Hydrogen-bonded metallosupramolecular helices composed of a nona-protonated spherical RhIII4ZnII4 cluster with twelve carboxylate arms
Yamashita, Ukyo; Yoshinari, Nobuto; Sodkhomkhum, Rapheepraew; Meundaeng, Natthaya; Konno, Takumi; CrystEngComm  (2020) –; doi:10.1039/D0CE00133C

data_7239963
_publ_section_title
;
 Hydrogen-bonded metallosupramolecular helices composed of a
 nona-protonated spherical RhIII4ZnII4 cluster with twelve carboxylate
 arms
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00133C
_journal_year                    2020
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C36 H69 N12 O25 Rh4 S12 Zn4, 3(Br),  29(O)'
_chemical_formula_sum            'C36 H69 Br3 N12 O54 Rh4 S12 Zn4'
_chemical_formula_weight         2831.60
_space_group_crystal_system      hexagonal
_space_group_IT_number           179
_space_group_name_Hall           'P 65 2 (0 0 1)'
_space_group_name_H-M_alt        'P 65 2 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2019-12-27 deposited with the CCDC.	2020-02-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   27.8380(16)
_cell_length_b                   27.8380(16)
_cell_length_c                   28.8132(8)
_cell_measurement_reflns_used    166622
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      16.05
_cell_measurement_theta_min      0.51
_cell_volume                     19337.4(17)
_computing_cell_refinement       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_collection       'RAPID-AUTO (Rigaku Corporation)'
_computing_data_reduction        'RAPID-AUTO (Rigaku Corporation)'
_computing_molecular_graphics
'Yadokari-XG 2009 (Wakita Nemoto et al., 2009)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 14.69
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Mercury2CCD detector'
_diffrn_measurement_method       /w
_diffrn_radiation_monochromator  Si(311)
_diffrn_radiation_source         'SPring-8 BL02B1 bending magnet'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.4248
_diffrn_reflns_av_R_equivalents  0.2236
_diffrn_reflns_av_unetI/netI     0.0908
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            315659
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        14.766
_diffrn_reflns_theta_max         16.012
_diffrn_reflns_theta_min         0.505
_exptl_absorpt_coefficient_mu    1.232
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.5048
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.459
_exptl_crystal_description       needle
_exptl_crystal_F_000             8388
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.751
_refine_diff_density_rms         0.090
_refine_ls_abs_structure_details
;
 Flack x determined using 3311 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.035(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.854
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     614
_refine_ls_number_reflns         14801
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      0.857
_refine_ls_R_factor_all          0.0669
_refine_ls_R_factor_gt           0.0428
_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^)+(0.0459P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0952
_refine_ls_wR_factor_ref         0.1012
_reflns_Friedel_coverage         0.793
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9800
_reflns_number_total             14801
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0ce00133c2.cif
_cod_data_source_block           2
_cod_original_cell_volume        19337(2)
_cod_database_code               7239963
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              88326
_shelx_fab_checksum              96338