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_7702572
_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            'C92 H74 Cl Nb O2'
_chemical_formula_weight         1339.97
_space_group_IT_number           2
_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             24-08-98
_audit_creation_method           from_MolEN_and_SHELXL
_cell_angle_alpha                109.4762(15)
_cell_angle_beta                 97.3407(17)
_cell_angle_gamma                102.6676(13)
_cell_formula_units_Z            2
_cell_length_a                   13.3332(4)
_cell_length_b                   15.3768(5)
_cell_length_c                   19.2026(5)
_cell_measurement_reflns_used    37974
_cell_measurement_temperature    203
_cell_measurement_theta_max      26
_cell_measurement_theta_min      4
_cell_volume                     3533.92(19)
_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  0.077
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            37974
_diffrn_reflns_theta_max         26.42
_diffrn_reflns_theta_min         4.00
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_T_max  0.9755
_exptl_absorpt_correction_T_min  0.5769
_exptl_absorpt_correction_type   refined_empirical_(Otwinowski_&_Minor,_1996)
_exptl_crystal_colour            yellow-orange
_exptl_crystal_density_diffrn    1.26
_exptl_crystal_description       palte
_exptl_crystal_F_000             1400
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.55
_refine_diff_density_min         -0.72
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    H_atoms_riding
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_refine_ls_number_parameters     865
_refine_ls_number_reflns         14354
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.059
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.6529P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.131
_reflns_number_gt                9824
_reflns_number_total             14354
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101722p.txt
_cod_data_source_block           MMS221
_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        3533.9(4)
_cod_original_sg_symbol_H-M      'p -1'
_cod_original_formula_sum        'C92 H74 Cl1 Nb1 O2'
_cod_database_code               7702572