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_4349404
_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
'C30 H32 Ag1.5 N4 P4 Se2, C28 H29 Ag1.5 N3.5 P4 Se2, 0.5(C6 H4 F2)'
_chemical_formula_sum            'C61 H63 Ag3 F N7.5 P8 Se4'
_chemical_formula_weight         1807.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-11-17
_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            8
_cell_length_a                   23.1914(7)
_cell_length_b                   15.5330(5)
_cell_length_c                   49.5060(16)
_cell_measurement_reflns_used    7182
_cell_measurement_temperature    293.03(10)
_cell_measurement_theta_max      71.9060
_cell_measurement_theta_min      3.5220
_cell_volume                     17833.6(10)
_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      air
_diffrn_ambient_temperature      293.03(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2850
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.974
_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   -109.00 -20.00   0.50   20.00    --  -38.50 -38.00 150.00  178
  2  \w    -88.00 -24.00   0.50   20.00    --  -38.50 125.00 120.00  128
  3  \w     23.00  52.00   0.50   20.00    --   42.50-125.00  90.00   58
  4  \w    106.00 171.00   0.50   80.00    --  111.00  30.00 120.00  130
  5  \w    103.00 145.00   0.50   80.00    --  111.00 106.00-156.00   84
  6  \w     40.00  88.00   0.50   80.00    --  111.00 -94.00-150.00   96
  7  \w     95.00 153.00   0.50   80.00    --  111.00 125.00-150.00  116
  8  \w     95.00 155.00   0.50   80.00    --  111.00 125.00 -60.00  120
  9  \w     39.00  79.00   0.50   80.00    --  111.00-125.00  30.00   80
 10  \w     57.00  97.00   0.50   80.00    --  111.00 -94.00-180.00   80
 11  \w     67.00 109.00   0.50   80.00    --  111.00  15.00  90.00   84
;
_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      0.0864950000
_diffrn_orient_matrix_UB_12      -0.0141261000
_diffrn_orient_matrix_UB_13      -0.0120824000
_diffrn_orient_matrix_UB_21      -0.0415159000
_diffrn_orient_matrix_UB_22      -0.0156381000
_diffrn_orient_matrix_UB_23      -0.0502708000
_diffrn_orient_matrix_UB_31      0.0248374000
_diffrn_orient_matrix_UB_32      0.0229267000
_diffrn_orient_matrix_UB_33      -0.0417160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0889
_diffrn_reflns_av_unetI/netI     0.0961
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       61
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            61178
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         78.110
_diffrn_reflns_theta_min         2.611
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    8.746
_exptl_absorpt_correction_T_max  0.845
_exptl_absorpt_correction_T_min  0.504
_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    1.346
_exptl_crystal_description       plate
_exptl_crystal_F_000             7100
_exptl_crystal_size_max          0.099
_exptl_crystal_size_mid          0.055
_exptl_crystal_size_min          0.018
_refine_diff_density_max         3.368
_refine_diff_density_min         -2.105
_refine_diff_density_rms         0.165
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     882
_refine_ls_number_reflns         19314
_refine_ls_number_restraints     453
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.1496
_refine_ls_R_factor_gt           0.1002
_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^)+(0.1530P)^2^+6.8165P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2715
