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_7702581
_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            'C97 H83 Cl2 N2 Nb O2'
_chemical_formula_weight         1472.57
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P n a 21'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.4539(2)
_cell_length_b                   22.0854(4)
_cell_length_c                   11.4593(9)
_cell_measurement_reflns_used    37476
_cell_measurement_temperature    150
_cell_measurement_theta_max      24
_cell_measurement_theta_min      5
_cell_volume                     7707.4(6)
_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    Direct_methods_(SIR97,_Altomare_et_al.,_1997)
_diffrn_ambient_temperature      150
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.127
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            37476
_diffrn_reflns_theta_max         24.73
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    0.268
_exptl_absorpt_correction_T_max  0.9735
_exptl_absorpt_correction_T_min  0.6883
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996)
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.27
_exptl_crystal_description       plate
_exptl_crystal_F_000             3080
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.30
_refine_diff_density_min         -0.41
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.43(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     940
_refine_ls_number_reflns         12716
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.058
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'1/[\s^2^(Fo^2^)+(0.0368P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3  '
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.095
_reflns_number_gt                10602
_reflns_number_total             12717
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101723n.txt
_cod_data_source_block           DTP22
_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        7707.4(5)
_cod_original_sg_symbol_H-M      'p n a 21'
_cod_original_formula_sum        'C97 H83 Cl2 N2 Nb1 O2'
_cod_database_code               7702581
_reflns_friedl_coverage          0.9202