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_4327707
_publ_section_title
;
 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 Nb O2'
_chemical_formula_weight         464.64
_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                   14.494(6)
_cell_length_b                   9.819(3)
_cell_length_c                   14.342(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    208(2)
_cell_measurement_theta_max      15.0?
_cell_measurement_theta_min      10.0
_cell_volume                     2041.1(12)
_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  0.0308
_diffrn_reflns_av_sigmaI/netI    0.0329
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3623
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    0.990
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.85
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_F_000             952
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.053
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.10(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.057
_refine_ls_goodness_of_fit_obs   1.073
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         1871
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.082
_refine_ls_restrained_S_obs      1.073
_refine_ls_R_factor_all          0.0296
_refine_ls_R_factor_obs          0.0235
_refine_ls_shift/esd_max         -0.837
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0262P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0556
_refine_ls_wR_factor_obs         0.0522
_reflns_number_observed          1690
_reflns_number_total             1871
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9704942B_4.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0262P)^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^)+(0.0262P)^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               4327707