Preparation of a rhodium(iii) cis-diaquacomplex by protic acid induced oxalate-release from mer-[Rh(C2O4)Cl(py)3]
Vasilchenko, Danila; Tkachev, Sergey; Baidina, Iraida; Korolkov, Ilya; Berdyugin, Semen; Kozlova, Ekaterina; Kozlov, Denis; New Journal of Chemistry 42 (2018) 19637–; doi:10.1039/C8NJ04264K

data_7057925
_publ_section_title
;
 Preparation of a rhodium(iii) cis-diaquacomplex by protic acid induced
 oxalate-release from mer-[Rh(C2O4)Cl(py)3]
;
_journal_issue                   24
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              19637
_journal_paper_doi               10.1039/C8NJ04264K
_journal_volume                  42
_journal_year                    2018
_chemical_formula_sum            'C17 H15 Cl N3 O4 Rh'
_chemical_formula_weight         463.68
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/4
_audit_update_record
;
2018-10-22 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.9999(6)
_cell_length_b                   12.0930(7)
_cell_length_c                   14.9368(8)
_cell_measurement_reflns_used    9895
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.17
_cell_volume                     1806.29(18)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/4 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Apex DUO'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0297
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            31362
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.601
_diffrn_reflns_theta_min         2.167
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.121
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_description       stick
_exptl_crystal_F_000             928
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_min          0.100
_exptl_transmission_factor_max   0.8962
_exptl_transmission_factor_min   0.7747
_refine_diff_density_max         1.592
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 2022 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.018(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         5538
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0284
_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^)+(0.0395P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0654
_refine_ls_wR_factor_ref         0.0683
_reflns_Friedel_coverage         0.774
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.993
_reflns_number_gt                4941
_reflns_number_total             5538
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04264k2.cif
_cod_data_source_block           publication_text
_cod_depositor_comments
'Adding full bibliography for 7057925--7057926.cif.'
_cod_database_code               7057925
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_min   0.775
_shelx_estimated_absorpt_t_max   0.896
_shelx_res_checksum              70516
_shelx_hkl_checksum              6631