Formation of Triniobocene Cationic and Neutral Mononiobocene Species as a Function of Solvent in the Reaction of Cp2Nb{(μ-H)2BR2} (R2= C4H8, C5H10, C8H14) with B(C6F5)3
Liu, Shengming; Liu, Fu-Chen; Renkes, Gordon; Shore, Sheldon G.; Organometallics 20 (2001) 5717–; doi:10.1021/om0107744

data_4077446
_publ_section_title
;
 Formation of Triniobocene Cationic and Neutral Mononiobocene Species as a
 Function of Solvent in the Reaction of Cp2Nb{(\m-H)2BR2} (R2= C4H8,
 C5H10, C8H14) with B(C6F5)3
;
_journal_issue                   26
_journal_name_full               Organometallics
_journal_page_first              5717
_journal_paper_doi               10.1021/om0107744
_journal_volume                  20
_journal_year                    2001
_chemical_formula_sum            'C28 H10 B F15 Nb'
_chemical_formula_weight         735.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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            8
_cell_length_a                   15.5363(10)
_cell_length_b                   16.0828(10)
_cell_length_c                   19.6394(10)
_cell_measurement_reflns_used    '10 frames'
_cell_measurement_temperature    203(2)
_cell_volume                     4907.2(5)
_computing_cell_refinement       'DENZO (Oywinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Oywinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w at 55/-55'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0280
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            20429
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.626
_exptl_absorpt_correction_T_max  0.8108
_exptl_absorpt_correction_T_min  0.7970
_exptl_absorpt_correction_type   'SORTAV (blessing, 1995)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.990
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             2872
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.319
_refine_diff_density_min         -0.329
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         4339
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0379
_refine_ls_R_factor_gt           0.0271
_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^)+(0.0309P)^2^+3.1926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0641
_refine_ls_wR_factor_ref         0.0683
_reflns_number_gt                3599
_reflns_number_total             4339
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0107744.cif
_cod_data_source_block           Compound2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               4077446