A novel, rigid diphosphine with an active NHC spacer; di- and trinuclear complexes of d10 coinage metals
Pengfei Ai; Andreas A. Danopoulos; Pierre Braunstein; Kirill Yu. Monakhovc; Chem.Commun. 50 (2013) 103–; doi:10.1039/c3cc47370h

data_7110166
_publ_section_title
;
 A novel, rigid diphosphine with an active NHC spacer; di- and trinuclear
 complexes of d10 coinage metals
;
_journal_name_full               Chem.Commun.
_journal_page_first              103
_journal_paper_doi               10.1039/c3cc47370h
_journal_volume                  50
_journal_year                    2013
_chemical_formula_moiety
'C38 H76 Ag3 N4 P4, 3(C F3 O3 S), 2(C H2 Cl2)'
_chemical_formula_sum            'C43 H80 Ag3 Cl4 F9 N4 O9 P4 S3'
_chemical_formula_weight         1653.58
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.5334(6)
_cell_length_b                   15.6264(5)
_cell_length_c                   25.5667(7)
_cell_measurement_reflns_used    8880
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.95
_cell_measurement_theta_min      2.40
_cell_volume                     6605.3(4)
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  triumph
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_sigmaI/netI    0.0495
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            34171
_diffrn_reflns_theta_full        31.02
_diffrn_reflns_theta_max         31.02
_diffrn_reflns_theta_min         1.53
_exptl_absorpt_coefficient_mu    1.308
_exptl_absorpt_correction_T_max  0.7798
_exptl_absorpt_correction_T_min  0.7272
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.663
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3344
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.765
_refine_diff_density_min         -1.403
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         10868
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0454
_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^)+(0.0308P)^2^+20.4278P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0904
_refine_ls_wR_factor_ref         0.1137
_reflns_number_gt                6629
_reflns_number_total             10868
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c3cc47370h.txt
_cod_data_source_block           pbad130425
_cod_database_code               7110166