Pyrazolato-Bridged Dinuclear Complexes of Ruthenium(II) and Rhodium(III) with N-Heterocyclic Carbene Ligands: Synthesis, Characterization, and Electrochemical Properties
Reindl, Stefan A.; Pöthig, Alexander; Drees, Markus; Bechlars, Bettina; Herdtweck, Eberhardt; Herrmann, Wolfgang A.; Kühn, Fritz E.; Organometallics 32 (2013) 4082–; doi:10.1021/om400106f

data_4080924
_publ_section_title
;
 Pyrazolato-Bridged Dinuclear Complexes of Ruthenium(II) and Rhodium(III)
 with N-Heterocyclic Carbene Ligands: Synthesis, Characterization, and
 Electrochemical Properties
;
_journal_issue                   15
_journal_name_full               Organometallics
_journal_page_first              4082
_journal_paper_doi               10.1021/om400106f
_journal_volume                  32
_journal_year                    2013
_chemical_formula_moiety         'C33 H47 Cl3 N6 Rh2, 2(F6 P)'
_chemical_formula_sum            'C33 H47 Cl3 F12 N6 P2 Rh2'
_chemical_formula_weight         1129.88
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 114.723(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.8183(12)
_cell_length_b                   8.8631(4)
_cell_length_c                   22.7017(11)
_cell_measurement_reflns_used    9951
_cell_measurement_temperature    123
_cell_measurement_theta_max      25.3477
_cell_measurement_theta_min      2.4692
_cell_volume                     4535.9(4)
_computing_cell_refinement       'SAINT (Bruker, 2008b)'
_computing_data_collection       'APEX II Control Software (Bruker, 2008a)'
_computing_data_reduction        'SAINT (Bruker, 2008b)'
_computing_molecular_graphics    'PLATON (Spek, 2011)'
_computing_publication_material  'PLATON (Spek, 2011), enCIFer (Allen, 2004)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      123
_diffrn_detector                 ' CCD plate '
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       ' \k-geometry diffractometer '
_diffrn_measurement_device_type  ' Bruker APEX-II CCD '
_diffrn_measurement_method       ' phi- and omega-rotation '
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'rotating anode FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0426
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44055
_diffrn_reflns_reduction_process
;
;
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.056
_exptl_absorpt_correction_T_max  0.831
_exptl_absorpt_correction_T_min  0.519
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker, 2008b'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.655
_exptl_crystal_density_method    'Not Measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2264
_exptl_crystal_size_max          0.710
_exptl_crystal_size_mid          0.420
_exptl_crystal_size_min          0.180
_platon_squeeze_details
;
The unit cell contains 3 acetonitrile molecules which have been treated as a 
diffuse contribution to the overall scattering without specific atom positions 
by SQUEEZE/PLATON.
;
_refine_diff_density_max         0.781
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     269
_refine_ls_number_reflns         4145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.091
_refine_ls_R_factor_all          0.0295
_refine_ls_R_factor_gt           0.0287
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0485P)^2^+12.9982P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0835
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                3994
_reflns_number_total             4145
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om400106f_si_002.cif
_cod_data_source_block           Compound_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4080924