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_4349408
_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 Ag N4 P8 Se4, C F3 O3 S'
_chemical_formula_sum            'C53 H52 Ag F3 N4 O3 P8 S Se4'
_chemical_formula_weight         1553.51
_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             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                 106.3674(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.99198(14)
_cell_length_b                   15.06651(12)
_cell_length_c                   24.3428(2)
_cell_measurement_reflns_used    24973
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      76.3370
_cell_measurement_theta_min      3.9790
_cell_volume                     5979.44(9)
_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      99.98(13)
_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 0.995
_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    -24.00  62.00   0.50    0.50    --   42.50 -38.00  30.00  172
  2  \w      8.00  73.00   0.50    0.50    --   42.50 -99.00  30.00  130
  3  \w      4.00  39.00   0.50    0.50    --   42.50 -99.00 -30.00   70
  4  \w     30.00  76.00   0.50    2.00    --  111.00 -94.00-150.00   92
  5  \w     82.00 108.00   0.50    2.00    --  111.00 -94.00-150.00   52
  6  \w    111.00 136.00   0.50    2.00    --  111.00 -77.00-150.00   50
  7  \w     95.00 121.00   0.50    2.00    --  111.00-125.00 -30.00   52
  8  \w     85.00 121.00   0.50    2.00    --  111.00-125.00  30.00   72
  9  \w     64.00 107.00   0.50    2.00    --  111.00 -94.00 -90.00   86
 10  \w     62.00 134.00   0.50    2.00    --  111.00 -30.00 -90.00  144
 11  \w    103.00 130.00   0.50    2.00    --  111.00 -30.00   0.00   54
 12  \w     75.00 176.00   0.50    2.00    --  111.00  15.00 120.00  202
 13  \w     62.00  90.00   0.50    2.00    --  111.00 -30.00   0.00   56
 14  \w     52.00 105.00   0.50    2.00    --  111.00 -45.00  60.00  106
 15  \w     51.00  81.00   0.50    2.00    --  111.00-125.00 -30.00   60
 16  \w     57.00  84.00   0.50    2.00    --  111.00-125.00 -60.00   54
 17  \w     40.00 121.00   0.50    2.00    --  111.00-125.00-150.00  162
 18  \w     78.00 107.00   0.50    2.00    --  111.00 -94.00-180.00   58
 19  \w     75.00 147.00   0.50    2.00    --  111.00 -15.00-150.00  144
 20  \w     98.00 162.00   0.50    2.00    --  111.00  30.00-180.00  128
 21  \w     87.00 178.00   0.50    2.00    --  111.00  45.00-120.00  182
 22  \w     55.00 108.00   0.50    2.00    --  111.00-125.00  90.00  106
 23  \w     42.00  99.00   0.50    2.00    --  111.00 -77.00  90.00  114
 24  \w     39.00 121.00   0.50    2.00    --  111.00-125.00 120.00  164
 25  \w     43.00 136.00   0.50    2.00    --  111.00 -61.00 -60.00  186
 26  \w     44.00  73.00   0.50    2.00    --  111.00 -77.00-150.00   58
 27  \w     43.00 135.00   0.50    2.00    --  111.00 -45.00-180.00  184
 28  \w    -27.00  -2.00   0.50    0.50    --  -38.50 125.00 -60.00   50
 29  \w    -92.00 -12.00   0.50    0.50    --  -38.50 -57.00 -90.00  160
 30  \w    -22.00   9.00   0.50    0.50    --   42.50 -70.00 157.00   62
 31  \w   -109.00 -12.00   0.50    0.50    --  -38.50 -57.00-180.00  194
;
_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      -0.0041422000
_diffrn_orient_matrix_UB_12      0.0808007000
_diffrn_orient_matrix_UB_13      0.0378781000
_diffrn_orient_matrix_UB_21      -0.0426506000
_diffrn_orient_matrix_UB_22      -0.0574582000
_diffrn_orient_matrix_UB_23      0.0354990000
_diffrn_orient_matrix_UB_31      0.0841628000
_diffrn_orient_matrix_UB_32      -0.0250394000
_diffrn_orient_matrix_UB_33      0.0407480000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            31916
_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         76.534
_diffrn_reflns_theta_min         3.785
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.302
_exptl_absorpt_correction_T_max  0.413
_exptl_absorpt_correction_T_min  0.134
_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    1.726
_exptl_crystal_description       block
_exptl_crystal_F_000             3072
_exptl_crystal_size_max          0.359
_exptl_crystal_size_mid          0.245
_exptl_crystal_size_min          0.186
_refine_diff_density_max         2.537
_refine_diff_density_min         -1.995
_refine_diff_density_rms         0.124
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.220
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     390
_refine_ls_number_reflns         6261
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.220
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0592
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0127P)^2^+90.0766P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1267
_refine_ls_wR_factor_ref         0.1267
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6250
_reflns_number_total             6261
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag{(PPh)4Se2(NMe)2}][OTf]_file005_file009.cif'
_cod_data_source_block           AgSe
_cod_original_cell_volume        5979.43(9)
_cod_database_code               4349408
_chemical_oxdiff_formula         C53H52AgF3N4O3P8S1Se4
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: Ag1(0.5) S1(0.5) F2(0.5) O1(0.5) O3(0.5) F1(0.5) C27(0.5) F3(0.5)
 O2(0.5)
3.a Aromatic/amide H refined with riding coordinates:
 C20(H20), C8(H8), C14(H14), C24(H24), C21(H), C10(HA), C12(H12), C9(HB),
 C4(HC), C6(H6), C23(H23), C5(HD), C22(HE), C11(HF), C18(H18), C3(HG), C15(H15),
  C2(H2), C16(HH), C17(HI)
3.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C)
;
_shelx_res_checksum              24363
_shelx_hkl_checksum              30171
_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 1.739
_oxdiff_exptl_absorpt_empirical_full_min 0.608