Synthesis, Structure, and Hydrothiolation Activity of Rhodium Pyrazolylborate Complexes
Fraser, Lauren R.; Bird, Jeffrey; Wu, Qiming; Cao, Changsheng; Patrick, Brian O.; Love, Jennifer A.; Organometallics 26 (2007) 5602–; doi:10.1021/om700564t

data_4073706
_publ_section_title
;
 Synthesis, Structure, and Hydrothiolation Activity of Rhodium
 Pyrazolylborate Complexes
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              5602
_journal_paper_doi               10.1021/om700564t
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C68 H64 B N6 P2 Rh'
_chemical_formula_weight         1140.91
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 107.914(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.4909(9)
_cell_length_b                   18.5240(10)
_cell_length_c                   18.5170(10)
_cell_measurement_reflns_used    7821
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.84
_cell_measurement_theta_min      2.48
_cell_volume                     5708.7(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker X8 APEX II'
_diffrn_measurement_method       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            59783
_diffrn_reflns_theta_full        27.98
_diffrn_reflns_theta_max         27.98
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.403
_exptl_absorpt_correction_T_max  0.986
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       irregular
_exptl_crystal_F_000             2376
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.824
_refine_diff_density_min         -0.554
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     701
_refine_ls_number_reflns         13758
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0533
_refine_ls_R_factor_gt           0.0366
_refine_ls_shift/su_max          0.370
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0396P)^2^+4.0370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0931
_reflns_number_gt                10811
_reflns_number_total             13758
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om700564t-file003.cif
_cod_data_source_block           jl033
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4073706