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_4323543
_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            'C44 H62 Cl2 Nb O3 P'
_chemical_formula_weight         833.77
_chemical_name_systematic        ' ?'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_type_scat_source
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_cell_angle_alpha                85.553(9)
_cell_angle_beta                 73.433(9)
_cell_angle_gamma                89.794(7)
_cell_formula_units_Z            2
_cell_length_a                   13.1862(9)
_cell_length_b                   13.3274(12)
_cell_length_c                   13.4391(16)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296
_cell_measurement_theta_max      25
_cell_measurement_theta_min      18
_cell_volume                     2256.5(4)
_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      296
_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  0.018
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            9565
_diffrn_reflns_theta_max         26.32
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        -36.93
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.442
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.23
_exptl_crystal_description       plate
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.64
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.35
_refine_diff_density_max         0.35
_refine_diff_density_min         -0.64
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.169
_refine_ls_goodness_of_fit_obs   1.038
_refine_ls_hydrogen_treatment    H_atoms_refined_U=1.3_x_U_bonding_atom
_refine_ls_matrix_type           full
_refine_ls_number_parameters     474
_refine_ls_number_reflns         9161
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_refine_ls_R_factor_all          0.071
_refine_ls_R_factor_obs          0.039
_refine_ls_shift/esd_max         0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+1.4651P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.112
_refine_ls_wR_factor_obs         0.086
_reflns_number_observed          6968
_reflns_number_total             9161
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            ic970331l_6.cif
_cod_data_source_block           p32
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C45 H62 B L2 N O3 P' to 'C44 H62 Cl2 Nb O3 P'.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0402P)^2^+1.4651P] 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^)+(0.0402P)^2^+1.4651P] 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        2256.5(5)
_cod_original_formula_sum        'C44 H62 CL2 NB1 O3 P1'
_cod_database_code               4323543