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_7220381
_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         '2(C41 H34 Ag N P2 S)'
_chemical_formula_sum            'C82 H68 Ag2 N2 P4 S2'
_chemical_formula_weight         1485.12
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           80
_space_group_name_Hall           'I 4bw'
_space_group_name_H-M_alt        'I 41'
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-03-17
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   20.4449(5)
_cell_length_b                   20.4449(5)
_cell_length_c                   34.6253(9)
_cell_measurement_reflns_used    3370
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      68.6410
_cell_measurement_theta_min      3.9500
_cell_volume                     14473.2(6)
_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 0.9845
_diffrn_measured_fraction_theta_max 0.5592
_diffrn_measurement_details
;
  1 omega   36.00   62.00   1.0000    1.0500
omega____ theta____ kappa____ phi______ frames
    -        0.0000  178.0000  -90.0000 26

  2 omega  -97.00  -60.00   1.0000    1.0500
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000    0.0000 37

  3 omega  -65.00   27.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      -54.7289   77.0000 -150.0000 92

  4 omega -157.00 -122.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      -54.7289 -126.0000  150.0000 35

  5 omega -107.00  -82.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      -54.7289  -95.0000  -60.0000 25

  6 omega   23.00   70.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000 -150.0000 47

  7 omega   12.00   65.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000  120.0000 53

  8 omega   75.00  113.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577 -112.0000  -90.0000 38

  9 omega   30.00   71.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000   60.0000 41

 10 omega   95.00  130.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577  178.0000   30.0000 35

 11 omega   16.00   67.00   1.0000    4.1900
omega____ theta____ kappa____ phi______ frames
    -      109.4577  -38.0000  -90.0000 51
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Titan'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0647385000
_diffrn_orient_matrix_UB_12      0.0348743000
_diffrn_orient_matrix_UB_13      -0.0099646000
_diffrn_orient_matrix_UB_21      0.0374070000
_diffrn_orient_matrix_UB_22      -0.0646360000
_diffrn_orient_matrix_UB_23      0.0057341000
_diffrn_orient_matrix_UB_31      -0.0099214000
_diffrn_orient_matrix_UB_32      -0.0167083000
_diffrn_orient_matrix_UB_33      -0.0429519000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0641
_diffrn_reflns_av_unetI/netI     0.0673
_diffrn_reflns_laue_measured_fraction_full 0.983
_diffrn_reflns_laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            11942
_diffrn_reflns_point_group_measured_fraction_full 0.570
_diffrn_reflns_point_group_measured_fraction_max 0.559
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         70.10
_diffrn_reflns_theta_min         3.06
_diffrn_source                   'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    6.059
_exptl_absorpt_correction_T_max  0.521
_exptl_absorpt_correction_T_min  0.172
_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    1.363
_exptl_crystal_F_000             6080
_exptl_crystal_size_max          0.5747
_exptl_crystal_size_mid          0.1946
_exptl_crystal_size_min          0.1398
_refine_diff_density_max         1.022
_refine_diff_density_min         -1.584
_refine_diff_density_rms         0.125
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.19(2)
_refine_ls_extinction_coef       0.000032(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   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     852
_refine_ls_number_reflns         7691
_refine_ls_number_restraints     241
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.053
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1731P)^2^+5.4814P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2519
_refine_ls_wR_factor_ref         0.2832
_reflns_Friedel_coverage         0.135
_reflns_friedel_fraction_full    0.141
_reflns_friedel_fraction_max     0.135
_reflns_number_gt                4710
_reflns_number_total             7691
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5ce00626k2.cif
_cod_data_source_block           goutam5_1
_cod_depositor_comments
'Adding full bibliography for 7220380--7220385.cif.'
_cod_original_cell_volume        14473.2(8)
_cod_database_code               7220381
_chemical_oxdiff_formula         'Ag2 P4 N2 S2 C82 H67'
_reflns_odcompleteness_completeness 98.45
_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
N2 \\sim C42 \\sim C41 \\sim C40: within 1.7A with sigma of 0.03 and sigma for terminal atoms of 0.06
C37 \\sim C38 \\sim C39 \\sim N1: within 1.7A with sigma of 0.03 and sigma for terminal atoms of 0.06
N4 \\sim C84 \\sim C83 \\sim C82: within 1.7A with sigma of 0.03 and sigma for terminal atoms of 0.06
C79 \\sim C80 \\sim C81 \\sim N3: within 1.7A with sigma of 0.03 and sigma for terminal atoms of 0.06
C76 \\sim C75 \\sim C74 \\sim C73 \\sim C78 \\sim C77: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C7 \\sim C8 \\sim C9 \\sim C10 \\sim C11 \\sim C12: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C1 \\sim C6 \\sim C5 \\sim C4 \\sim C3 \\sim C2: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C40 \\sim C41 \\sim C42: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C55 \\sim C56 \\sim C57 \\sim C58 \\sim C59 \\sim C60: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C37 \\sim C38 \\sim C39 \\sim N1 \\sim C39 \\sim C38: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C40 \\sim C41 \\sim C42 \\sim N2 \\sim C42 \\sim C41: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C38 \\sim C39 \\sim N1 \\sim C39 \\sim C38 \\sim C37: within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(C82) \\sim Ueq, Uanis(C79) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C37) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C41) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
3. Others
 Fixed Sof: S1(0.5) S4(0.5) S3(0.5) S2(0.5)
4.a Aromatic/amide H refined with riding coordinates:
 C26(H26), C83(H83), C44(H44), C34(H34), C20(H20), C62(H62), C72(H72), C6(H6),
 C66(H66), C68(H68), C76(H76), C35(H35), C77(H77), C80(H80), C70(H70), C22(H22),
  C15(H15), C33(H33), C51(H51), C52(H52), C57(H57), C21(H21), C58(H58),
 C63(H63), C53(H53), C54(H54), C45(H45), C46(H46), C12(H12), C30(H30), C5(H5),
 C2(H2), C56(H56), C39(H39), C38(H38), C64(H64), C3(H3), C84(H84), C59(H59),
 C74(H74), C48(H48), C18(H18), C16(H16), C41(H41), C36(H36), C32(H32), C4(H4),
 C65(H65), C69(H69), C14(H14), C10(H10), C27(H27), C75(H75), C23(H23), C71(H71),
  C78(H78), C50(H50), C28(H28), C8(H8), C17(H17), C11(H11), C60(H60), C47(H47),
 C42(H42), C9(H9), C29(H29), C81(H81), C24(H24)
;
_shelxl_version_number           2013-4