Lewis base character of the phosphorus atom in phosphanido-niobocene complexes. Synthesis of new early‒early homo- and heterobimetallic entities
Reguillo-Carmona, R.; Antiñolo, A.; García-Yuste, S.; López-Solera, I.; Otero, A.; Dalton Transactions 40 (2011) 2622–; doi:10.1039/c0dt00865f

data_7014448
_publ_section_title
;
 Lewis base character of the phosphorus atom in phosphanido-niobocene
 complexes. Synthesis of new early--early homo- and heterobimetallic
 entities
;
_journal_issue                   11
_journal_name_full               'Dalton Transactions'
_journal_page_first              2622
_journal_paper_doi               10.1039/c0dt00865f
_journal_volume                  40
_journal_year                    2011
_chemical_formula_sum            'C29 H37 Cl6 Nb O P Si2 Ta'
_chemical_formula_weight         975.30
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 95.035(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.515(3)
_cell_length_b                   12.939(3)
_cell_length_c                   13.888(4)
_cell_measurement_temperature    250(2)
_cell_volume                     1882.2(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      250(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0973
_diffrn_reflns_av_sigmaI/netI    0.1539
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6395
_diffrn_reflns_theta_full        19.53
_diffrn_reflns_theta_max         19.53
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    3.764
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.313282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             956
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.787
_refine_diff_density_min         -0.504
_refine_diff_density_rms         0.121
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         3206
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          2.113
_refine_ls_shift/su_mean         0.113
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0377P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1488
_reflns_number_gt                2131
_reflns_number_total             3206
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00865F.TXT
_cod_data_source_block           9
_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.

'_exptl_absorpt_correction_type' value 'MULTI-SCAN' changed
to 'multi-scan' 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_enum 1555 2011-01-17 13:19:09Z saulius 
;
_cod_original_cell_volume        1882.1(9)
_cod_original_sg_symbol_H-M      P2(1)
_cod_database_code               7014448