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_7220383
_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         'C87 H72 Ag3 N3 P4 Se3, H2 O, C H4 O'
_chemical_formula_sum            'C88 H79 Ag3 N3 O2 P4 Se3'
_chemical_formula_weight         1894.91
_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   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2014-05-09
_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                97.323(3)
_cell_angle_beta                 112.344(4)
_cell_angle_gamma                94.429(3)
_cell_formula_units_Z            2
_cell_length_a                   14.6363(6)
_cell_length_b                   16.8676(5)
_cell_length_c                   19.0727(10)
_cell_measurement_reflns_used    8303
_cell_measurement_temperature    293
_cell_measurement_theta_max      69.2720
_cell_measurement_theta_min      3.9540
_cell_volume                     4278.9(3)
_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
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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
_diffrn_detector_area_resol_mean 8.3200
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9805
_diffrn_measurement_details
;
  1 omega   -9.00   23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -99.0000   30.0000 32

  2 omega  -48.00   12.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   67.0000 -167.0000 60

  3 omega   35.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   67.0000 -167.0000 65

  4 omega -155.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -77.0000 -180.0000 147

  5 omega -157.00  -89.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  -60.0000 68

  6 omega -147.00  -74.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000    0.0000 73

  7 omega -145.00 -105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000 -120.0000 40

  8 omega  -35.00   25.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  -30.0000    0.0000 60

  9 omega  -38.00   59.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  -30.0000 -150.0000 97

 10 omega   43.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289 -126.0000  -30.0000 74

 11 omega   36.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -150.0000 78

 12 omega    7.00   60.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -12.0000  120.0000 53

 13 omega   89.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   30.0000 26

 14 omega   14.00   40.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000    0.0000 26

 15 omega    7.00  105.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  150.0000 98

 16 omega   48.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000 -120.0000 33

 17 omega   66.00  145.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   77.0000    0.0000 79

 18 omega  116.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000 -150.0000 41

 19 omega    6.00   58.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000  -90.0000 52

 20 omega   16.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000 -150.0000 90

 21 omega   84.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000  -90.0000 73

 22 omega   82.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   64.0000   60.0000 58

 23 omega   74.00  141.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   64.0000  -30.0000 67

 24 omega   57.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000   90.0000 26

 25 omega   83.00  144.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000 -180.0000 61

 26 omega   84.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -12.0000  120.0000 26

 27 omega  124.00  155.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -12.0000  120.0000 31

 28 omega   38.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000 -150.0000 34

 29 omega   79.00  146.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000  -90.0000 67

 30 omega   57.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000    0.0000 25

 31 omega   74.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000 -180.0000 65
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0737224000
_diffrn_orient_matrix_UB_12      -0.0090627000
_diffrn_orient_matrix_UB_13      -0.0395894000
_diffrn_orient_matrix_UB_21      0.0531823000
_diffrn_orient_matrix_UB_22      -0.0565978000
_diffrn_orient_matrix_UB_23      0.0551921000
_diffrn_orient_matrix_UB_31      -0.0702498000
_diffrn_orient_matrix_UB_32      -0.0731856000
_diffrn_orient_matrix_UB_33      -0.0569225000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0712
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            28724
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.980
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.157
_diffrn_reflns_theta_min         3.274
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.979
_exptl_absorpt_correction_T_max  0.355
_exptl_absorpt_correction_T_min  0.064
_exptl_absorpt_correction_type   analytical
_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)
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)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       block
_exptl_crystal_F_000             1894
_exptl_crystal_size_max          0.7404
_exptl_crystal_size_mid          0.3575
_exptl_crystal_size_min          0.2067
_refine_diff_density_max         1.202
_refine_diff_density_min         -1.245
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00030(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   0.990
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     934
_refine_ls_number_reflns         15959
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.990
_refine_ls_R_factor_all          0.0995
_refine_ls_R_factor_gt           0.0691
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1236P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1868
_refine_ls_wR_factor_ref         0.2144
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10689
_reflns_number_total             15959
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00626k2.cif
_cod_data_source_block           exp_8
_cod_depositor_comments
'Adding full bibliography for 7220380--7220385.cif.'
_cod_database_code               7220383
_chemical_oxdiff_formula         'Ag3 N3 P4 C88 H72 Se3'
_reflns_odcompleteness_completeness 99.81
_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, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C72(H72), C2(H2), C30(H30), C78(H78), C84(H84), C5(H5), C18(H18), C73(H73),
 C6(H6), C8(H8), C70(H70), C20(H20), C76(H76), C66(H66), C45(H45), C4(H4),
 C47(H47), C82(H82), C74(H74), C28(H28), C87(H87), C64(H64), C49(H49), C81(H81),
  C43(H43), C44(H44), C33(H33), C38(H38), C39(H39), C32(H32), C79(H79),
 C14(H14), C46(H46), C36(H36), C29(H29), C35(H35), C75(H75), C80(H80), C69(H69),
  C3(H3), C59(H59), C51(H51), C10(H10), C50(H50), C16(H16), C55(H55), C85(H85),
 C17(H17), C41(H41), C68(H68), C9(H9), C12(H12), C34(H34), C53(H53), C21(H21),
 C67(H67), C27(H27), C52(H52), C62(H62), C86(H86), C61(H61), C26(H26), C24(H24),
  C63(H63), C15(H15), C11(H11), C22(H22), C23(H23), C58(H58), C57(H57),
 C56(H56), C40(H40)
2.c Idealised Me refined as rotating group:
 C88(H88A,H88B,H88C)
2.d Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelxl_version_number           2013-4