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_7220385
_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         'C59 H49 Ag N P3 S, C H4 O'
_chemical_formula_sum            'C60 H53 Ag N O P3 S'
_chemical_formula_weight         1036.87
_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             2015-01-23
_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                85.935(5)
_cell_angle_beta                 74.285(5)
_cell_angle_gamma                71.483(5)
_cell_formula_units_Z            2
_cell_length_a                   11.4611(6)
_cell_length_b                   12.6240(7)
_cell_length_c                   19.6133(13)
_cell_measurement_reflns_used    6710
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.8650
_cell_measurement_theta_min      3.6900
_cell_volume                     2589.9(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
;
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 0.9869
_diffrn_measured_fraction_theta_max 0.9665
_diffrn_measurement_details
;
  1 omega   46.00  100.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 54

  2 omega  -95.00  -38.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   90.0000 57

  3 omega   35.00   61.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000  120.0000 26

  4 omega  -46.00    4.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000   77.0000 -150.0000 50

  5 omega  -95.00  -42.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289   61.0000  120.0000 53

  6 omega  -31.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289   61.0000  120.0000 77

  7 omega -152.00  -87.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000   30.0000 65

  8 omega -127.00  -80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  -90.0000 47

  9 omega -127.00  -80.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  120.0000 47

 10 omega -152.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -77.0000 -150.0000 144

 11 omega   42.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  -45.0000    0.0000 33

 12 omega    7.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289 -126.0000    0.0000 110

 13 omega   23.00   84.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000   90.0000 61

 14 omega   20.00   64.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000   90.0000 44

 15 omega   81.00  150.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000  -30.0000 69

 16 omega   81.00  127.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  100.0000 -145.0000 46

 17 omega   38.00  143.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000   90.0000 105

 18 omega   78.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   12.0000 -150.0000 26

 19 omega   45.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -64.0000   60.0000 113

 20 omega   83.00  157.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000 -180.0000 74

 21 omega  103.00  129.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000   60.0000 26

 22 omega   14.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   12.0000 -150.0000 58

 23 omega   37.00   82.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000   60.0000 45

 24 omega   82.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000   60.0000 76

 25 omega   90.00  158.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -92.0000   90.0000 68

 26 omega    8.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   60.0000 106

 27 omega    8.00   49.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000  -60.0000 41

 28 omega   16.00  110.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  -60.0000 94
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0684531000
_diffrn_orient_matrix_UB_12      0.0527971000
_diffrn_orient_matrix_UB_13      0.0744270000
_diffrn_orient_matrix_UB_21      -0.1266584000
_diffrn_orient_matrix_UB_22      0.0433198000
_diffrn_orient_matrix_UB_23      -0.0214007000
_diffrn_orient_matrix_UB_31      -0.0297817000
_diffrn_orient_matrix_UB_32      -0.1087966000
_diffrn_orient_matrix_UB_33      0.0259743000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0762
_diffrn_reflns_laue_measured_fraction_full 0.985
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            16270
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.166
_diffrn_reflns_theta_min         3.693
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.689
_exptl_absorpt_correction_T_max  0.531
_exptl_absorpt_correction_T_min  0.399
_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_density_diffrn    1.330
_exptl_crystal_F_000             1072
_exptl_crystal_size_max          0.5456
_exptl_crystal_size_mid          0.4414
_exptl_crystal_size_min          0.3463
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.526
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       0.0052(5)
_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   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     601
_refine_ls_number_reflns         9535
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.1047
_refine_ls_R_factor_gt           0.0844
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1579P)^2^+3.1427P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2321
_refine_ls_wR_factor_ref         0.2586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7432
_reflns_number_total             9535
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00626k2.cif
_cod_data_source_block           goutam10_1
_cod_depositor_comments
'Adding full bibliography for 7220380--7220385.cif.'
_cod_database_code               7220385
_chemical_oxdiff_formula         'Ag P3 N S O C60 H53'
_reflns_odcompleteness_completeness 98.69
_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
2. Uiso/Uaniso restraints and constraints
Uanis(C54) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(C56) \\sim Ueq, Uanis(C55) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C61) = Uanis(O60)
3.a Aromatic/amide H refined with riding coordinates:
 C43(H43), C53(H53), C31(H31), C2(H2), C17(H17), C29(H29), C25(H25), C35(H35),
 C47(H47), C37(H37), C50(H50), C58(H58), C32(H32), C40(H40), C23(H23), C13(H13),
  C26(H26), C52(H52), C41(H41), C15(H15), C44(H44), C49(H49), C8(H8), C57(H57),
 C10(H10), C11(H11), C59(H59), C9(H9), C33(H33), C51(H51), C28(H28), C56(H56),
 C34(H34), C55(H55), C38(H38), C46(H46), C14(H14), C21(H21), C45(H45), C5(H5),
 C22(H22), C7(H7), C20(H20), C3(H3), C19(H19), C4(H4), C16(H16), C27(H27),
 C39(H39)
3.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C)
3.c Idealised tetrahedral OH refined as rotating group:
 O60(H60)
;
_shelxl_version_number           2013-4