Crystal structure of dimethanol-(μ2-squarato-κ2 O:O′)-tetrakis(tri-p-tolylphosphane-κP)disilver(I) – methanol (1/2), C92H98Ag2O8P4
Liu, Kuanguan; Nie, Jing; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 565–567; doi:10.1515/ncrs-2017-0322

data_8106218
_publ_section_title
;
 Crystal structure of dimethanol-(\m2-squarato-\k2
 O:O&#x2032;)-tetrakis(tri-p-tolylphosphane-\kP)disilver(I) -- methanol
 (1/2), C92H98Ag2O8P4
;
_journal_issue                   4
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              565
_journal_page_last               567
_journal_paper_doi               10.1515/ncrs-2017-0322
_journal_volume                  233
_journal_year                    2018
_chemical_formula_sum            'C46 H49 Ag O4 P2'
_chemical_formula_weight         835.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                83.607(8)
_cell_angle_beta                 78.636(9)
_cell_angle_gamma                83.128(9)
_cell_formula_units_Z            2
_cell_length_a                   11.179(3)
_cell_length_b                   12.623(3)
_cell_length_c                   15.656(4)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    294(2)
_cell_measurement_theta_max      0.916
_cell_measurement_theta_min      0.894
_cell_volume                     2141.6(9)
_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-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0336
_diffrn_reflns_av_unetI/netI     0.0385
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            31691
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.564
_diffrn_reflns_theta_min         2.939
_exptl_absorpt_coefficient_mu    0.586
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6982
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.296
_exptl_crystal_description       block
_exptl_crystal_F_000             868
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.490
_refine_diff_density_rms         0.060
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         9890
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0436P)^2^+1.3722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0924
_refine_ls_wR_factor_ref         0.1034
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                7480
_reflns_number_total             9890
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2017-0322_suppl.cif
_cod_data_source_block           mo
_cod_original_cell_volume        2141.6(10)
_cod_database_code               8106218
_shelx_estimated_absorpt_t_min   0.892
_shelx_estimated_absorpt_t_max   0.917
_exptl_absorpt_special_details
;
 The following wavelength and cell were deduced by SADABS from the
 direction cosines etc. They are given here for emergency use only:
 CELL 0.71241   11.247   12.706   15.739   83.608   78.467   83.147
;
_shelx_res_checksum              5153
_shelx_hkl_checksum              88530