Niobium η-cyclopentadienyl compounds with imido and amido ligands derived from tert-butylamine
Humphries, Martin J.; Green, Malcolm L. H.; Leech, Michael A.; Gibson, Vernon C.; Jolly, Matthew; Williams, David N.; Elsegood, Mark R. J.; Clegg, William; Journal of the Chemical Society, Dalton Transactions  (2000) 4044–; doi:10.1039/b006333i

data_7010132
_publ_section_title
;
 Niobium \h-cyclopentadienyl compounds with imido and amido ligands
 derived from tert-butylamine
;
_journal_issue                   22
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              4044
_journal_paper_doi               10.1039/b006333i
_journal_year                    2000
_chemical_formula_sum            'C21 H32 Cl N2 Nb'
_chemical_formula_weight         440.85
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 96.78(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.165(2)
_cell_length_b                   14.166(4)
_cell_length_c                   16.807(3)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    160(2)
_cell_measurement_theta_max      12.52
_cell_measurement_theta_min      10.92
_cell_volume                     2166.8(9)
_computing_cell_refinement       'Stoe DIF4'
_computing_data_collection       'Stoe DIF4'
_computing_data_reduction        'local programs'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      160(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  '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  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            4430
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.66
_diffrn_standards_decay_%        1
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    0.685
_exptl_absorpt_correction_T_max  0.8262
_exptl_absorpt_correction_T_min  0.7761
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             920
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.29
_refine_diff_density_max         0.806
_refine_diff_density_min         -1.309
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     238
_refine_ls_number_reflns         3822
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0612
_refine_ls_R_factor_gt           0.0396
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+4.1726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1021
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                2970
_reflns_number_total             3822
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b006333i.txt
_cod_data_source_block           vcg31
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7010132