Assembled structures of tetrakis(biimidazole)dirhodium complexes hydrogen-bonded with common inorganic anions
Jin-Long; Uemura, Kazuhiro; Ebihara, Masahiro; Acta Crystallographica Section B 70 (2014) 1006–1019; doi:10.1107/S2052520614021428

data_2105971
_publ_section_title
;
 Assembled structures of tetrakis(biimidazole)dirhodium complexes
 hydrogen-bonded with common inorganic anions
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section B'
_journal_page_first              1006
_journal_page_last               1019
_journal_paper_doi               10.1107/S2052520614021428
_journal_volume                  70
_journal_year                    2014
_chemical_formula_moiety
'C60 H60 N38 Rh4, Si F6,  6(Cl O4), 12.7(H2 O)'
_chemical_formula_sum            'C60 H85.4 Cl6 F6 N38 O36.7 Rh4 Si'
_chemical_formula_weight         2692.69
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.170(2)
_cell_length_b                   21.875(3)
_cell_length_c                   22.541(3)
_cell_measurement_reflns_used    25234
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.4816
_cell_measurement_theta_min      3.2963
_cell_volume                     9946(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection
'CrystalClear (Molecular Structure Corporation & Rigaku Corporation, 2001)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material
'Yadokari-XG 2009 (Wakita, Nemoto et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0351
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            71587
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.29
_diffrn_source                   'rotating-anode X-ray tube'
_exptl_absorpt_coefficient_mu    0.938
_exptl_absorpt_correction_T_max  0.8941
_exptl_absorpt_correction_T_min  0.8316
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'NUMABS (Higashi, 1999)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.777
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             5420
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.648
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         11379
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.170
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0594
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0782P)^2^+29.1806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1555
_refine_ls_wR_factor_ref         0.1800
_reflns_number_gt                10339
_reflns_number_total             11352
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ry5061sup1.cif
_cod_data_source_block           VI
_cod_original_sg_symbol_H-M      Pbca
_cod_original_formula_sum        'C60 H85.40 Cl6 F6 N38 O36.70 Rh4 Si'
_cod_database_code               2105971
_publcif_datablock.id            {071fb849-d75e-4493-9690-073d25f41f23}