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_4349401
_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         'C58 H62 Ag2 N6 P8 Se4, 2(C F3 O3 S)'
_chemical_formula_sum            'C60 H62 Ag2 F6 N6 O6 P8 S2 Se4'
_chemical_formula_weight         1920.61
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-09-28
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.5846(3)
_cell_length_b                   14.59839(18)
_cell_length_c                   24.2899(3)
_cell_measurement_reflns_used    28490
_cell_measurement_temperature    193.15
_cell_measurement_theta_max      31.7970
_cell_measurement_theta_min      3.5520
_cell_volume                     7299.16(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      193.15
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.0696
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
;
  1 omega   -4.00   63.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3625   77.0000 -120.0000 67

  2 omega   42.00   75.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3625 -112.0000 -151.0000 33

  3 omega  -41.00   45.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -       26.3625  -57.0000  150.0000 86

  4 omega  -51.00   42.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438   77.0000   60.0000 93

  5 omega  -95.00    0.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438  -77.0000   30.0000 95

  6 omega  -74.00    0.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438  112.0000  -58.0000 74

  7 omega  -47.00   35.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438   77.0000 -120.0000 82

  8 omega  -97.00    1.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438  -77.0000  120.0000 98

  9 omega  -92.00    3.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438  -77.0000  -60.0000 95

 10 omega -100.00  -60.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438 -178.0000    0.0000 40

 11 omega  -88.00    3.00   1.0000   22.5000
omega____ theta____ kappa____ phi______ frames
    -      -27.1438  -19.0000  120.0000 91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0067409000
_diffrn_orient_matrix_UB_12      0.0463303000
_diffrn_orient_matrix_UB_13      -0.0066451000
_diffrn_orient_matrix_UB_21      0.0058693000
_diffrn_orient_matrix_UB_22      -0.0127324000
_diffrn_orient_matrix_UB_23      -0.0277567000
_diffrn_orient_matrix_UB_31      -0.0332646000
_diffrn_orient_matrix_UB_32      0.0071607000
_diffrn_orient_matrix_UB_33      -0.0062528000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            122835
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         28.280
_diffrn_reflns_theta_min         3.386
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.831
_exptl_absorpt_correction_T_max  0.514
_exptl_absorpt_correction_T_min  0.312
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.748
_exptl_crystal_description       block
_exptl_crystal_F_000             3792
_exptl_crystal_size_max          0.5597
_exptl_crystal_size_mid          0.377
_exptl_crystal_size_min          0.3416
_refine_diff_density_max         1.230
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.079
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         9048
_refine_ls_number_restraints     32
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0309P)^2^+9.5093P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0698
_refine_ls_wR_factor_ref         0.0747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7768
_reflns_number_total             9048
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag2{(PPh)4Se2(NMe)2}EtCN2][OTf]2_file036_file013.cif'
_cod_data_source_block           Ag2Se
_cod_original_cell_volume        7299.16(16)
_cod_database_code               4349401
_chemical_oxdiff_formula         'C53 H52 O6 F6 N4 P8 S2 Se4 Ag2'
_reflns_odcompleteness_completeness 99.69
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     28.22
_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
 C29A-C28 \\sim C29B-C28
 with sigma of 0.02
 C30A-C29A \\sim C30B-C29B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C29A \\sim C29B \\sim C30A \\sim C30B: within 1.7A with sigma of 0.01 and sigma
for terminal atoms of 0.02
4. Others
 Sof(C30B)=Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(C29B)=Sof(H29A)=Sof(H29B)=1-FVAR(1)
 Sof(C29A)=Sof(H29C)=Sof(H29D)=Sof(C30A)=Sof(H30D)=Sof(H30E)=Sof(H30F)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C29B(H29A,H29B), C29A(H29C,H29D)
5.b Aromatic/amide H refined with riding coordinates:
 C4(H4), C26(H26), C25(H25), C8(H8), C20(H20), C16(H16), C14(H14), C5(H5),
 C22(H22), C24(H24), C23(H23), C18(H18), C12(H12), C10(H10), C19(H19), C17(H17),
  C7(H7), C6(H6), C13(H13), C11(H11)
5.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C1(H1A,H1B,H1C), C30B(H30A,H30B,H30C), C30A(H30D,H30E,H30F)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'