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_4349411
_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_absolute_configuration ad
_chemical_formula_moiety         'C26 H26 N2 P4 S2'
_chemical_formula_sum            'C26 H26 N2 P4 S2'
_chemical_formula_weight         554.49
_chemical_name_systematic
3,7-dimethyl-2,4,6,8-tetraphenyl-1,5,3,7,2,4,6,8-dithiadiazatetraphosphocane
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 113.0921(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.08745(9)
_cell_length_b                   11.01972(7)
_cell_length_c                   11.82438(10)
_cell_measurement_reflns_used    20194
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      76.3260
_cell_measurement_theta_min      3.9950
_cell_volume                     1328.95(2)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 0.997
_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     25.00  80.00   0.50    1.00    --   42.75  38.00 -90.00  110
  2  \w     90.00 115.00   0.50    1.00    --   42.75  38.00 -90.00   50
  3  \w     68.00  96.00   0.50    1.00    --   42.75  77.00 -60.00   56
  4  \w     66.00 117.00   0.50    1.00    --   42.75  77.00   0.00  102
  5  \w     92.00 117.00   0.50    1.00    --   42.75  77.00  60.00   50
  6  \w     57.00 120.00   0.50    1.00    --   42.75  19.00 150.00  126
  7  \w    133.00 169.00   0.50    4.00    --  111.00  61.00  30.00   72
  8  \w    131.00 173.00   0.50    4.00    --  111.00  77.00 -30.00   84
  9  \w    137.00 164.00   0.50    4.00    --  111.00  45.00-120.00   54
 10  \w    118.00 176.00   0.50    4.00    --  111.00  77.00-150.00  116
 11  \w    115.00 150.00   0.50    4.00    --  111.00  77.00 -60.00   70
 12  \w     87.00 120.00   0.50    4.00    --  111.00  45.00-120.00   66
 13  \w     84.00 111.00   0.50    4.00    --  111.00  61.00-120.00   54
 14  \w     83.00 109.00   0.50    4.00    --  111.00  61.00-150.00   52
 15  \w     84.00 124.00   0.50    4.00    --  111.00  61.00-180.00   80
 16  \w     80.00 171.00   0.50    4.00    --  111.00  77.00-180.00  182
 17  \w     80.00 106.00   0.50    4.00    --  111.00  77.00 -30.00   52
 18  \w     84.00 128.00   0.50    4.00    --  111.00  61.00 -60.00   88
 19  \w     83.00 110.00   0.50    4.00    --  111.00  61.00  30.00   54
 20  \w     83.00 130.00   0.50    4.00    --  111.00  61.00   0.00   94
 21  \w     83.00 156.00   0.50    4.00    --  111.00  61.00 -30.00  146
 22  \w     83.00 175.00   0.50    4.00    --  111.00  61.00  90.00  184
 23  \w    153.00 178.00   0.50    4.00    --  111.00  61.00 120.00   50
 24  \w    128.00 178.00   0.50    4.00    --  111.00  61.00 150.00  100
 25  \w     87.00 126.00   0.50    4.00    --  111.00  45.00  60.00   78
 26  \w     80.00 177.00   0.50    4.00    --  111.00  77.00 120.00  194
 27  \w     80.00 170.00   0.50    4.00    --  111.00  77.00   0.00  180
 28  \w     84.00 111.00   0.50    4.00    --  111.00  61.00 150.00   54
 29  \w     83.00 116.00   0.50    4.00    --  111.00  61.00 120.00   66
 30  \w     83.00 162.00   0.50    4.00    --  111.00  61.00  60.00  158
 31  \w     84.00 177.00   0.50    4.00    --  111.00  61.00 -90.00  186
 32  \w     80.00 106.00   0.50    4.00    --  111.00  77.00 -60.00   52
 33  \w     80.00 130.00   0.50    4.00    --  111.00  77.00-120.00  100
 34  \w     81.00 108.00   0.50    4.00    --  111.00  77.00-150.00   54
