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_4349406
_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
'C52 H52 Ag N4 P8 S4, C F3 O3 S, 3(C4 H8 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C66 H77.5 Ag F3 N4.5 O6 P8 S5'
_chemical_formula_weight         1602.75
_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_Hall           'P 2 2ab'
_space_group_name_H-M_alt        'P 21 21 2'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-02-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.0999(3)
_cell_length_b                   25.8868(3)
_cell_length_c                   10.92456(9)
_cell_measurement_reflns_used    33989
_cell_measurement_temperature    99.98(13)
_cell_measurement_theta_max      76.4060
_cell_measurement_theta_min      3.7830
_cell_volume                     7381.10(13)
_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 0.998
_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    -59.00  29.00   0.50    3.50    --  -38.50  38.00 -90.00  176
  2  \w     62.00 113.00   0.50    3.50    --   42.50  38.00 -90.00  102
  3  \w    111.00 155.00   0.50   14.00    --  111.00 125.00-150.00   88
  4  \w    123.00 156.00   0.50   14.00    --  111.00 125.00-180.00   66
  5  \w    127.00 152.00   0.50   14.00    --  111.00  77.00-150.00   50
  6  \w    130.00 178.00   0.50   14.00    --  111.00  61.00 -60.00   96
  7  \w    131.00 178.00   0.50   14.00    --  111.00   0.00-150.00   94
  8  \w     98.00 173.00   0.50   14.00    --  111.00  45.00 -30.00  150
  9  \w     94.00 166.00   0.50   14.00    --  111.00 125.00  90.00  144
 10  \w    117.00 165.00   0.50   14.00    --  111.00 125.00 150.00   96
 11  \w     99.00 133.00   0.50   14.00    --  111.00  45.00  90.00   68
 12  \w     82.00 116.00   0.50   14.00    --  111.00 -30.00  30.00   68
 13  \w     83.00 109.00   0.50   14.00    --  111.00 -94.00 -60.00   52
 14  \w     84.00 127.00   0.50   14.00    --  111.00 -30.00-120.00   86
 15  \w     91.00 157.00   0.50   14.00    --  111.00  30.00 -90.00  132
 16  \w     95.00 173.00   0.50   14.00    --  111.00 125.00   0.00  156
 17  \w     88.00 115.00   0.50   14.00    --  111.00  61.00 -60.00   54
 18  \w     83.00 164.00   0.50   14.00    --  111.00  61.00 -90.00  162
 19  \w     80.00 108.00   0.50   14.00    --  111.00  77.00-150.00   56
 20  \w     31.00  86.00   0.50   14.00    --  111.00   0.00-150.00  110
 21  \w     54.00  81.00   0.50   14.00    --  111.00 -30.00-120.00   54
 22  \w     41.00 106.00   0.50   14.00    --  111.00 -94.00 -90.00  130
 23  \w     50.00 101.00   0.50   14.00    --  111.00 -94.00   0.00  102
 24  \w     79.00 106.00   0.50   14.00    --  111.00 -94.00 120.00   54
 25  \w     95.00 121.00   0.50   14.00    --  111.00-125.00 120.00   52
 26  \w     42.00  79.00   0.50   14.00    --  111.00-125.00  60.00   74
 27  \w     39.00 117.00   0.50   14.00    --  111.00-125.00  90.00  156
 28  \w     39.00 120.00   0.50   14.00    --  111.00-125.00 150.00  162
 29  \w     39.00  92.00   0.50   14.00    --  111.00 -77.00 150.00  106
 30  \w     44.00  91.00   0.50   14.00    --  111.00-125.00 120.00   94
 31  \w     33.00 109.00   0.50   14.00    --  111.00 -94.00 150.00  152
 32  \w     21.00  81.00   0.50    3.50    --   42.50 -99.00   0.00  120
 33  \w    -87.00  -2.00   0.50    3.50    --  -38.50 125.00 120.00  170
 34  \w   -111.00 -16.00   0.50    3.50    --  -38.50 -38.00 -60.00  190
 35  \w   -110.00 -54.00   0.50    3.50    --  -38.50-153.00 -25.00  112
;
_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      -0.0584040000
_diffrn_orient_matrix_UB_12      -0.0083243000
