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_4349409
_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 Se2'
_chemical_formula_sum            'C26 H26 N2 P4 Se2'
_chemical_formula_weight         648.29
_chemical_name_systematic
3,7-dimethyl-2,4,6,8-tetraphenyl-1,5,3,7,2,4,6,8-diselenadiazatetraphosphocane
_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                 112.1812(11)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.15421(9)
_cell_length_b                   10.99823(7)
_cell_length_c                   11.85068(11)
_cell_measurement_reflns_used    17616
_cell_measurement_temperature    99.99(14)
_cell_measurement_theta_max      76.4040
_cell_measurement_theta_min      3.9940
_cell_volume                     1346.21(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      99.99(14)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.5700
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_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    -18.00  32.00   0.50    0.50    --  -38.50  57.00 -60.00  100
  2  \w     22.00  70.00   0.50    0.50    --   42.75  38.00 -30.00   96
  3  \w     11.00 113.00   0.50    0.50    --   42.75  77.00-120.00  204
  4  \w     80.00 108.00   0.50    2.00    --  111.00  77.00 -90.00   56
  5  \w    115.00 171.00   0.50    2.00    --  111.00  61.00 -60.00  112
  6  \w    126.00 168.00   0.50    2.00    --  111.00  61.00 -90.00   84
  7  \w    122.00 155.00   0.50    2.00    --  111.00  77.00-180.00   66
  8  \w     83.00 109.00   0.50    2.00    --  111.00  61.00 -60.00   52
  9  \w     88.00 127.00   0.50    2.00    --  111.00  45.00 -30.00   78
 10  \w     83.00 165.00   0.50    2.00    --  111.00  61.00 -30.00  164
 11  \w    119.00 177.00   0.50    2.00    --  111.00 125.00 120.00  116
 12  \w     83.00 170.00   0.50    2.00    --  111.00  61.00 120.00  174
 13  \w     84.00 164.00   0.50    2.00    --  111.00  61.00  30.00  160
 14  \w     83.00 173.00   0.50    2.00    --  111.00  61.00  60.00  180
 15  \w     83.00 127.00   0.50    2.00    --  111.00  61.00 150.00   88
 16  \w     84.00 169.00   0.50    2.00    --  111.00  61.00  90.00  170
 17  \w     83.00 127.00   0.50    2.00    --  111.00  61.00   0.00   88
 18  \w     81.00 107.00   0.50    2.00    --  111.00  77.00  90.00   52
 19  \w     80.00 106.00   0.50    2.00    --  111.00  77.00 120.00   52
 20  \w     80.00 106.00   0.50    2.00    --  111.00  77.00  60.00   52
 21  \w     80.00 106.00   0.50    2.00    --  111.00  77.00  30.00   52
 22  \w     80.00 174.00   0.50    2.00    --  111.00  77.00   0.00  188
 23  \w     83.00 109.00   0.50    2.00    --  111.00  61.00-180.00   52
 24  \w     84.00 144.00   0.50    2.00    --  111.00  61.00-150.00  120
 25  \w     84.00 111.00   0.50    2.00    --  111.00  61.00-120.00   54
 26  \w     84.00 109.00   0.50    2.00    --  111.00  61.00 -90.00   50
 27  \w     81.00 173.00   0.50    2.00    --  111.00  77.00-120.00  184
 28  \w     80.00 159.00   0.50    2.00    --  111.00  77.00-150.00  158
 29  \w     80.00 106.00   0.50    2.00    --  111.00  77.00 -30.00   52
 30  \w     80.00 108.00   0.50    2.00    --  111.00  77.00-180.00   56
 31  \w     41.00 134.00   0.50    2.00    --  111.00 -45.00-150.00  186
 32  \w     71.00 121.00   0.50    2.00    --  111.00-125.00-180.00  100
 33  \w     66.00 109.00   0.50    2.00    --  111.00 -94.00-180.00   86
 34  \w     49.00 107.00   0.50    2.00    --  111.00 -94.00-120.00  116
 35  \w     76.00 119.00   0.50    2.00    --  111.00-125.00   0.00   86
 36  \w     40.00 124.00   0.50    2.00    --  111.00 -45.00  90.00  168
 37  \w     42.00 119.00   0.50    2.00    --  111.00-125.00  90.00  154
 38  \w     28.00  69.00   0.50    0.50    --   42.75 -99.00  60.00   82