 35  \w     80.00 106.00   0.50    4.00    --  111.00  77.00 -90.00   52
 36  \w     80.00 107.00   0.50    4.00    --  111.00  77.00  60.00   54
 37  \w     80.00 106.00   0.50    4.00    --  111.00  77.00  90.00   52
 38  \w     80.00 115.00   0.50    4.00    --  111.00  77.00 150.00   70
 39  \w     16.00  61.00   0.50    1.00    --   42.75  77.00   0.00   90
 40  \w     11.00  66.00   0.50    1.00    --   42.75  77.00 -60.00  110
 41  \w     11.00  62.00   0.50    1.00    --   42.75  77.00-150.00  102
 42  \w     42.00 131.00   0.50    4.00    --  111.00 -45.00-150.00  178
 43  \w     94.00 121.00   0.50    4.00    --  111.00-125.00-180.00   54
 44  \w     73.00 138.00   0.50    4.00    --  111.00 -61.00 -90.00  130
 45  \w     79.00 121.00   0.50    4.00    --  111.00-125.00 -30.00   84
 46  \w     87.00 121.00   0.50    4.00    --  111.00-125.00  60.00   68
 47  \w     36.00  97.00   0.50    4.00    --  111.00 -94.00  60.00  122
 48  \w     42.00 118.00   0.50    4.00    --  111.00-125.00 150.00  152
 49  \w     24.00  80.00   0.50    1.00    --   42.75-125.00 120.00  112
 50  \w      6.00  53.00   0.50    1.00    --   42.75  19.00 150.00   94
 51  \w     11.00  67.00   0.50    1.00    --   42.75  77.00  60.00  112
 52  \w     15.00  64.00   0.50    1.00    --   42.75  77.00 120.00   98
 53  \w    -59.00  32.00   0.50    1.00    --  -38.50  38.00  60.00  182
 54  \w      6.00  81.00   0.50    1.00    --   42.75 -99.00 -90.00  150
 55  \w     54.00  89.00   0.50    4.00    --  111.00-125.00-180.00   70
 56  \w     43.00  99.00   0.50    4.00    --  111.00 -77.00-150.00  112
 57  \w     30.00 107.00   0.50    4.00    --  111.00 -94.00-180.00  154
 58  \w    -58.00 -13.00   0.50    1.00    --  -38.50 -19.00-180.00   90
 59  \w    -60.00  32.00   0.50    1.00    --  -38.50  57.00-180.00  184
;
_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      0.0186615000
_diffrn_orient_matrix_UB_12      0.1231261000
_diffrn_orient_matrix_UB_13      -0.0526965000
_diffrn_orient_matrix_UB_21      0.1471779000
_diffrn_orient_matrix_UB_22      -0.0027775000
_diffrn_orient_matrix_UB_23      0.0833965000
_diffrn_orient_matrix_UB_31      0.0285464000
_diffrn_orient_matrix_UB_32      -0.0660788000
_diffrn_orient_matrix_UB_33      -0.1016307000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0170
_diffrn_reflns_av_unetI/netI     0.0116
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            23842
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.560
_diffrn_reflns_theta_min         4.012
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.238
_exptl_absorpt_correction_T_max  0.698
_exptl_absorpt_correction_T_min  0.503
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.386
_exptl_crystal_description       block
_exptl_crystal_F_000             576
_exptl_crystal_size_max          0.244
_exptl_crystal_size_mid          0.202
_exptl_crystal_size_min          0.123
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.166
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.482(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         5394
_refine_ls_number_restraints     722
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0275
_refine_ls_R_factor_gt           0.0274
_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^)+(0.0562P)^2^+0.2178P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0778
