Crystal structure of (μ-1,4-dicarboxybutane-1,4-dicarboxylato)bis[bis(triphenylphosphane)silver(I)] dichloromethane trisolvate
Frenzel, Peter; Korb, Marcus; Lang, Heinrich; Acta Crystallographica Section E 72 (2016) 215–219; doi:10.1107/S2056989016000797

data_2241518
_publ_section_title
;
 Crystal structure of
 (\m-1,4-dicarboxybutane-1,4-dicarboxylato)bis[bis(triphenylphosphane)silver(I)]
 dichloromethane trisolvate
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              215
_journal_page_last               219
_journal_paper_doi               10.1107/S2056989016000797
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ag2 (C8 H8 O8) (C18 H15 P)4], 3C H2 Cl2'
_chemical_formula_moiety         'C80 H68 Ag2 O8 P4, 3(C H2 Cl2)'
_chemical_formula_sum            'C83 H74 Ag2 Cl6 O8 P4'
_chemical_formula_weight         1751.74
_chemical_name_systematic
;
(\m-1,4-Dicarboxybutane-1,4-dicarboxylato)bis[bis(triphenylphosphane)silver(I)]
dichloromethane trisolvate
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                112.306(3)
_cell_angle_beta                 96.080(3)
_cell_angle_gamma                103.601(3)
_cell_formula_units_Z            1
_cell_length_a                   10.0279(3)
_cell_length_b                   12.9540(4)
_cell_length_c                   16.8190(5)
_cell_measurement_reflns_used    12088
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.8140
_cell_measurement_theta_min      3.4170
_cell_volume                     1917.80(12)
_computing_cell_refinement
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_data_collection
;
CrysAlis CCD (Oxford Diffraction, 2006)
;
_computing_data_reduction
;
CrysAlis RED (Oxford Diffraction, 2006)
;
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 2012) and SHELXTL (Sheldrick,
2008)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) and publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution    'SHELXS2013 (Sheldrick, 200)'
_diffrn_ambient_temperature      110(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Oxford Gemini S'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0242
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21441
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.903
_diffrn_reflns_theta_min         2.931
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 50
_diffrn_standards_interval_time  10
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    0.860
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.88867
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis
RED</i>; Oxford Diffraction,
2006)
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.280
_refine_diff_density_min         -0.614
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     507
_refine_ls_number_reflns         8700
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+2.6912P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0803
_refine_ls_wR_factor_ref         0.0827
_reflns_number_gt                7959
_reflns_number_total             8700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            zl2653sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        1917.80(11)
_cod_database_code               2241518
_cod_database_fobs_code          2241518
_shelx_hkl_checksum              77731
_shelx_res_checksum              79535