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_4349403
_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         'C60 H64 Ag3 N8 P8 Se4, 3(C1 F3 O3 S1)'
_chemical_formula_sum            'C63 H64 Ag3 F9 N8 O9 P8 S3 Se4'
_chemical_formula_weight         2231.74
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_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            8
_cell_length_a                   34.4220(5)
_cell_length_b                   34.4220(5)
_cell_length_c                   15.4107(5)
_cell_measurement_reflns_used    26950
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.2960
_cell_measurement_theta_min      1.8720
_cell_volume                     18259.7(7)
_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_temperature      173.0(10)
_diffrn_detector                 'CCD plate'
_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  \f    -64.43  44.47   0.30   29.99  67.75 -17.26  30.17    --   363
  2  \w    -32.15   5.05   0.30   30.00    --  -18.36 -45.20 -99.33  124
  3  \w    256.95 325.05   0.30   60.00    --  -18.36 -45.20 -99.33  227
  4  \w    -53.16  45.84   0.30   60.00    --  -18.36  82.76  37.64  330
  5  \f     -9.83 139.86   0.30   60.01  67.75 -17.26  30.17    --   500
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0146727000
_diffrn_orient_matrix_UB_12      0.0089710000
_diffrn_orient_matrix_UB_13      -0.0254245000
_diffrn_orient_matrix_UB_21      0.0123854000
_diffrn_orient_matrix_UB_22      -0.0161183000
_diffrn_orient_matrix_UB_23      0.0073228000
_diffrn_orient_matrix_UB_31      -0.0074780000
_diffrn_orient_matrix_UB_32      -0.0091667000
_diffrn_orient_matrix_UB_33      -0.0376777000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0445
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -44
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            74609
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         27.482
_diffrn_reflns_theta_min         1.673
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.521
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69022
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_description       block
_exptl_crystal_F_000             9624
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.630
_refine_diff_density_min         -1.230
_refine_diff_density_rms         0.153
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.40(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     678
_refine_ls_number_reflns         20672
_refine_ls_number_restraints     521
_refine_ls_restrained_S_all      1.277
_refine_ls_R_factor_all          0.1072
_refine_ls_R_factor_gt           0.0753
_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^)+(0.1527P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2193
_refine_ls_wR_factor_ref         0.2397
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                12433
_reflns_number_total             20672
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file
'[Ag3{(PPh)4Se2(NMe)2}(MeCN)4][OTf]_SQUEEZE_file001_file001.cif'
_cod_data_source_block           Ag3Se
_cod_original_cell_volume        18259.7(8)
_cod_database_code               4349403
_chemical_oxdiff_formula         C63H64Ag3N8P8Se4F9O9S3
_reflns_odcompleteness_completeness 99.83
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.60(2) 0.40(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3. Restrained distances
 N1A-C1 \\sim N2B-C51B \\sim N2A-C2 \\sim N1B-C52B
 with sigma of 0.01
 Se2B-P4 \\sim Se1A-P4 \\sim Se1A-P1 \\sim Se1B-P1 \\sim Se1B-P2 \\sim Se2A-P2
\\sim Se2A-P3 \\sim Se2B-P3
 \\sim Se4-P6 \\sim Se4-P7 \\sim Se3-P5 \\sim Se3-P8
 with sigma of 0.01
 P6-N3 \\sim P5-N3 \\sim P8-N4 \\sim P7-N4 \\sim P1-N1A \\sim P2-N1A \\sim
P4-N1B \\sim P1-N1B \\sim P3-N2A ~
 P4-N2A \\sim P2-N2B \\sim P3-N2B
 with sigma of 0.01
 N2B-C51B \\sim N2A-C2 \\sim N1B-C52B \\sim N1A-C1 \\sim N4-C28 \\sim N3-C27
 with sigma of 0.01
4. Restrained planarity
 Ag2, N5, N6, N7, C53, C54, C55, C56, C57, C58
 with sigma of 0.01
5. Uiso/Uaniso restraints and constraints
N6 \\sim C55 \\sim C56: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.02
C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60 \\sim
C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim
C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41 \\sim C46 \\sim C45 \\sim C44 \\sim
C43 \\sim C42 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51 \\sim C52 \\sim
C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9 \\sim C14 \\sim C13
\\sim C12 \\sim C11 \\sim C10 \\sim C15 \\sim C16 \\sim C17 \\sim C18 \\sim C19
\\sim C20 \\sim C21 \\sim C26 \\sim C25 \\sim C24 \\sim C23 \\sim C22 \\sim C27
\\sim C28 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
6. Same fragment restrains
{N6, C55, C56} sigma for 1-2: 0.001, 1-3: 0.001
{N7, C57, C58} sigma for 1-2: 0.001, 1-3: 0.001
{N8, C59, C60} sigma for 1-2: 0.001, 1-3: 0.001
as
{N5, C53, C54}
7. Others
 Sof(Se1B)=Sof(Se2B)=Sof(N2B)=Sof(N1B)=Sof(C51B)=Sof(H51A)=Sof(H51B)=Sof(H51C)=
 Sof(C52B)=Sof(H52A)=Sof(H52B)=Sof(H52C)=1-FVAR(1)
 Sof(Se2A)=Sof(Se1A)=Sof(N1A)=Sof(N2A)=Sof(C1)=Sof(H1A)=Sof(H1B)=Sof(H1C)=
 Sof(C2)=Sof(H2A)=Sof(H2B)=Sof(H2C)=FVAR(1)
8.a Aromatic/amide H refined with riding coordinates:
 C30(H30), C31(H31), C32(H32), C33(H33), C34(H34), C36(H36), C37(H37),
 C38(H38), C39(H39), C40(H40), C46(H46), C45(H45), C44(H44), C43(H43), C42(H42),
  C48(H48), C49(H49), C50(H50), C51(H51), C52(H52), C4(H4), C5(H5), C6(H6),
 C7(H7), C8(H8), C14(H14), C13(H13), C12(H12), C11(H11), C10(H10), C16(H16),
 C17(H17), C18(H18), C19(H19), C20(H20), C26(H26), C25(H25), C24(H24), C23(H23),
  C22(H22)
8.b Fitted hexagon refined as free rotating group:
 C29(C30,C31,C32,C33,C34), C35(C36,C37,C38,C39,C40), C41(C46,C45,C44,C43,C42),
 C47(C48,C49,C50,C51,C52), C3(C4,C5,C6,C7,C8), C9(C14,C13,C12,C11,C10), C15(C16,
 C17,C18,C19,C20), C21(C26,C25,C24,C23,C22)
8.c Idealised Me refined as rotating group:
 C54(H54A,H54B,H54C), C56(H56A,H56B,H56C), C58(H58A,H58B,H58C), C60(H60A,H60B,
 H60C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C1(H1A,H1B,H1C), C51B(H51A,
 H51B,H51C), C2(H2A,H2B,H2C), C52B(H52A,H52B,H52C)
;
_shelx_res_checksum              73360
_shelx_hkl_checksum              75895
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.276
_oxdiff_exptl_absorpt_empirical_full_min 0.911