_refine_ls_wR_factor_ref         0.0779
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5388
_reflns_number_total             5394
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            S-8-Ring_file024_file038.cif
_cod_data_source_block           S-8-ring
_cod_database_code               4349411
_chemical_oxdiff_formula         'C52 H52 N4 P8 S4 '
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.518(19) 0.482(19)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Uiso/Uaniso restraints and constraints
C1A \\sim C2A \\sim C3A \\sim C4A \\sim C5A \\sim C6A \\sim C7A \\sim C8A \\sim
C9A \\sim C10A \\sim C11A \\sim C12A \\sim C13A \\sim C14A \\sim C15A \\sim
C16A \\sim C17A \\sim C18A \\sim C19A \\sim C20A \\sim C21A \\sim C22A \\sim
C23A \\sim C24A \\sim C12B \\sim C4B \\sim C20B \\sim C8B \\sim C16B \\sim C24B
\\sim C2B \\sim C6B \\sim C10B \\sim C14B \\sim C18B \\sim C22B \\sim C1B \\sim
C3B \\sim C5B \\sim C7B \\sim C9B \\sim C11B \\sim C13B \\sim C15B \\sim C17B
\\sim C19B \\sim C21B \\sim C23B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C20A) = Uanis(C20B)
Uanis(C7A) = Uanis(C7B)
4. Others
 Sof(C26B)=Sof(H26D)=Sof(H26E)=Sof(H26F)=Sof(C1B)=Sof(C6B)=Sof(H6B)=Sof(C5B)=
 Sof(H5B)=Sof(C4B)=Sof(H4B)=Sof(C3B)=Sof(H3B)=Sof(C2B)=Sof(H2B)=Sof(C7B)=
 Sof(C8B)=Sof(H8B)=Sof(C9B)=Sof(H9B)=Sof(C10B)=Sof(H10B)=Sof(C11B)=Sof(H11B)=
 Sof(C12B)=Sof(H12B)=Sof(C13B)=Sof(C14B)=Sof(H14B)=Sof(C15B)=Sof(H15B)=
 Sof(C16B)=Sof(H16B)=Sof(C17B)=Sof(H17B)=Sof(C18B)=Sof(H18B)=Sof(C19B)=
 Sof(C20B)=Sof(H20B)=Sof(C21B)=Sof(H21B)=Sof(C22B)=Sof(H22B)=Sof(C23B)=
 Sof(H23B)=Sof(C24B)=Sof(H24B)=Sof(C25B)=Sof(H25D)=Sof(H25E)=Sof(H25F)=Sof(S1B)=
 Sof(S2B)=Sof(P1B)=Sof(P2B)=Sof(P3B)=Sof(P4B)=1-FVAR(1)
 Sof(S1A)=Sof(S2A)=Sof(P1A)=Sof(P2A)=Sof(P3A)=Sof(P4A)=Sof(C1A)=Sof(C2A)=
 Sof(H2A)=Sof(C3A)=Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=
 Sof(H6A)=Sof(C7A)=Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(H9A)=Sof(C10A)=Sof(H10A)=
 Sof(C11A)=Sof(H11A)=Sof(C12A)=Sof(H12A)=Sof(C13A)=Sof(C14A)=Sof(H14A)=
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=
 Sof(H18A)=Sof(C19A)=Sof(C20A)=Sof(H20A)=Sof(C21A)=Sof(H21A)=Sof(C22A)=
 Sof(H22A)=Sof(C23A)=Sof(H23A)=Sof(C24A)=Sof(H24A)=Sof(C25A)=Sof(H25A)=
 Sof(H25B)=Sof(H25C)=Sof(C26A)=Sof(H26A)=Sof(H26B)=Sof(H26C)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A), C8A(H8A), C9A(H9A),
 C10A(H10A), C11A(H11A), C12A(H12A), C14A(H14A), C15A(H15A), C16A(H16A),
 C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A), C22A(H22A), C23A(H23A),
 C24A(H24A), C6B(H6B), C5B(H5B), C4B(H4B), C3B(H3B), C2B(H2B), C8B(H8B),
 C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B), C14B(H14B), C15B(H15B),
 C16B(H16B), C17B(H17B), C18B(H18B), C20B(H20B), C21B(H21B), C22B(H22B),
 C23B(H23B), C24B(H24B)
5.b Fitted hexagon refined as free rotating group:
 C1A(C2A,C3A,C4A,C5A,C6A), C7A(C8A,C9A,C10A,C11A,C12A), C13A(C14A,C15A,C16A,
 C17A,C18A), C19A(C20A,C21A,C22A,C23A,C24A), C1B(C6B,C5B,C4B,C3B,C2B), C7B(C8B,
 C9B,C10B,C11B,C12B), C13B(C14B,C15B,C16B,C17B,C18B), C19B(C20B,C21B,C22B,C23B,
 C24B)
5.c Idealised Me refined as rotating group:
 C25A(H25A,H25B,H25C), C26A(H26A,H26B,H26C), C26B(H26D,H26E,H26F), C25B(H25D,
 H25E,H25F)
;
_shelx_res_checksum              41493
_shelx_hkl_checksum              74133
_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 1.199
_oxdiff_exptl_absorpt_empirical_full_min 0.821