Crystal structure of an unknown tetrahydrofuran solvate of tetrakis(<i>{μ</i>}~3~-cyanato-κ^3^<i>N</i>:<i>N</i>:<i>N</i>)tetrakis[(triphenylphosphane-κ<i>P</i>)silver(I)]
Frenzel, Peter; Schaarschmidt, Dieter; Jakob, Alexander; Lang, Heinrich; Acta Crystallographica Section E 71 (2015) 1262–1265; doi:10.1107/S2056989015017636

data_2241170
_publ_section_title
;
 Crystal structure of an unknown tetrahydrofuran solvate of
 tetrakis(<i>{\m</i>}~3~-cyanato-\k^3^<i>N</i>:<i>N</i>:<i>N</i>)tetrakis[(triphenylphosphane-\k<i>P</i>)silver(I)]
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1262
_journal_page_last               1265
_journal_paper_doi               10.1107/S2056989015017636
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ag4 (C N O)4 (C18 H15 P)4]'
_chemical_formula_moiety         'C76 H60 Ag4 N4 O4 P4'
_chemical_formula_sum            'C76 H60 Ag4 N4 O4 P4'
_chemical_formula_weight         1648.64
_chemical_name_systematic
Tetrakis(\m~3~-cyanato-\k^3^<i>N</i>)tetrakis[(triphenylphosphane-\k<i>P</i>)silver(I)]
_space_group_crystal_system      tetragonal
_space_group_IT_number           81
_space_group_name_Hall           'P -4'
_space_group_name_H-M_alt        'P -4'
_symmetry_space_group_name_Hall  'P -4'
_symmetry_space_group_name_H-M   'P -4'
_atom_sites_solution_hydrogens   geom
_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                   24.0846(3)
_cell_length_b                   24.0846(3)
_cell_length_c                   15.2037(3)
_cell_measurement_reflns_used    20599
_cell_measurement_temperature    110
_cell_measurement_theta_max      27.9850
_cell_measurement_theta_min      3.3080
_cell_volume                     8819.2(2)
_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), SHELXTL (Sheldrick, 2008),
PLATON
(Spek, 2009), SQUEEZE (Spek, 2015)
;
_computing_publication_material
;
WINGX (Farrugia, 2012), publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS2013 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      110
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.918
_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  0.0482
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            105239
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.644
_diffrn_reflns_theta_min         2.934
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 10
_diffrn_standards_number         50
_exptl_absorpt_coefficient_mu    0.989
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91216
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis RED</i>; Oxford Diffraction, 2006)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.242
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.677
_refine_diff_density_min         -1.882
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 5170 quotients
[(<i>I</i>^+^)--(<i>I</i>^--^)]/[(<i>I</i>^+^)+(<i>I</i>^--^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.023(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1018
_refine_ls_number_reflns         20082
_refine_ls_number_restraints     1206
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0833
_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
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+1.5343P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                12667
_reflns_number_total             20082
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5201sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        8819.2(3)
_cod_database_code               2241170
_cod_database_fobs_code          2241170
_shelx_hkl_checksum              43605
_shelx_res_checksum              60412
_shelx_fab_checksum              36266
_shelxl_version_number           .2013