The isolation and chemistry of niobium and tantalum dimethylamides containing mono- and di-aryloxide ancillary ligands
Schweiger, Scott W.; Tillison, Dana L.; Thorn, Matt G.; Fanwick, Phillip E.; Rothwell, Ian P.; Journal of the Chemical Society, Dalton Transactions  (2001) 2401–; doi:10.1039/b101723n

data_7702580
_publ_section_title
;
 The isolation and chemistry of niobium and tantalum dimethylamides
 containing mono- and di-aryloxide ancillary ligands
;
_journal_issue                   16
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2401
_journal_paper_doi               10.1039/b101723n
_journal_year                    2001
_chemical_formula_sum            'C15 H21 Cl3 N3 Ta'
_chemical_formula_weight         530.66
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.191(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.1788(7)
_cell_length_b                   7.2144(4)
_cell_length_c                   14.3129(6)
_cell_measurement_reflns_used    14249
_cell_measurement_temperature    173
_cell_measurement_theta_max      27
_cell_measurement_theta_min      4
_cell_volume                     1919.95(15)
_computing_cell_refinement       DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_data_collection       Collect_(Nonius,_1998)
_computing_data_reduction        DENZO/SCALEPACK_(Otwinowski,_1996)
_computing_molecular_graphics
;
ORTEP (Johnson, 1976)
Xtal_GX (Hall, 1995)
PLUTON (Spek, 1991)
;
_computing_publication_material  CIF_VAX_MolEN_(Fair,_1990)
_computing_structure_refinement  SHELX97_(Sheldrick,_1997)
_computing_structure_solution    PATTY_(DIRDIF92,_Beurskins,_1992)
_diffrn_ambient_temperature      173
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.088
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            14249
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    6.080
_exptl_absorpt_correction_T_max  0.6338
_exptl_absorpt_correction_T_min  0.3723
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996)
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.84
_exptl_crystal_description       plate
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.80
_refine_diff_density_min         -1.73
_refine_ls_extinction_coef       0.37E-02
_refine_ls_extinction_method     SHELXL97_(Sheldrick_1997)
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4305
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.037
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0436P)^2^+2.1492P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.085
_reflns_number_gt                3872
_reflns_number_total             4625
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101723n.txt
_cod_data_source_block           MT26I
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_refine_ls_weighting_scheme' value 'calc ' was changed to
'calc' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/RSC/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1919.9(3)
_cod_original_sg_symbol_H-M      'p 1 21/c 1'
_cod_database_code               7702580