 39  \w     38.00  92.00   0.50    2.00    --  111.00 -94.00  90.00  108
 40  \w     11.00 110.00   0.50    0.50    --   42.75  77.00   0.00  198
 41  \w     80.00 174.00   0.50    2.00    --  111.00  77.00 150.00  188
 42  \w     13.00  98.00   0.50    0.50    --   42.75  77.00  60.00  170
 43  \w     12.00  87.00   0.50    0.50    --   42.75  77.00 -60.00  150
 44  \w     11.00 103.00   0.50    0.50    --   42.75  77.00 150.00  184
 45  \w    -58.00 -12.00   0.50    0.50    --  -38.50 -57.00-150.00   92
 46  \w    -60.00  20.00   0.50    0.50    --  -38.50  38.00-180.00  160
 47  \w    -91.00  -2.00   0.50    0.50    --  -38.50 125.00-180.00  178
 48  \w   -104.00 -73.00   0.50    0.50    --  -38.50 -57.00-150.00   62
 49  \w   -111.00 -52.00   0.50    0.50    --  -38.50-160.00 -92.00  118
;
_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      0.1267969000
_diffrn_orient_matrix_UB_12      0.0313398000
_diffrn_orient_matrix_UB_13      -0.0169337000
_diffrn_orient_matrix_UB_21      0.0181896000
_diffrn_orient_matrix_UB_22      -0.1350862000
_diffrn_orient_matrix_UB_23      -0.0240131000
_diffrn_orient_matrix_UB_31      -0.0763931000
_diffrn_orient_matrix_UB_32      0.0197751000
_diffrn_orient_matrix_UB_33      -0.1372768000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0202
_diffrn_reflns_av_unetI/netI     0.0139
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       14
_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            23543
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.613
_diffrn_reflns_theta_min         4.019
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.827
_exptl_absorpt_correction_T_max  0.520
_exptl_absorpt_correction_T_min  0.347
_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    1.599
_exptl_crystal_description       block
_exptl_crystal_F_000             648
_exptl_crystal_size_max          0.293
_exptl_crystal_size_mid          0.227
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.061
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.20(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5229
_refine_ls_number_restraints     722
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0274
_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^)+(0.0313P)^2^+1.2126P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0716
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.995
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5222
_reflns_number_total             5229
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            Se-8-Ring_file032_file042.cif
_cod_data_source_block           Se-8-ring
_cod_database_code               4349409
_chemical_oxdiff_formula         'C52 H52 N4 P8 Se4 '
_chemical_oxdiff_usercomment     'full sphere'
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.80(3) 0.20(3)
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
C19A \\sim C20A \\sim C21A \\sim C22A \\sim C23A \\sim C24A \\sim C19B \\sim
C20B \\sim C21B \\sim C22B \\sim C23B \\sim C24B \\sim C1A \\sim C2A \\sim C3A
\\sim C4A \\sim C5A \\sim C6A \\sim C1B \\sim C6B \\sim C5B \\sim C4B \\sim C3B
\\sim C2B \\sim C7A \\sim C8A \\sim C9A \\sim C10A \\sim C11A \\sim C12A \\sim
C7B \\sim C8B \\sim C9B \\sim C10B \\sim C11B \\sim C12B \\sim C13A \\sim C14A
\\sim C15A \\sim C16A \\sim C17A \\sim C18A \\sim C13B \\sim C14B \\sim C15B
\\sim C16B \\sim C17B \\sim C18B: within 2A with sigma of 0.01 and sigma for
terminal atoms of 0.02
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(Se1B)=Sof(Se2B)=Sof(P1B)=Sof(P2B)=Sof(P3B)=Sof(P4B)=1-FVAR(1)
 Sof(Se1A)=Sof(Se2A)=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              61311
_shelx_hkl_checksum              27396
_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 1.129
_oxdiff_exptl_absorpt_empirical_full_min 0.817