Studies of the alkylation of niobium and tantalum halides containing 2,6-diarylphenoxide ancillary ligation
Schweiger, Scott W.; Salberg, Michelle M.; Pulvirenti, April L.; Freeman, Emily E.; Fanwick, Phillip E.; Rothwell, Ian P.; Journal of the Chemical Society, Dalton Transactions  (2001) 2020–; doi:10.1039/b101722p

data_7702571
_publ_section_title
;
 Studies of the alkylation of niobium and tantalum halides containing
 2,6-diarylphenoxide ancillary ligation
;
_journal_issue                   13
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              2020
_journal_paper_doi               10.1039/b101722p
_journal_year                    2001
_chemical_formula_sum            'C44 H48 Cl O2 Si2 Ta'
_chemical_formula_weight         881.45
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             5-09-00
_audit_creation_method           from_MolEN_and_SHELXL
_cell_angle_alpha                63.9019(8)
_cell_angle_beta                 87.6411(7)
_cell_angle_gamma                68.9612(8)
_cell_formula_units_Z            1
_cell_length_a                   10.0085(2)
_cell_length_b                   10.8522(2)
_cell_length_c                   11.2929(2)
_cell_measurement_reflns_used    11150
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1018.06(3)
_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      150
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.027
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11150
_diffrn_reflns_theta_max         27.89
_diffrn_reflns_theta_min         5.00
_exptl_absorpt_coefficient_mu    2.825
_exptl_absorpt_correction_T_max  0.5684
_exptl_absorpt_correction_T_min  0.2607
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996)
_exptl_crystal_colour            'pale yellow '
_exptl_crystal_density_diffrn    1.44
_exptl_crystal_description       chunk
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.12
_refine_diff_density_min         -2.32
_refine_ls_abs_structure_details
'Flack H. D. (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.403(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7769
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.042
_refine_ls_shift/su_max          0.049
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0503P)^2^+6.2442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.108
_reflns_number_gt                7776
_reflns_number_total             7777
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101722p.txt
_cod_data_source_block           ROT1
_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        1018.06(4)
_cod_original_sg_symbol_H-M      'p 1'
_cod_original_formula_sum        'C44 H48 Cl1 O2 Si2 Ta1'
_cod_database_code               7702571
_reflns_friedl_coverage          0.7728