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_7122746
_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 Br3 Cd3 Co3 N6 O12 S6, 9(O)'
_chemical_formula_sum            'C36 H60 Br3 Cd3 Co3 N6 O21 S6'
_chemical_formula_weight         1858.98
_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                   11.0674(9)
_cell_length_b                   24.976(2)
_cell_length_c                   22.7050(18)
_cell_measurement_reflns_used    19713
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.64
_cell_measurement_theta_min      3.06
_cell_volume                     6276.1(9)
_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  0.0428
_diffrn_reflns_av_unetI/netI     0.0438
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            24927
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.479
_diffrn_reflns_theta_min         3.062
_diffrn_source                   'Rigaku FR-E SuperBright'
_exptl_absorpt_coefficient_mu    3.952
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.4951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       block
_exptl_crystal_F_000             3648
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.722
_refine_diff_density_min         -0.526
_refine_diff_density_rms         0.087
_refine_ls_abs_structure_details
;
 Flack x determined using 2856 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     355
_refine_ls_number_reflns         7189
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0313
_refine_ls_R_factor_gt           0.0289
_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^)+(0.0385P)^2^+3.2987P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0726
_refine_ls_wR_factor_ref         0.0737
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    0.993
_reflns_Friedel_fraction_max     0.994
_reflns_number_gt                6828
_reflns_number_total             7189
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc09121h2.cif
_cod_data_source_block           D3-1Br
_cod_database_code               7122746
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.505
_shelx_estimated_absorpt_t_max   0.827
_shelx_res_checksum              53838