Hemilabile silver(i) complexes containing pyridyl chalcogenolate (S, Se) ligands and their utility as molecular precursors for silver chalcogenides
Kole, Goutam Kumar; Vivekananda, K. V.; Kumar, Mukesh; Ganguly, Rakesh; Dey, Sandip; Jain, Vimal K.; CrystEngComm 17 (2015) 4367–; doi:10.1039/C5CE00626K

data_7220382
_publ_section_title
;
 Hemilabile silver(i) complexes containing pyridyl chalcogenolate (S, Se)
 ligands and their utility as molecular precursors for silver
 chalcogenides
;
_journal_issue                   23
_journal_name_full               CrystEngComm
_journal_page_first              4367
_journal_paper_doi               10.1039/C5CE00626K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C46 H38 Ag2 N2 P2 S2'
_chemical_formula_sum            'C46 H38 Ag2 N2 P2 S2'
_chemical_formula_weight         960.58
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-27
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_audit_update_record
;
2015-03-27 deposited with the CCDC.
2015-04-30 downloaded from the CCDC.
;
_cell_angle_alpha                93.498(4)
_cell_angle_beta                 90.926(5)
_cell_angle_gamma                103.226(4)
_cell_formula_units_Z            2
_cell_length_a                   9.9533(6)
_cell_length_b                   14.2851(6)
_cell_length_c                   15.2400(10)
_cell_measurement_reflns_used    5923
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.7720
_cell_measurement_theta_min      4.1580
_cell_volume                     2104.5(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3200
_diffrn_measured_fraction_theta_full 0.9979
_diffrn_measured_fraction_theta_max 0.9732
_diffrn_measurement_details
;
  1 omega  -68.00  -36.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -60.0000 32

  2 omega  -48.00  -15.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 33

  3 omega   54.00   98.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 44

  4 omega  -10.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 41

  5 omega -143.00 -117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000   90.0000 26

  6 omega -157.00  -88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  150.0000 69

  7 omega -152.00  -97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000 -150.0000 55

  8 omega -140.00  -83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  -60.0000 57

  9 omega -130.00  -83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  -30.0000 47

 10 omega -149.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -77.0000   30.0000 141

 11 omega -113.00  -81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000 -180.0000 32

 12 omega -146.00  -82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000   90.0000 64

 13 omega   20.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289 -126.0000 -180.0000 95

 14 omega   40.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000   60.0000 30

 15 omega   79.00  151.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000 -180.0000 72

 16 omega   61.00  137.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   77.0000  -90.0000 76

 17 omega   82.00  111.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -180.0000 29

 18 omega   10.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -180.0000 54

 19 omega   84.00  112.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000  150.0000 28

 20 omega   38.00  151.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000   60.0000 113

 21 omega   11.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   60.0000 103

 22 omega  107.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000 -180.0000 48

 23 omega    7.00  102.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   30.0000 95

 24 omega   31.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000 -180.0000 69

 25 omega   64.00  154.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   64.0000 -120.0000 90

 26 omega   42.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000   90.0000 30

 27 omega   27.00   70.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000   30.0000 43

 28 omega   44.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000   60.0000 113
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.1166835000
_diffrn_orient_matrix_UB_12      0.0229012000
_diffrn_orient_matrix_UB_13      -0.0564329000
_diffrn_orient_matrix_UB_21      -0.0470054000
_diffrn_orient_matrix_UB_22      -0.1072263000
_diffrn_orient_matrix_UB_23      -0.0317733000
_diffrn_orient_matrix_UB_31      -0.0971994000
_diffrn_orient_matrix_UB_32      -0.0174407000
_diffrn_orient_matrix_UB_33      0.0778627000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0767
_diffrn_reflns_av_unetI/netI     0.0840
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            13083
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.186
_diffrn_reflns_theta_min         2.906
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    9.371
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.516
_exptl_crystal_F_000             968
_exptl_crystal_size_max          0.5467
_exptl_crystal_size_mid          0.3178
_exptl_crystal_size_min          0.2225
_refine_diff_density_max         1.916
_refine_diff_density_min         -2.126
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       0.0045(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     488
_refine_ls_number_reflns         7805
_refine_ls_number_restraints     132
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0991
_refine_ls_R_factor_gt           0.0796
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1741P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2154
_refine_ls_wR_factor_ref         0.2533
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5829
_reflns_number_total             7805
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00626k2.cif
_cod_data_source_block           goutam5_2
_cod_depositor_comments
'Adding full bibliography for 7220380--7220385.cif.'
_cod_database_code               7220382
_chemical_oxdiff_formula         'C60 N4 S4 Ag2 P4 H58'
_reflns_odcompleteness_completeness 99.79
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
C46 \\sim C45 \\sim C44 \\sim C43 \\sim C42 \\sim C41: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C35 \\sim C40 \\sim C39 \\sim C38 \\sim C37 \\sim C36: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C13 \\sim C18 \\sim C17 \\sim C16 \\sim C15 \\sim C14: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C45) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq, Uanis(C42) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3.a Aromatic/amide H refined with riding coordinates:
 C17(H17), C14(H14), C26(H26), C2(H2), C22(H22), C16(H16), C34(H34), C9(H9),
 C21(H21), C28(H28), C27(H27), C23(H23), C37(H37), C25(H25), C30(H30), C12(H12),
  C6(H6), C42(H42), C38(H38), C46(H46), C36(H36), C18(H18), C8(H8), C3(H3),
 C20(H20), C4(H4), C33(H33), C15(H15), C31(H31), C5(H5), C11(H11), C44(H44),
 C40(H40), C32(H32), C10(H10), C39(H39), C45(H45), C43(H43)
;
_shelxl_version_number           2013-4