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_7702576
_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            'C66 H86 Nb O2 P2'
_chemical_formula_weight         1066.27
_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             26-09-97
_audit_creation_method           from_MolEN_and_SHELXL
_cell_angle_alpha                106.078(16)
_cell_angle_beta                 97.680(16)
_cell_angle_gamma                111.580(13)
_cell_formula_units_Z            1
_cell_length_a                   11.4726(17)
_cell_length_b                   11.9803(19)
_cell_length_c                   12.491(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    203
_cell_measurement_theta_max      19
_cell_measurement_theta_min      17
_cell_volume                     1479.8(6)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        PROCESS_MolEN_(Fair,_1990)
_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      203
_diffrn_measurement_device_type  Enraf_Nonius_CAD4
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_type           Mo-K\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.030
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4869
_diffrn_reflns_theta_max         24.06
_diffrn_reflns_theta_min         2.93
_diffrn_standards_decay_%        0.71
_diffrn_standards_interval_time  83
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.287
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.20
_exptl_crystal_description       needle
_exptl_crystal_F_000             569
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.43
_refine_diff_density_min         -0.62
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.130
_refine_ls_hydrogen_treatment
;
Chemically significant hydrogens refined isotropically
Others riding, U=1.3*Ueq of bonding atom
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         4629
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.043
_refine_ls_shift/su_max          0.013
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0407P)^2^+1.3591P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.117
_reflns_number_gt                3479
_reflns_number_total             4629
_reflns_threshold_expression     >2.0\s(I)
_cod_data_source_file            b101722p.txt
_cod_data_source_block           MMS172
_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        1479.8(13)
_cod_original_sg_symbol_H-M      'p -1'
_cod_original_formula_sum        'C66 H86 Nb1 O2 P2'
_cod_database_code               7702576