Two-step chiral transfer from d-penicillamine to metallosupramolecular ionic crystals.
Yasukawa, Yuhei; Yoshinari, Nobuto; Konno, Takumi; Chemical communications (Cambridge, England) 54 (2018) 5003–5006; doi:10.1039/c8cc02619j

data_7121558
_publ_section_title
;
 Two-step chiral transfer from d-penicillamine to metallosupramolecular
 ionic crystals.
;
_journal_issue                   39
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              5003
_journal_page_last               5006
_journal_paper_doi               10.1039/c8cc02619j
_journal_volume                  54
_journal_year                    2018
_chemical_absolute_configuration rm
_chemical_formula_moiety
'C24 H72 N12 O Rh4 S12 Zn4, C15 H27 N3 O6 Rh S3, 3(N O3), 20(H2 O)'
_chemical_formula_sum            'C39 H139 N18 O36 Rh5 S15 Zn4'
_chemical_formula_weight         2693.60
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-04-23 downloaded from the CCDC.
;
_cell_angle_alpha                95.771(15)
_cell_angle_beta                 94.901(10)
_cell_angle_gamma                96.534(16)
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_cell_length_b                   13.782(10)
_cell_length_c                   14.450(10)
_cell_measurement_reflns_used    331
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      18.61
_cell_measurement_theta_min      3.11
_cell_volume                     2601(3)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.987
_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  0.0300
_diffrn_reflns_av_unetI/netI     0.0915
_diffrn_reflns_Laue_measured_fraction_full 0.995
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_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            20849
_diffrn_reflns_point_group_measured_fraction_full 0.821
_diffrn_reflns_point_group_measured_fraction_max 0.781
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.485
_diffrn_reflns_theta_min         3.066
_exptl_absorpt_coefficient_mu    2.054
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.719
_exptl_crystal_description       block
_exptl_crystal_F_000             1372
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
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_refine_diff_density_max         1.263
_refine_diff_density_min         -1.551
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_refine_ls_abs_structure_details
;
 Flack x determined using 3939 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.053(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         18623
_refine_ls_number_restraints     53
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1196
_refine_ls_R_factor_gt           0.0850
_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^)+(0.1260P)^2^+11.6685P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2126
_refine_ls_wR_factor_ref         0.2410
_reflns_Friedel_coverage         0.582
_reflns_Friedel_fraction_full    0.648
_reflns_Friedel_fraction_max     0.574
_reflns_number_gt                13233
_reflns_number_total             18623
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02619j2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7121557--7121558.cif.'
_cod_original_cell_volume        2602(3)
_cod_database_code               7121558
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.821
_shelx_estimated_absorpt_t_max   0.821
_shelx_res_checksum              45234