Oxidative Addition of N-H Bonds to a Metal Center: Synthesis, Characterization, and Crystal Structure of New Rhodium(III) Hydrido-Pyrazolate Complexes
G. Attilio Ardizzoia; Stefano Brenna; Girolamo LaMonica; Angelo Maspero; Norberto Masciocchi; Massimo Moret; Inorganic Chemistry 41 (2002) 610–614; doi:10.1021/ic010852f

data_4317504
_publ_section_title
;
 Oxidative Addition of N-H Bonds to a Metal Center: Synthesis,
 Characterization, and Crystal Structure of New Rhodium(III)
 Hydrido-Pyrazolate Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              610
_journal_page_last               614
_journal_paper_doi               10.1021/ic010852f
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C92 H90 N12 O8 P4 Rh2'
_chemical_formula_weight         1821.46
_chemical_name_systematic
;
?
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ab'
_symmetry_space_group_name_H-M   'P b n 21'
_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                   12.537(2)
_cell_length_b                   18.113(3)
_cell_length_c                   38.231(6)
_cell_measurement_temperature    293(2)
_cell_volume                     8682(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.511
_diffrn_measured_fraction_theta_max 0.511
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0434
_diffrn_reflns_av_sigmaI/netI    0.0559
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            18362
_diffrn_reflns_theta_full        24.95
_diffrn_reflns_theta_max         24.95
_diffrn_reflns_theta_min         2.24
_exptl_absorpt_coefficient_mu    0.517
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3760
_refine_diff_density_max         0.717
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.064
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.33(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.124
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1064
_refine_ls_number_reflns         6752
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.124
_refine_ls_R_factor_all          0.0472
_refine_ls_R_factor_gt           0.0472
_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^)+(0.0492P)^2^+0.4758P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0896
_refine_ls_wR_factor_ref         0.0896
_reflns_number_gt                6752
_reflns_number_total             6752
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010852f.cif
_cod_data_source_block           aa982
_cod_database_code               4317504