Toward Unidirectional Rotary Motion in Nickelacarboranes: Characterization of Diastereomeric Nickel Bis(Dicarbollide) Complexes Derived from the [Nido-7-CH3-7,8-C2B9H11]- Anion
Robert D. Kennedy; Carolyn B. Knobler; M. Frederick Hawthorne; Inorganic Chemistry 48 (2009) 9377–9384; doi:10.1021/ic901175e

data_4303283
_publ_contact_author
; 
  Hawthorne, M. F.,
  Department of Chemistry and Biochemistry,
  University of California,
  Los Angeles, CA 90095-1569.  USA
;
_publ_contact_author_email       hawthornem@missouri.edu
_publ_contact_author_fax         573-884-6900
_publ_contact_author_phone       573-882-7016
_publ_section_title
;
Toward Unidirectional Rotary Motion in Nickelacarboranes: Characterization
of Diastereomeric Nickel Bis(Dicarbollide) Complexes Derived from the
[Nido-7-CH3-7,8-C2B9H11]- Anion
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9377
_journal_page_last               9384
_journal_paper_doi               10.1021/ic901175e
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C4 H22 B18 Ni, C4 H12 N'
_chemical_formula_sum            'C8 H34 B18 N Ni'
_chemical_formula_weight         397.65
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                   9.8187(7)
_cell_length_b                   10.3706(7)
_cell_length_c                   21.8015(15)
_cell_measurement_reflns_used    4109
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.20
_cell_measurement_theta_min      2.86
_cell_volume                     2220.0(3)
_computing_cell_refinement       'Bruker SMART 1000 software'
_computing_data_collection       'Bruker SMART 1000 software'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0275
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            6842
_diffrn_reflns_theta_full        28.27
_diffrn_reflns_theta_max         28.27
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.190
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.299
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     88
_refine_ls_number_reflns         1470
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0311
_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^)+(0.0643P)^2^+0.5365P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0925
_refine_ls_wR_factor_ref         0.0956
_reflns_number_gt                1227
_reflns_number_total             1470
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901175e_si_002_2.cif
_cod_data_source_block           rkni3dlmn
_cod_database_code               4303283