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_7057926
_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_moiety         'C15 H19 Cl N3 O2 Rh, 2(Cl O4), H2 O'
_chemical_formula_sum            'C15 H21 Cl3 N3 O11 Rh'
_chemical_formula_weight         628.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   mixed
_audit_creation_date             2018-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-10-27 deposited with the CCDC.
2018-11-07 downloaded from the CCDC.
;
_cell_angle_alpha                105.068(4)
_cell_angle_beta                 103.546(4)
_cell_angle_gamma                104.836(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9296(11)
_cell_length_b                   11.0733(14)
_cell_length_c                   12.0046(15)
_cell_measurement_reflns_used    5125
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      2.23
_cell_measurement_theta_min      29.25
_cell_volume                     1166.4(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150.15
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0492
_diffrn_reflns_av_unetI/netI     0.0615
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23552
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         30.682
_diffrn_reflns_theta_min         1.856
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  0.9247
_exptl_absorpt_correction_T_min  0.8571
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.790
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.07
_refine_diff_density_max         2.691
_refine_diff_density_min         -1.988
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     298
_refine_ls_number_reflns         7206
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_gt           0.0497
_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^)+(0.0557P)^2^+1.6696P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1220
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5623
_reflns_number_total             7206
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8nj04264k2.cif
_cod_data_source_block           h
_cod_depositor_comments
'Adding full bibliography for 7057925--7057926.cif.'
_cod_original_cell_volume        1166.4(2)
_cod_database_code               7057926
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.925
_shelx_estimated_absorpt_t_min   0.857
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All O(H,H) groups
2. Restrained distances
 H1WA-H1WB
 1.65 with sigma of 0.05
 H2A-H2B
 1.65 with sigma of 0.05
 H1A-H1B
 1.65 with sigma of 0.05
3.a Riding coordinates:
 O1(H1A,H1B), O2(H2A,H2B), O1W(H1WA,H1WB)
3.b Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C21(H21), C22(H22),
 C23(H23), C24(H24), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34), C35(H35)
;
_shelx_res_checksum              58425
_shelx_hkl_checksum              64372
_olex2_submission_special_instructions 'No special instructions were received'