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_4349410
_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
'C52 H52 Ag2 N4 P8 S4, 2(C F3 O3 S), C H2 Cl2'
_chemical_formula_sum            'C55 H54 Ag2 Cl2 F6 N4 O6 P8 S6'
_chemical_formula_weight         1707.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-06
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 94.1997(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   10.89505(8)
_cell_length_b                   16.55095(12)
_cell_length_c                   18.80048(13)
_cell_measurement_reflns_used    14902
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.3200
_cell_measurement_theta_min      4.5380
_cell_volume                     3381.06(4)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.990
_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     10.00  65.00   1.00    1.00    --   42.50 -38.00 120.00   55
  2  \w     72.00 178.00   1.00    4.00    --  111.00  15.00  90.00  106
  3  \w    131.00 178.00   1.00    4.00    --  111.00  30.00 120.00   47
  4  \w    103.00 177.00   1.00    4.00    --  111.00 125.00 150.00   74
  5  \w     94.00 135.00   1.00    4.00    --  111.00 -30.00  60.00   41
  6  \w     70.00  97.00   1.00    4.00    --  111.00 -94.00 -60.00   27
  7  \w    106.00 138.00   1.00    4.00    --  111.00 -61.00-120.00   32
  8  \w     86.00 139.00   1.00    4.00    --  111.00 -61.00-180.00   53
  9  \w     50.00  94.00   1.00    4.00    --  111.00 -94.00 -30.00   44
 10  \w     51.00 139.00   1.00    4.00    --  111.00 -61.00  30.00   88
 11  \w     41.00  91.00   1.00    4.00    --  111.00-107.00-129.00   50
 12  \w     40.00  91.00   1.00    4.00    --  111.00 -45.00-150.00   51
 13  \w     30.00 108.00   1.00    4.00    --  111.00 -94.00-120.00   78
 14  \w    -40.00   0.00   1.00    1.00    --  -38.50  38.00-180.00   40
 15  \w    -69.00 -17.00   1.00    1.00    --  -38.50  77.00 -60.00   52
 16  \w    -68.00  34.00   1.00    1.00    --  -38.50  77.00  60.00  102
;
_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      0.1360277000
_diffrn_orient_matrix_UB_12      0.0154597000
_diffrn_orient_matrix_UB_13      0.0247473000
_diffrn_orient_matrix_UB_21      0.0139323000
_diffrn_orient_matrix_UB_22      -0.0889654000
_diffrn_orient_matrix_UB_23      0.0233215000
_diffrn_orient_matrix_UB_31      0.0377744000
_diffrn_orient_matrix_UB_32      -0.0226645000
_diffrn_orient_matrix_UB_33      -0.0747352000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0228
_diffrn_reflns_av_unetI/netI     0.0250
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            19726
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.556
_diffrn_reflns_theta_min         3.562
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.478
_exptl_absorpt_correction_T_max  0.549
_exptl_absorpt_correction_T_min  0.208
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
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    1.677
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     417
_refine_ls_number_reflns         7032
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0250
_refine_ls_R_factor_gt           0.0245
_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^)+(0.0326P)^2^+2.3480P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0625
_refine_ls_wR_factor_ref         0.0629
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6875
_reflns_number_total             7032
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag2{(PPh)4S2(NMe)2}][OTf]2x2CH2Cl2_file042_file025.cif'
_cod_data_source_block           Ag2S
_cod_database_code               4349410
_chemical_oxdiff_formula         'C108 H104 Ag4 F12 N8 O12 P16 S12 '
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. 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
2. Others
 Fixed Sof: Cl1(0.5) C22(0.5) H22A(0.5) H22B(0.5) Cl2(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C22(H22A,H22B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C8(H8), C00N(H00N), C3(H3), C9(H9), C4(H4), C5(H5), C10(H10),
 C00W(H00W), C00X(H00X), C18(H18), C14(H14), C010(H010), C12(H12), C15(H15),
 C013(H013), C11(H11), C16(H16), C17(H17)
3.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_shelx_res_checksum              91611
_shelx_hkl_checksum              82278
_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 1.417
_oxdiff_exptl_absorpt_empirical_full_min 0.695