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_4327704
_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            'C16 H27 Cl3 N O2 Ta'
_chemical_formula_weight         552.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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            4
_cell_length_a                   14.430(3)
_cell_length_b                   9.813(2)
_cell_length_c                   14.370(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      13
_cell_measurement_theta_min      10.5
_cell_volume                     2034.8(7)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      208(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w 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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0241
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3262
_diffrn_reflns_theta_max         24.39
_diffrn_reflns_theta_min         2.51
_diffrn_standards_decay_%        '< 1%'
_diffrn_standards_interval_count 197
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.803
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_correction_T_min  0.615
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.804
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.457
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.074
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_coef       0.00022(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   0.965
_refine_ls_goodness_of_fit_obs   0.980
_refine_ls_matrix_type           full
_refine_ls_number_parameters     210
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.965
_refine_ls_restrained_S_obs      0.980
_refine_ls_R_factor_all          0.0247
_refine_ls_R_factor_obs          0.0183
_refine_ls_shift/esd_max         -0.175
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0266P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0420
_refine_ls_wR_factor_obs         0.0396
_reflns_number_observed          1473
_reflns_number_total             1670
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704942B_1.cif
_cod_data_source_block           compound1
_cod_depositor_comments
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The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0266P)^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^)+(0.0266P)^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_database_code               4327704