_diffrn_orient_matrix_UB_13      -0.0057239000
_diffrn_orient_matrix_UB_21      0.0055288000
_diffrn_orient_matrix_UB_22      -0.0491536000
_diffrn_orient_matrix_UB_23      0.0785231000
_diffrn_orient_matrix_UB_31      -0.0065788000
_diffrn_orient_matrix_UB_32      0.0324683000
_diffrn_orient_matrix_UB_33      0.1170242000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0828
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            88268
_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         76.577
_diffrn_reflns_theta_min         2.404
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.645
_exptl_absorpt_correction_T_max  0.849
_exptl_absorpt_correction_T_min  0.399
_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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.442
_exptl_crystal_description       needle
_exptl_crystal_F_000             3308
_exptl_crystal_size_max          0.325
_exptl_crystal_size_mid          0.046
_exptl_crystal_size_min          0.031
_refine_diff_density_max         2.810
_refine_diff_density_min         -1.920
_refine_diff_density_rms         0.129
_refine_ls_abs_structure_details
;
 Flack x determined using 6070 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.015(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     770
_refine_ls_number_reflns         15468
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0568
_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^)+(0.1081P)^2^+5.2430P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1497
_refine_ls_wR_factor_ref         0.1554
_reflns_Friedel_coverage         0.817
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                14529
_reflns_number_total             15468
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag{(PPh)4S2(NMe)2}][OTf]x0.5MeCNx3THF_file001.cif'
_cod_data_source_block           AgS-THF
_cod_original_cell_volume        7381.09(13)
_cod_original_formula_sum        'C66 H77.50 Ag F3 N4.50 O6 P8 S5'
_cod_database_code               4349406
_chemical_oxdiff_formula         C264H310Ag4F12N18O24P32S20
_reflns_odcompleteness_completeness 99.96
_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. Restrained distances
 O4-C59 = O4-C56 = O5-C60 = O5-C63 = O6-C67 = O6-C64
 1.435 with sigma of 0.02
 C60-C61 = C61-C62 = C63-C62 = C65-C64 = C66-C65 = C67-C66 = C59-C58 = C58-C57
 = C57-C56
 1.531 with sigma of 0.02
3. Same fragment restrains
{O5, C60, C61, C62, C63} sigma for 1-2: 0.02, 1-3: 0.02
{O4, C56, C57, C58, C59} sigma for 1-2: 0.02, 1-3: 0.02
as
{O6, C64, C65, C66, C67}
4. Others
 Fixed Sof: N5(0.5) C54(0.5) C55(0.5) H55A(0.5) H55B(0.5) H55C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C64(H64A,H64B), C65(H65A,H65B), C66(H66A,H66B), C67(H67A,H67B), C56(H56A,
 H56B), C57(H57A,H57B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,H60B),
 C61(H61A,H61B), C62(H62A,H62B), C63(H63A,H63B)
5.b Me refined with riding coordinates:
 C55(H55A,H55B,H55C)
5.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C8(H8), C9(H9), C10(H10), C11(H11),
 C12(H12), C14(H14), C15(H15), C16(H16), C17(H17), C18(H18), C20(H20), C21(H21),
  C22(H22), C23(H23), C24(H24), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C40(H40), C41(H41),
  C42(H42), C43(H43), C44(H44), C46(H46), C47(H47), C48(H48), C49(H49), C50(H50)
5.d Idealised Me refined as rotating group:
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C51(H51A,H51B,H51C), C52(H52A,H52B,
 H52C)
;
_shelx_res_checksum              41511
_shelx_hkl_checksum              81904
_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 1.695
_oxdiff_exptl_absorpt_empirical_full_min 0.538