A trigonal and hindered tertiary phosphine ligand rendered anionic by a niobate anchor: Formation of zwitterionic M(i) (M = Cu, Ag, Au, Rh) complexes
Creutz, Sidney E.; Krummenacher, Ivo; Clough, Christopher R.; Cummins, Christopher C.; Chemical Science 2 (2011) 2166–; doi:10.1039/c1sc00375e

data_1515563
_publ_section_title
;
 A trigonal and hindered tertiary phosphine ligand rendered anionic by a
 niobate anchor: Formation of zwitterionic M(i) (M = Cu, Ag, Au, Rh)
 complexes
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              2166
_journal_paper_doi               10.1039/c1sc00375e
_journal_volume                  2
_journal_year                    2011
_chemical_formula_sum            'C105 H138 N3 Na Nb O9 P'
_chemical_formula_weight         1733.05
_chemical_name_common            '[Na(thf)6][(Ar[Np]N)3Nb(OC[CPh2])3P]'
_space_group_IT_number           148
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   17.736(2)
_cell_length_b                   17.736(2)
_cell_length_c                   51.913(7)
_cell_measurement_reflns_used    9835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.26
_cell_measurement_theta_min      2.30
_cell_volume                     14142(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.1119
_diffrn_reflns_av_sigmaI/netI    0.0509
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       69
_diffrn_reflns_limit_l_min       -69
_diffrn_reflns_number            94854
_diffrn_reflns_theta_full        28.37
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.18
_exptl_absorpt_coefficient_mu    0.208
_exptl_absorpt_correction_T_max  0.9856
_exptl_absorpt_correction_T_min  0.9518
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             5568
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.838
_refine_diff_density_min         -0.735
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7872
_refine_ls_number_restraints     270
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0495
_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^)+(0.0570P)^2^+43.9684P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1179
_refine_ls_wR_factor_ref         0.1362
_reflns_number_gt                5983
_reflns_number_total             7872
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00375e.txt
_cod_data_source_block           r3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
according to
/usr/data/users/saulius/automatic-downloads/retrospective/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        14143(3)
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               1515563