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_7220384
_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 Se, 2(C H4 O)'
_chemical_formula_sum            'C61 H57 Ag N O2 P3 Se'
_chemical_formula_weight         1115.81
_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     iterative
_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                87.407(7)
_cell_angle_beta                 86.817(7)
_cell_angle_gamma                69.329(7)
_cell_formula_units_Z            2
_cell_length_a                   12.2175(10)
_cell_length_b                   13.7065(10)
_cell_length_c                   17.1985(15)
_cell_measurement_reflns_used    4258
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      69.7400
_cell_measurement_theta_min      3.8630
_cell_volume                     2689.5(4)
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.3200
_diffrn_measured_fraction_theta_full 0.9916
_diffrn_measured_fraction_theta_max 0.9743
_diffrn_measurement_details
;
  1 omega  -70.00  -41.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  130.0000 -168.0000 29

  2 omega  -42.00  -16.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 26

  3 omega  -71.00  -43.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 28

  4 omega -103.00  -75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 28

  5 omega    4.00   46.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -57.0000 -120.0000 42

  6 omega -131.00 -106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  150.0000 25

  7 omega -154.00  -99.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000 -120.0000 55

  8 omega -149.00 -107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000   60.0000 42

  9 omega -151.00 -125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000 -150.0000 26

 10 omega -105.00  -14.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  130.0000 -168.0000 91

 11 omega -157.00 -125.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000   30.0000 32

 12 omega -156.00 -107.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000 -180.0000 49

 13 omega  109.00  156.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  126.0000 -120.0000 47

 14 omega  109.00  135.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289  126.0000 -180.0000 26

 15 omega  -42.00  140.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       54.7289   15.0000 -180.0000 182

 16 omega    8.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  -60.0000 25

 17 omega   49.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -180.0000 57

 18 omega  121.00  147.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  112.0000  -60.0000 26

 19 omega   31.00   57.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   90.0000 26

 20 omega   17.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000  -30.0000 52

 21 omega   18.00  115.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000 -120.0000 97

 22 omega    7.00  114.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000    0.0000 107

 23 omega   31.00   69.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000    0.0000 38

 24 omega   13.00   47.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000 -180.0000 34

 25 omega   35.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -64.0000 -150.0000 73

 26 omega   68.00   93.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  -60.0000 25

 27 omega   82.00  108.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000   90.0000 26

 28 omega   78.00  151.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   50.0000  150.0000 73

 29 omega   10.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -25.0000 -150.0000 62

 30 omega   64.00  121.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   77.0000 -180.0000 57

 31 omega   64.00  154.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577   64.0000   90.0000 90

 32 omega   10.00  139.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -77.0000    0.0000 129

 33 omega   56.00   81.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -50.0000 -120.0000 25
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0601254000
_diffrn_orient_matrix_UB_12      -0.0135517000
_diffrn_orient_matrix_UB_13      -0.0819258000
_diffrn_orient_matrix_UB_21      0.1204850000
_diffrn_orient_matrix_UB_22      -0.0425792000
_diffrn_orient_matrix_UB_23      0.0365988000
_diffrn_orient_matrix_UB_31      -0.0025090000
_diffrn_orient_matrix_UB_32      -0.1114686000
_diffrn_orient_matrix_UB_33      -0.0013190000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0693
_diffrn_reflns_av_unetI/netI     0.0996
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.974
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17132
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.974
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.245
_diffrn_reflns_theta_min         3.871
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.956
_exptl_absorpt_correction_T_max  0.624
_exptl_absorpt_correction_T_min  0.284
_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    1.378
_exptl_crystal_F_000             1144
_exptl_crystal_size_max          0.4129
_exptl_crystal_size_mid          0.3036
_exptl_crystal_size_min          0.1212
_refine_diff_density_max         1.319
_refine_diff_density_min         -2.664
_refine_diff_density_rms         0.113
_refine_ls_extinction_coef       0.00050(14)
_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   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     627
_refine_ls_number_reflns         9975
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1307
_refine_ls_R_factor_gt           0.0802
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1321P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2005
_refine_ls_wR_factor_ref         0.2390
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6002
_reflns_number_total             9975
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00626k2.cif
_cod_data_source_block           goutam8_2
_cod_depositor_comments
'Adding full bibliography for 7220380--7220385.cif.'
_cod_database_code               7220384
_chemical_oxdiff_formula         'Ag Se N P3 C61 H57 O2'
_reflns_odcompleteness_completeness 99.16
_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.a Aromatic/amide H refined with riding coordinates:
 C44(H44), C47(H47), C59(H59), C8(H8), C32(H32), C48(H48), C3(H3), C30(H30),
 C29(H29), C34(H34), C41(H41), C15(H15), C50(H50), C56(H56), C10(H10), C9(H9),
 C52(H52), C12(H12), C27(H27), C42(H42), C6(H6), C39(H39), C16(H16), C18(H18),
 C5(H5), C11(H11), C4(H4), C53(H53), C24(H24), C33(H33), C54(H54), C35(H35),
 C2(H2), C20(H20), C38(H38), C26(H26), C58(H58), C45(H45), C28(H28), C57(H57),
 C21(H21), C14(H14), C23(H23), C46(H46), C17(H17), C40(H40), C51(H51), C36(H36),
  C22(H22)
2.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C60(H60A,H60B,H60C)
2.c Idealised tetrahedral OH refined as rotating group:
 O2(H2A), O1(H1)
;
_shelxl_version_number           2013-4