Coinage metal complexes supported by the tri- and tetraphosphine ligands.
Dau, Minh Thuy; Shakirova, Julia R.; Karttunen, Antti J.; Grachova, Elena V.; Tunik, Sergey P.; Melnikov, Alexey S.; Pakkanen, Tapani A.; Koshevoy, Igor O.; Inorganic chemistry 53 (2014) 4705–4715; doi:10.1021/ic500402m

data_4338175
_publ_section_title
;
 Coinage metal complexes supported by the tri- and tetraphosphine ligands.
;
_journal_issue                   9
_journal_name_full               'Inorganic chemistry'
_journal_page_first              4705
_journal_page_last               4715
_journal_paper_doi               10.1021/ic500402m
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety
'C66 H61 Ag2 Au N P6, 3(Cl O4), C2 H3 N, C H4 O'
_chemical_formula_sum            'C69 H68 Ag2 Au Cl3 N2 O13 P6'
_chemical_formula_weight         1838.13
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3970(8)
_cell_length_b                   18.6453(11)
_cell_length_c                   27.3658(15)
_cell_measurement_reflns_used    9267
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      32.58
_cell_measurement_theta_min      2.60
_cell_volume                     7346.0(7)
_computing_cell_refinement       'SAINT (Bruker AXS, 2009)'
_computing_data_collection       'APEX2 (Bruker AXS, 2010)'
_computing_data_reduction        'SAINT (Bruker AXS, 2009)'
_computing_molecular_graphics    'Diamond v.3.2g (Brandenburg, 2011)'
_computing_publication_material  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 16
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device
'62mm x 62mm CCD camera on three-circle goniostat'
_diffrn_measurement_device_type  'Bruker SMART APEX II CCD'
_diffrn_measurement_method       '\f scans and \w scans'
_diffrn_radiation_monochromator  'flat graphite crystal'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0785
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            49778
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.000
_diffrn_reflns_theta_min         1.598
_exptl_absorpt_coefficient_mu    2.821
_exptl_absorpt_correction_T_max  0.559
_exptl_absorpt_correction_T_min  0.460
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.662
_exptl_crystal_description       block
_exptl_crystal_F_000             3656
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.298
_exptl_crystal_size_min          0.233
_refine_diff_density_max         3.060
_refine_diff_density_min         -1.850
_refine_diff_density_rms         0.155
_refine_ls_abs_structure_details
;
 Flack x determined using 6925 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   0.070(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     875
_refine_ls_number_reflns         19223
_refine_ls_number_restraints     89
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0528
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+12.4704P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1169
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.818
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                17123
_reflns_number_total             19223
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic500402m_si_003.cif
_cod_data_source_block           3b
_cod_depositor_comments
'Adding full bibliography for 4338172--4338179.cif.'
_cod_database_code               4338175
_shelx_estimated_absorpt_t_min   0.460
_shelx_estimated_absorpt_t_max   0.559