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_4309897
_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_sum            'C29 H39 B10 Cl2 N3 Ni'
_chemical_formula_weight         667.34
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 111.944(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.558(3)
_cell_length_b                   18.357(4)
_cell_length_c                   16.282(4)
_cell_measurement_reflns_used    245
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      5
_cell_volume                     3481.5(14)
_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 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0359
_diffrn_reflns_av_sigmaI/netI    0.0506
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            21177
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.55
_diffrn_reflns_theta_min         1.75
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.736
_exptl_absorpt_correction_T_max  0.842
_exptl_absorpt_correction_T_min  0.677
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1384
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.258
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         7962
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1042P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1559
_refine_ls_wR_factor_ref         0.1676
_reflns_number_gt                5558
_reflns_number_total             7962
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic051115csi20050705_061607_3.cif
_cod_data_source_block           2b
_cod_database_code               4309897