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_4323542
_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            'C32 H45 Cl3 Nb O2 P'
_chemical_formula_weight         691.95
_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_type_scat_source
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.153(4)
_cell_length_b                   17.372(5)
_cell_length_c                   10.461(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    297
_cell_measurement_theta_max      18
_cell_measurement_theta_min      8
_cell_volume                     3481(3)
_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  SHELX93_(Sheldrick,_1993)
_computing_structure_solution    Patterson_and_Fourier
_diffrn_ambient_temperature      297
_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       -20
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            2609
_diffrn_reflns_theta_max         22.56
_diffrn_reflns_theta_min         2.62
_diffrn_standards_decay_%        -29.11
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.633
_exptl_absorpt_correction_T_max  0.8837
_exptl_absorpt_correction_T_min  0.5922
_exptl_absorpt_correction_type   refined_empirical_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.32
_exptl_crystal_description       needle
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.72
_refine_diff_density_min         -0.74
_refine_ls_abs_structure_Flack   -0.1(0)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.000
_refine_ls_goodness_of_fit_obs   1.075
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     362
_refine_ls_number_reflns         2425
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.230
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/esd_max         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.8767P] where P=(Fo^2^+2Fc^2^)/'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.000
_refine_ls_wR_factor_obs         0.114
_reflns_number_observed          0
_reflns_number_total             2425
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            ic970331l_5.cif
_cod_data_source_block           p23
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C33 H45 B L3 N O2 P' to 'C32 H45 Cl3 Nb O2 P'.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+34.8767P] where P=(Fo^2^+2Fc^2^)/' 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^)+(0.0000P)^2^+34.8767P] where P=(Fo^2^+2Fc^2^)/'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3480(4)
_cod_original_formula_sum        'C32 H45 CL3 NB1 O2 P1'
_cod_database_code               4323542