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_7014449
_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            'C41 H53 Cl5 N Nb2 O2 P Si2'
_chemical_formula_weight         1042.06
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.091(2)
_cell_angle_beta                 93.465(2)
_cell_angle_gamma                90.778(3)
_cell_formula_units_Z            2
_cell_length_a                   12.0250(18)
_cell_length_b                   12.1588(18)
_cell_length_c                   15.964(2)
_cell_measurement_temperature    180(2)
_cell_volume                     2329.6(6)
_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      180(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0503
_diffrn_reflns_av_sigmaI/netI    0.0740
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            10199
_diffrn_reflns_theta_full        21.29
_diffrn_reflns_theta_max         21.29
_diffrn_reflns_theta_min         2.06
_exptl_absorpt_coefficient_mu    0.899
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.746808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.486
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prismatic
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.972
_refine_diff_density_min         -1.300
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.314
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     495
_refine_ls_number_reflns         5041
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.314
_refine_ls_R_factor_all          0.0952
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.029
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.5549P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2044
_refine_ls_wR_factor_ref         0.2156
_reflns_number_gt                3899
_reflns_number_total             5041
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            C0DT00865F.TXT
_cod_data_source_block           12
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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        2329.5(6)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7014449