Terminal phosphinidene formation via tantalaziridine complexes.
Rankin, Matthew A.; Cummins, Christopher C.; Dalton transactions (Cambridge, England : 2003) 41 (2012) 9615–9618; doi:10.1039/c2dt31082a

data_7019922
_publ_section_title
;
 Terminal phosphinidene formation via tantalaziridine complexes.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9615
_journal_page_last               9618
_journal_paper_doi               10.1039/c2dt31082a
_journal_volume                  41
_journal_year                    2012
_chemical_formula_sum            'C39.5 H61 Cl3.25 N3 Ta'
_chemical_formula_weight         874.08
_chemical_name_common            (Ar(CH2tBu)N)3TaCl2
_chemical_name_systematic
;
?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.0310(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   22.3937(19)
_cell_length_b                   13.1868(11)
_cell_length_c                   29.573(3)
_cell_measurement_reflns_used    9830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.02
_cell_measurement_theta_min      2.60
_cell_volume                     8304.1(13)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2009)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2009)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker Smart APEX-II CCD'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0244
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            103293
_diffrn_reflns_theta_full        29.57
_diffrn_reflns_theta_max         29.57
_diffrn_reflns_theta_min         1.45
_exptl_absorpt_coefficient_mu    2.886
_exptl_absorpt_correction_T_max  0.5096
_exptl_absorpt_correction_T_min  0.3633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             3578
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.27
_platon_squeeze_details
; The unit cell contains 2 molecules of chloroform and 2 molecules of
methylene chloride which have been treated as a diffuse contribution
to the overall scattering without specific atom positions by SQUEEZE/
PLATON.
;
_refine_diff_density_max         2.234
_refine_diff_density_min         -0.764
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     421
_refine_ls_number_reflns         11619
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0318P)^2^+66.5885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0855
_refine_ls_wR_factor_ref         0.0873
_reflns_number_gt                10572
_reflns_number_total             11619
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2dt31082a.txt
_cod_data_source_block           09187p_e
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        8304.0(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_original_formula_sum        'C39.50 H61 Cl3.25 N3 Ta'
_cod_database_code               7019922