Molecular Structures and FT-Raman Spectroscopy of Luminescent Niobium and Tantalum Arylimido Compounds
Kurt S. Heinselman; Vincent M. Miskowski; Steven J. Geib; Louis C. Wang; Michael D. Hopkins; Inorganic Chemistry 36 (1997) 5530–5538; doi:10.1021/ic970494+

data_4327705
_publ_section_title
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 Molecular Structures and FT-Raman Spectroscopy of Luminescent Niobium and
 Tantalum Arylimido Compounds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5530
_journal_page_last               5538
_journal_paper_doi               10.1021/ic970494+
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C18 H33 Cl3 N3 Ta'
_chemical_formula_weight         578.77
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
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_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   16.722(14)
_cell_length_b                   15.509(13)
_cell_length_c                   17.739(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     4600(7)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0330
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -20
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_exptl_absorpt_correction_T_max  .721
_exptl_absorpt_correction_T_min  .540
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_F_000             2288
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.965
_refine_diff_density_min         -0.861
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00009(9)
_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   0.835
_refine_ls_goodness_of_fit_obs   0.822
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_refine_ls_number_reflns         3271
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_refine_ls_R_factor_obs          0.0327
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_refine_ls_shift/esd_mean        0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1228
_refine_ls_wR_factor_obs         0.0965
_reflns_number_observed          2578
_reflns_number_total             3271
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704942B_2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1000P)^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^)+(0.1000P)^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        4600.5(67)
_cod_database_code               4327705