Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of Polynuclear Silver(I) Sandwich Complexes.
Yogendra, Sivathmeehan; Hennersdorf, Felix; Weigand, Jan J.; Inorganic chemistry 56 (2017) 8698–8704; doi:10.1021/acs.inorgchem.7b00141

data_4349407
_publ_section_title
;
 Nitrogen-Phosphorus(III)-Chalcogen Macrocycles for the Synthesis of
 Polynuclear Silver(I) Sandwich Complexes.
;
_journal_issue                   15
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8698
_journal_page_last               8704
_journal_paper_doi               10.1021/acs.inorgchem.7b00141
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C56 H52 Ag4 F12 N4 O12 P8 S8, 5(C2 H4 Cl2)'
_chemical_formula_sum            'C66 H72 Ag4 Cl10 F12 N4 O12 P8 S8'
_chemical_formula_weight         2631.49
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2015-10-18
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 91.735(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.9653(4)
_cell_length_b                   28.0732(4)
_cell_length_c                   17.7396(3)
_cell_measurement_reflns_used    16437
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      76.2070
_cell_measurement_theta_min      3.7410
_cell_volume                     9440.5(3)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     29.00 110.00   1.00    2.50    --   42.75  38.00 -30.00   81
  2  \w     51.00 115.00   1.00    2.50    --   42.75  38.00-120.00   64
  3  \w     84.00 167.00   1.00   10.00    --  111.00  61.00-180.00   83
  4  \w     96.00 123.00   1.00   10.00    --  111.00 125.00 -30.00   27
  5  \w    147.00 174.00   1.00   10.00    --  111.00 125.00 -30.00   27
  6  \w    130.00 171.00   1.00   10.00    --  111.00 125.00  60.00   41
  7  \w    152.00 178.00   1.00   10.00    --  111.00  61.00  90.00   26
  8  \w    121.00 175.00   1.00   10.00    --  111.00  61.00  30.00   54
  9  \w    107.00 173.00   1.00   10.00    --  111.00 125.00  90.00   66
 10  \w     94.00 127.00   1.00   10.00    --  111.00 125.00  60.00   33
 11  \w     83.00 170.00   1.00   10.00    --  111.00  61.00  60.00   87
 12  \w     87.00 114.00   1.00   10.00    --  111.00  61.00  30.00   27
 13  \w     83.00 135.00   1.00   10.00    --  111.00  61.00  90.00   52
 14  \w     87.00 178.00   1.00   10.00    --  111.00  45.00 150.00   91
 15  \w     86.00 141.00   1.00   10.00    --  111.00 -77.00   0.00   55
 16  \w     85.00 121.00   1.00   10.00    --  111.00-125.00  30.00   36
 17  \w     96.00 121.00   1.00   10.00    --  111.00-125.00 120.00   25
 18  \w     90.00 117.00   1.00   10.00    --  111.00-125.00 150.00   27
 19  \w     56.00  94.00   1.00   10.00    --  111.00 -94.00 120.00   38
 20  \w     42.00 127.00   1.00   10.00    --  111.00 -61.00  90.00   85
 21  \w     79.00 106.00   1.00   10.00    --  111.00 -94.00   0.00   27
 22  \w     45.00  73.00   1.00   10.00    --  111.00-125.00  30.00   28
 23  \w     44.00  85.00   1.00   10.00    --  111.00 -77.00   0.00   41
 24  \w     44.00 108.00   1.00   10.00    --  111.00 -94.00 -90.00   64
 25  \w     90.00 120.00   1.00   10.00    --  111.00-125.00-150.00   30
 26  \w     39.00 121.00   1.00   10.00    --  111.00-125.00 -90.00   82
 27  \w     44.00  72.00   1.00    2.50    --   42.75-125.00  90.00   28
 28  \w     24.00  83.00   1.00    2.50    --   42.75 -99.00 -90.00   59
 29  \w    -61.00  31.00   1.00    2.50    --  -38.50  57.00-180.00   92
 30  \w   -109.00 -12.00   1.00    2.50    --  -38.50 -57.00  30.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0591400000
_diffrn_orient_matrix_UB_12      -0.0317668000
_diffrn_orient_matrix_UB_13      -0.0299545000
_diffrn_orient_matrix_UB_21      0.0554890000
_diffrn_orient_matrix_UB_22      0.0362812000
_diffrn_orient_matrix_UB_23      0.0288587000
_diffrn_orient_matrix_UB_31      0.0050706000
_diffrn_orient_matrix_UB_32      -0.0261921000
_diffrn_orient_matrix_UB_33      0.0762967000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_unetI/netI     0.0217
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18591
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.762
_diffrn_reflns_theta_min         2.813
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    12.808
_exptl_absorpt_correction_T_max  0.667
_exptl_absorpt_correction_T_min  0.130
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Analytical numeric absorption correction using a multifaceted crystal
			model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       block
_exptl_crystal_F_000             5224
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.034
_refine_diff_density_max         2.605
_refine_diff_density_min         -1.475
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     562
_refine_ls_number_reflns         18591
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0598
_refine_ls_R_factor_gt           0.0495
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1075P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1488
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14929
_reflns_number_total             18591
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 179.9586\% 
 around [-0.03 -0.00 1.00] (reciprocal) or [0.00 -0.00 1.00] (direct)
;
_cod_data_source_file
'[Ag4{(PPh)4S2(NMe)2}][OTf]4x5C2H4Cl2_file013_file032.cif'
_cod_data_source_block           Ag4S
_cod_database_code               4349407
_chemical_oxdiff_formula         C66H72Ag4Cl12F12N4O12P8S6
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.5807(8) 0.4193(8)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C33(H33A,H33B), C29(H29A,H29B), C30(H30A,H30B), C32(H32A,H32B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C13(H13), C16(H16), C9(H9), C26(H26), C22(H22), C10(H10), C17(H17), C15(H15),
 C11(H11), C19(H19), C23(H23), C18(H18), C12(H12), C3(H3), C25(H25), C6(H6),
 C2(H2), C4(H4), C24(H24), C5(H5)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C7(H7A,H7B,H7C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.656
_oxdiff_exptl_absorpt_empirical_full_min 0.706
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2