Synthesis and structural characterisation of new organo-diimido tantalum and niobium complexes
Antiñolo, Antonio; Dorado, Iván; Fajardo, Mariano; Garcés, Andrés; Kubicki, Marek M.; López-Mardomingo, Carmen; Otero, Antonio; Dalton Transactions  (2003) 910–; doi:10.1039/b211126h

data_7012464
_publ_section_title
;
 Synthesis and structural characterisation of new organo-diimido
 tantalum and niobium complexes
;
_journal_issue                   5
_journal_name_full               'Dalton Transactions'
_journal_page_first              910
_journal_paper_doi               10.1039/b211126h
_journal_year                    2003
_chemical_formula_sum            'C38 H56 Cl2 N2 Si4 Ta2'
_chemical_formula_weight         1086.01
_chemical_name_systematic
; 
? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 97.408(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.9570(4)
_cell_length_b                   26.464(2)
_cell_length_c                   11.6880(7)
_cell_measurement_temperature    110(2)
_cell_volume                     2133.9(2)
_computing_cell_refinement       'HKL Scalepack'
_computing_data_collection       'KappaCCD supergui'
_computing_data_reduction        'DENZO & Scalepack'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      110(2)
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_method       CCD
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0500
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4730
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    5.390
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.690
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1068
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.08
_refine_diff_density_max         4.067
_refine_diff_density_min         -3.240
_refine_diff_density_rms         0.338
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.163
_refine_ls_goodness_of_fit_obs   1.185
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         4729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.164
_refine_ls_restrained_S_obs      1.185
_refine_ls_R_factor_all          0.0733
_refine_ls_R_factor_obs          0.0694
_refine_ls_shift/esd_max         -0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+40.1006P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1801
_refine_ls_wR_factor_obs         0.1762
_reflns_number_observed          4378
_reflns_number_total             4730
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b211126h.txt
_cod_data_source_block           13a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+40.1006P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0868P)^2^+40.1006P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7012464