A General Route to Labile Niobium and Tantalum d0 Monoimides. Discussion of Metal-Nitrogen Vibrational Modes
Andrey V. Korolev; Arnold L. Rheingold; Darryl S. Williams; Inorganic Chemistry 36 (1997) 2647–2655; doi:10.1021/ic961360j

data_4323465
_publ_contact_author
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        Dr. D.S. Williams
    Department of Chemistry, 145
    Wayne State University
    Detroit, MI  48202
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_publ_contact_author_email       williams@chem.wayne.edu
_publ_contact_author_fax         (313)-577-3102
_publ_contact_author_phone       (313)-577-3102
_publ_section_title
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 A General Route to Labile Niobium and Tantalum d0 Monoimides. Discussion
 of Metal-Nitrogen Vibrational Modes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2647
_journal_page_last               2655
_journal_paper_doi               10.1021/ic961360j
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C8 H19 Cl3 N Nb O2'
_chemical_formula_weight         360.50
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.626(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   30.565(4)
_cell_length_b                   7.2406(13)
_cell_length_c                   13.915(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    249(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      2
_cell_volume                     3079.3(8)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      249(2)
_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  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2912
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.67
_exptl_absorpt_coefficient_mu    1.287
_exptl_crystal_colour            yellow-green
_exptl_crystal_density_diffrn    1.555
_exptl_crystal_description       rod
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.633
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.089
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.08(10)
_refine_ls_extinction_coef       0.0023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   0.991
_refine_ls_goodness_of_fit_obs   1.052
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         2460
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.051
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_obs          0.0392
_refine_ls_shift/esd_max         -0.026
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1107
_refine_ls_wR_factor_obs         0.1025
_reflns_number_observed          2101
_reflns_number_total             2463
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic961360j.cif
_cod_data_source_block           darr01
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3079.4(8)
_cod_database_code               4323465