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_7702577
_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            'C70 H56 Cl3 Nb O2'
_chemical_formula_weight         1128.49
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_type_scat_source
'International Tables for Crystallography (Vol C)'
_audit_creation_date             22-10-98
_audit_creation_method           from_MolEN_and_SHELXL
_audit_update_record             ' ?'
_cell_angle_alpha                90.00
_cell_angle_beta                 96.2926(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.3325(2)
_cell_length_b                   21.2903(3)
_cell_length_c                   23.9340(4)
_cell_measurement_reflns_used    46609
_cell_measurement_temperature    203
_cell_measurement_theta_max      30
_cell_measurement_theta_min      4
_cell_volume                     5739.82(16)
_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      203
_diffrn_radiation_type           MO-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            46609
_diffrn_reflns_theta_max         30.52
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.384
_exptl_absorpt_correction_T_max  0.9260
_exptl_absorpt_correction_T_min  0.7239
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.31
_exptl_crystal_description       prism
_exptl_crystal_F_000             2336
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.53
_refine_diff_density_min         -0.83
_refine_ls_extinction_coef       0.44E-02
_refine_ls_extinction_method     SHELXL97_(Sheldrick_1997)
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    H_atoms_riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     690
_refine_ls_number_reflns         15178
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.049
_refine_ls_shift/su_max          0.052
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0685P)^2^+0.9643P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.119
_reflns_number_gt                10376
_reflns_number_total             15178
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101722p.txt
_cod_data_source_block           MMS229
_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        5739.8(3)
_cod_original_sg_symbol_H-M      'p 1 21/n 1'
_cod_original_formula_sum        'C70 H56 Cl3 Nb1 O2'
_cod_database_code               7702577