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_4323538
_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            'C48 H68 Cl6 Nb2 O4'
_chemical_formula_weight         1107.60
_chemical_name_systematic        ' ?'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 90.607(14)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.735(2)
_cell_length_b                   15.527(3)
_cell_length_c                   13.620(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    295
_cell_measurement_theta_max      42
_cell_measurement_theta_min      18
_cell_volume                     2693.0(8)
_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      295
_diffrn_measurement_device       Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Cu-K\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.048
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4662
_diffrn_reflns_theta_max         62.30
_diffrn_reflns_theta_min         2.59
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.665
_exptl_absorpt_correction_T_max  0.4103
_exptl_absorpt_correction_T_min  0.1886
_exptl_absorpt_correction_type   refined_empirical_(Walker_&_Stuart,_1983)
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.37
_exptl_crystal_description       cube
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.96
_refine_diff_density_min         -0.86
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.129
_refine_ls_goodness_of_fit_obs   0.997
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4256
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.183
_refine_ls_R_factor_obs          0.062
_refine_ls_shift/esd_max         0.028
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+29.2367P] where P=(Fo^2^+2Fc^2^)/'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.194
_refine_ls_wR_factor_obs         0.121
_reflns_number_observed          2248
_reflns_number_total             4258
_reflns_observed_criterion       >2.0\s(I)
_cod_data_source_file            ic970331l_1.cif
_cod_data_source_block           NB0A2CL3
_cod_depositor_comments
;
 Changing the _chemical_formula_sum data item value from
 'C49 H68 B2 L6 N O4' to 'C48 H68 Cl6 Nb2 O4'.

 Antanas Vaitkus,
 2017-01-04

The following automatic conversions were performed:

'_geom_bond_publ_flag' value 'YES' changed to 'yes' according to the
built-in table from CIF Core dictionary named 'cif_core.dic' version
2.4.1 from 2010-06-29 (9 times).

'_geom_bond_publ_flag' value 'NO'
changed to 'no' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (26
times).

'_geom_angle_publ_flag' value 'YES' changed to 'yes'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (18
times).

'_geom_angle_publ_flag' value 'NO' changed to 'no' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29 (39 times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0219P)^2^+29.2367P] 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^)+(0.0219P)^2^+29.2367P] 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        2693.0(14)
_cod_original_formula_sum        'C48 H68 CL6 NB2 O4'
_cod_database_code               4323538