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_7121557
_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), 12(H2 O)'
_chemical_formula_sum            'C39 H123 N18 O28 Rh5 S15 Zn4'
_chemical_formula_weight         2549.48
_space_group_crystal_system      trigonal
_space_group_IT_number           146
_space_group_name_Hall           'R 3'
_space_group_name_H-M_alt        'R 3 :H'
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            3
_cell_length_a                   20.2090(3)
_cell_length_b                   20.2090(3)
_cell_length_c                   21.1201(4)
_cell_measurement_reflns_used    22414
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.164
_cell_measurement_theta_min      2.552
_cell_volume                     7469.9(2)
_computing_cell_refinement       HKL3000
_computing_data_collection       PAL_ADSC_Quantum-210_ADX_Program
_computing_data_reduction        HKL3000
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.597
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  'Si(111) double crystal monochromator'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.600
_diffrn_reflns_av_R_equivalents  0.0320
_diffrn_reflns_av_unetI/netI     0.0401
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.597
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            22414
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.571
_diffrn_reflns_theta_full        21.100
_diffrn_reflns_theta_max         29.164
_diffrn_reflns_theta_min         2.552
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.9233
_exptl_absorpt_correction_T_min  0.8956
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
[c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.700
_exptl_crystal_description       block
_exptl_crystal_F_000             3876
_exptl_crystal_size_max          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.060
_refine_diff_density_max         1.134
_refine_diff_density_min         -1.379
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 2201 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.062(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         8525
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1161
_refine_ls_R_factor_gt           0.0908
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2667
_refine_ls_wR_factor_ref         0.2922
_reflns_Friedel_coverage         0.915
_reflns_Friedel_fraction_full    0.991
_reflns_Friedel_fraction_max     0.546
_reflns_number_gt                5505
_reflns_number_total             8525
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc02619j2.cif
_cod_data_source_block           3
_cod_depositor_comments
'Adding full bibliography for 7121557--7121558.cif.'
_cod_original_cell_volume        7469.9(3)
_cod_database_code               7121557
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.901
_shelx_estimated_absorpt_t_max   0.924
_shelx_res_checksum              45562