Synthesis of Nickel-Monocarbollide Complexes by Oxidative Insertion
Thomas D. McGrath; Andreas Franken; Jason A. Kautz; F. Gordon A. Stone; Inorganic Chemistry 44 (2005) 8135–8144; doi:10.1021/ic051115c

data_4309895
_publ_contact_author_address
; Department of Chemistry and Biochemistry
  Baylor University
  PO Box 97348
  Waco
  TX, 76798-7348
  USA
;
_publ_contact_author_email       Gordon_Stone@baylor.edu
_publ_contact_author_fax         '+1 254 710 2403'
_publ_contact_author_name        'Prof. F. Gordon A. Stone'
_publ_contact_author_phone       '+1 254 710 4427'
_publ_section_title
;
Synthesis of Nickel-Monocarbollide Complexes by Oxidative Insertion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8135
_journal_page_last               8144
_journal_paper_doi               10.1021/ic051115c
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C23 H32 B10 N Ni O P  C0.50 H Cl '
_chemical_formula_sum            'C23.5 H33 B10 Cl N Ni O P'
_chemical_formula_weight         578.74
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                100.440(9)
_cell_angle_beta                 97.678(18)
_cell_angle_gamma                107.274(10)
_cell_formula_units_Z            2
_cell_length_a                   9.7282(15)
_cell_length_b                   12.0324(16)
_cell_length_c                   13.360(3)
_cell_measurement_reflns_used    236
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     1439.0(5)
_computing_cell_refinement       'SAINT (Siemens, 1995)'
_computing_data_collection       'SMART (Siemens, 1995)'
_computing_data_reduction        'SAINT (Siemens, 1995)'
_computing_molecular_graphics    'SHELXTL (Siemens, 1995)'
_computing_publication_material  'SHELXTL (Siemens, 1995)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 60
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type
'Siemens SMART CCD area detector diffractometer'
_diffrn_measurement_method       '\w rotation with narrow frames'
_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  0.0369
_diffrn_reflns_av_sigmaI/netI    0.0666
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_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            14377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.82
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.843
_exptl_absorpt_correction_T_max  0.928
_exptl_absorpt_correction_T_min  0.795
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             598
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.705
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.947
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         6514
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0734
_refine_ls_R_factor_gt           0.0424
_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^)+(0.0549P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0968
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                4465
_reflns_number_total             6514
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051115csi20050705_061607_1.cif
_cod_data_source_block           5c
_cod_original_cell_volume        1439.0(4)
_cod_original_formula_sum        'C23.50 H33 B10 Cl N Ni O P'
_cod_database_code               4309895