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_1515564
_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            'C74.75 H97 N3 Na Nb O3 P'
_chemical_formula_weight         1232.42
_chemical_name_common            '[(Ar[Np]N)3Nb(OC[CPh2])2P][Na(thf)]'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.0020(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.715(2)
_cell_length_b                   16.1639(13)
_cell_length_c                   19.4189(16)
_cell_measurement_reflns_used    9305
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.51
_cell_measurement_theta_min      2.19
_cell_volume                     7118.5(10)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0380
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            109340
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         0.90
_exptl_absorpt_coefficient_mu    0.243
_exptl_absorpt_correction_T_max  0.9808
_exptl_absorpt_correction_T_min  0.9175
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.150
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2630
_exptl_crystal_size_max          0.36
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.009
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     892
_refine_ls_number_reflns         13042
_refine_ls_number_restraints     395
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0659
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+10.2114P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1156
_refine_ls_wR_factor_ref         0.1310
_reflns_number_gt                10072
_reflns_number_total             13042
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00375e.txt
_cod_data_source_block           09043
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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        7118.4(10)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               1515564