.cif
_cod_data_source_block           CdCl(Co(D-ebp))n
_cod_original_cell_volume        10199(4)
_cod_original_formula_sum        'C24 H71 Cd2 Cl2 Co2 N4 O23.50 S4'
_cod_database_code               7122745
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.840
_shelx_estimated_absorpt_t_max   0.840
_shelx_res_checksum              95886