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_4077445
_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            'C74 H45 B2 F25 Nb3'
_chemical_formula_weight         1709.45
_chemical_name_common            'triniobocene cation'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 98.857(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.5356(10)
_cell_length_b                   13.2679(10)
_cell_length_c                   51.3778(10)
_cell_measurement_reflns_used    '10 frames'
_cell_measurement_temperature    173(2)
_cell_volume                     13158.1(13)
_computing_cell_refinement       'DENZO (Otwinowsky & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowsky & Minor, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'omega 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  0.0919
_diffrn_reflns_av_sigmaI/netI    0.0746
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            40509
_diffrn_reflns_theta_full        25.06
_diffrn_reflns_theta_max         25.06
_diffrn_reflns_theta_min         2.30
_exptl_absorpt_coefficient_mu    0.630
_exptl_absorpt_correction_T_max  0.9114
_exptl_absorpt_correction_T_min  0.8896
_exptl_absorpt_correction_type   'SORTAV (blessing, 1995)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       chunk
_exptl_crystal_F_000             6776
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.720
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     952
_refine_ls_number_reflns         11582
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.1114
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          3.143
_refine_ls_shift/su_mean         0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+55.2067P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1205
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                7278
_reflns_number_total             11582
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0107744.cif
_cod_data_source_block           Compound1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_cell_volume        13158.1(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4077445