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_1515560
_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            'C96 H115 Ag N4 Nb O5.5 P'
_chemical_formula_weight         1644.67
_chemical_name_common            (pyr)AgP(C[CPh2]O)3Nb(N[Np]Ar)3
_space_group_IT_number           14
_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                 116.3960(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.086(2)
_cell_length_b                   14.0697(11)
_cell_length_c                   24.790(2)
_cell_measurement_temperature    100(2)
_cell_volume                     8462.3(11)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_data_collection       'APEX2 v2009.9.0 (Bruker-AXS, 2009)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Bruker Smart APEX 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  0.0543
_diffrn_reflns_av_sigmaI/netI    0.0977
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35973
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         29.53
_diffrn_reflns_theta_min         1.64
_exptl_absorpt_coefficient_mu    0.441
_exptl_absorpt_correction_T_max  0.8609
_exptl_absorpt_correction_T_min  0.8262
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.291
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3464
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.35
_refine_diff_density_max         1.438
_refine_diff_density_min         -1.094
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.969
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         21967
_refine_ls_number_restraints     1236
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.0897
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1391
_reflns_number_gt                13833
_reflns_number_total             21967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1sc00375e.txt
_cod_data_source_block           10096
_cod_original_cell_volume        8462.3(12)
_cod_original_sg_symbol_H-M      P21/c
_cod_original_formula_sum        'C96 H115 Ag N4 Nb O5.50 P'
_cod_database_code               1515560