Structural Distortions in Six-Coordinate Adducts of Niobium(V) and Tantalum(V)
Janet R. Clark; April L. Pulvirenti; Phillip E. Fanwick; Michaelis Sigalas; Odile Eisenstein; Ian P. Rothwell; Inorganic Chemistry 36 (1997) 3623–3631; doi:10.1021/ic970331l

data_4323541
_publ_contact_author
;
     I. P. Rothwell
     Department of Chemistry
     Purdue University
     W. Lafayette
     IN 47907
     USA
;
_publ_contact_author_email       rothwell@chem.purdue.edu
_publ_contact_author_fax         '(317) 494 0239'
_publ_contact_author_phone       '(317) 494 7012'
_publ_section_title
;
 Structural Distortions in Six-Coordinate Adducts of Niobium(V) and
 Tantalum(V)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3623
_journal_page_last               3631
_journal_paper_doi               10.1021/ic970331l
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C29 H39 Cl3 N O2 Ta'
_chemical_formula_weight         720.95
_chemical_name_systematic        ' ?'
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_type_scat_source           International_Tables_for_Xray_Crystallography
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.648(2)
_cell_length_b                   13.273(3)
_cell_length_c                   20.624(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      25
_cell_measurement_theta_min      19
_cell_volume                     3188.6(13)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_computing_molecular_graphics    ORTEP_(Johnson,_1976)
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  LSFM_MolEN_(Fair,_1990)
_computing_structure_solution    Patterson_and_Fourier
_diffrn_ambient_temperature      293
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3651
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         2.57
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.685
_exptl_absorpt_correction_T_max  0.2601
_exptl_absorpt_correction_T_min  0.2052
_exptl_absorpt_correction_type   refined_empirical_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.50
_exptl_crystal_description       chunk
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.61
_refine_diff_density_min         -0.15
_refine_ls_abs_structure_details
;
refinement results for the other absolute structure:
R = 0.046  Rw = 0.060  goodness_of_fit = 1.883
;
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_hydrogen_treatment    H_atoms_refined_U=1.3_x_U_bonding_atom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     325
_refine_ls_number_reflns         3090
_refine_ls_R_factor_all          0.046
_refine_ls_R_factor_obs          0.029
_refine_ls_shift/esd_max         0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1./(\sFo^2^ + ( 0.020*Fo )^2^ + 1.000 )'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.036
_reflns_number_observed          3090
_reflns_number_total             3651
_reflns_observed_criterion       >3.0\s(I)
_cod_data_source_file            ic970331l_4.cif
_cod_data_source_block           tacl3p
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C30 H39 A L3 N O2 T' to 'C29 H39 Cl3 N O2 Ta'.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value '1./(\sFo^2^ + ( 0.020*Fo )^2^ +
1.000 )' was changed to 'calc'. New tag
'_refine_ls_weighting_details' was created. The value of the new tag
was set to 'w = 1./(\sFo^2^ + ( 0.020*Fo )^2^ + 1.000 )'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3188(2)
_cod_original_formula_sum        'C29 H39 CL3 N1 O2 TA1'
_cod_database_code               4323541