Bis(η^5^-<i>tert</i>-butylcyclopentadienyl)dichloroniobium(IV)
McCamley, Andrew; Miller, Thomas J.; Clegg, William; Acta Crystallographica Section C 50 (1994) 33–36; doi:10.1107/S0108270193006961

data_2009409
_publ_section_title
;
 Bis(\h^5^-<i>tert</i>-butylcyclopentadienyl)dichloroniobium(IV)
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              33
_journal_page_last               36
_journal_paper_doi               10.1107/S0108270193006961
_journal_volume                  50
_journal_year                    1994
_chemical_formula_moiety         '[Nb Cl2 (C9 H13)2]'
_chemical_formula_sum            'C18 H26 Cl2 Nb'
_chemical_formula_weight         406.20
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.383(2)
_cell_length_b                   12.906(3)
_cell_length_c                   13.327(3)
_cell_measurement_reflns_used    31
_cell_measurement_temperature    160.0(10)
_cell_measurement_theta_max      12.42
_cell_measurement_theta_min      10.02
_cell_volume                     1785.9(7)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1988)'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-92 (Sheldrick, 1992)'
_computing_structure_solution    'SHELXTL/PC (Sheldrick, 1990)'
_diffrn_ambient_temperature      160.0(10)
_diffrn_measurement_device       'Stoe-Siemens diffractometer'
_diffrn_measurement_method       '\w/\q 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  '0.0795 (on F^2^)'
_diffrn_reflns_av_sigmaI/netI    0.0724
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3567
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.49
_diffrn_standards_decay_%        2
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.965
_exptl_absorpt_correction_T_max  0.84
_exptl_absorpt_correction_T_min  0.65
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       Prism???
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.31
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.61
_refine_diff_density_min         -1.03
_refine_ls_abs_structure_details 'Absolute structure parameter x = 0.16 (9)'
_refine_ls_abs_structure_Flack   0.16(9)
_refine_ls_extinction_coef       0.0010(4)
_refine_ls_extinction_method     'SHELXL92 (Sheldrick, 1992)'
_refine_ls_goodness_of_fit_all   1.053
_refine_ls_goodness_of_fit_obs   1.070
_refine_ls_hydrogen_treatment    'H atoms constrained'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         2418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_restrained_S_obs      1.070
_refine_ls_R_factor_all          0.0641
_refine_ls_R_factor_obs          0.0324
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;calc w = 1/[\s^2^(F~o~^2^) + (0.0353P)^2^ + 0.0000P] where
P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0831
_refine_ls_wR_factor_obs         0.0731
_reflns_number_observed          1858
_reflns_number_total             2418
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            mu1065.cif
_cod_data_source_block           am4
_cod_database_code               2009409