_refine_ls_wR_factor_ref         0.3052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10445
_reflns_number_total             19314
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag3{(PPh)4Se2(NMe)2}(MeCN)4][OTf]xC6H4F2_file021_file029.cif'
_cod_data_source_block           Ag3Se
_cod_original_formula_sum        'C61 H63 Ag3 F N7.50 P8 Se4'
_cod_database_code               4349404
_chemical_oxdiff_formula         Ag3C71F9N4O9P8S3Se4
_reflns_odcompleteness_completeness 99.88
_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. Uiso/Uaniso restraints and constraints
F1 \\sim F2 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Se2B \\sim Se2D \\sim Se3B \\sim N3B \\sim N3D \\sim N4D \\sim C27B \\sim C27D:
within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C1A \\sim C1C \\sim C2A \\sim C2C \\sim C3A \\sim C3C \\sim C4A \\sim C4C \\sim
C5A \\sim C5C \\sim C6A \\sim C6C \\sim C15A \\sim C15C \\sim C16A \\sim C16C
\\sim C17A \\sim C17C \\sim C18A \\sim C18C \\sim C19A \\sim C19C \\sim C20A
\\sim C20C: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
3. Same fragment restrains
{N4B, C28B, C29B} sigma for 1-2: 0.02, 1-3: 0.02
as
{N5A, C29A, C30A}
4. Others
 Sof(Se2D)=1-FVAR(1)
 Sof(N3D)=Sof(N4D)=Sof(C27D)=Sof(H27G)=Sof(H27H)=Sof(H27I)=Sof(C28D)=Sof(H28D)=
 Sof(H28E)=Sof(H28F)=0.5*(1-FVAR(2))
 Sof(Se2B)=Sof(Se3B)=0.5*FVAR(2)
 Sof(N3B)=Sof(C27B)=Sof(H27D)=Sof(H27E)=Sof(H27F)=FVAR(1)
 Sof(C15C)=Sof(C16C)=Sof(H16C)=Sof(C17C)=Sof(H17C)=Sof(C18C)=Sof(H18C)=
 Sof(C19C)=Sof(H19C)=Sof(C20C)=Sof(H20C)=1-FVAR(2)
 Sof(C15A)=Sof(C16A)=Sof(H16A)=Sof(C17A)=Sof(H17A)=Sof(C18A)=Sof(H18A)=
 Sof(C19A)=Sof(H19A)=Sof(C20A)=Sof(H20A)=FVAR(2)
 Sof(C1C)=Sof(C6C)=Sof(H6C)=Sof(C5C)=Sof(H5C)=Sof(C4C)=Sof(H4C)=Sof(C3C)=
 Sof(H3C)=Sof(C2C)=Sof(H2C)=1-FVAR(3)
 Sof(C1A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C4A)=Sof(H4A)=Sof(C3A)=
 Sof(H3A)=Sof(C2A)=Sof(H2A)=FVAR(3)
 Fixed Sof: H13A(0.5) H13B(0.5) H13C(0.5) H14A(0.5) H14B(0.5) H14C(0.5)
 H27A(0.5) H27B(0.5) H27C(0.5) H28A(0.5) H28B(0.5) H28C(0.5) N5B(0.5) H13D(0.5)
 H13E(0.5) H13F(0.5) H14D(0.5) H14E(0.5) H14F(0.5)
5.a Me refined with riding coordinates:
 C13A(H13A,H13B,H13C), C14A(H14A,H14B,H14C), C27A(H27A,H27B,H27C), C28A(H28A,
 H28B,H28C), C13B(H13D,H13E,H13F), C14B(H14D,H14E,H14F), C27D(H27G,H27H,H27I),
 C28D(H28D,H28E,H28F)
5.b Aromatic/amide H refined with riding coordinates:
 C6A(H6A), C5A(H5A), C4A(H4A), C3A(H3A), C2A(H2A), C6C(H6C), C5C(H5C),
 C4C(H4C), C3C(H3C), C2C(H2C), C8A(H8A), C9A(H9A), C10A(H10A), C11A(H11A),
 C12A(H12A), C16A(H16A), C17A(H17A), C18A(H18A), C19A(H19A), C20A(H20A),
 C16C(H16C), C17C(H17C), C18C(H18C), C19C(H19C), C20C(H20C), C22A(H22A),
 C23A(H23A), C24A(H24A), C25A(H25A), C26A(H26A), C2B(H2B), C3B(H3B), C4B(H4B),
 C5B(H5B), C6B(H6B), C8B(H8B), C9B(H9B), C10B(H10B), C11B(H11B), C12B(H12B),
 C16B(H16B), C17B(H17B), C18B(H18B), C19B(H19B), C20B(H20B), C22B(H22B),
 C23B(H23B), C24B(H24B), C25B(H25B), C26B(H26B), C35(H35), C36(H36), C37(H37),
 C38(H38)
5.c Fitted hexagon refined as free rotating group:
 C1A(C6A,C5A,C4A,C3A,C2A), C1C(C6C,C5C,C4C,C3C,C2C), C15A(C16A,C17A,C18A,C19A,
 C20A), C15C(C16C,C17C,C18C,C19C,C20C)
5.d Idealised Me refined as rotating group:
 C30A(H30A,H30B,H30C), C32A(H32A,H32B,H32C), C29B(H29A,H29B,H29C), C27B(H27D,
 H27E,H27F)
;
_shelx_res_checksum              4590
_shelx_hkl_checksum              56137
_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 1.939
_oxdiff_exptl_absorpt_empirical_full_min 0.544