#------------------------------------------------------------------------------
#$Date: 2019-11-24 00:36:07 +0200 (Sun, 24 Nov 2019) $
#$Revision: 235791 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/97/4349749.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4349749
loop_
_publ_author_name
'Das, Debarati'
'Biradha, Kumar'
_publ_section_title
;
 Metal--organic gels of silver salts with an α,β-unsaturated ketone: the
 influence of anions and solvents on gelation
;
_journal_issue                   8
_journal_name_full               'Inorganic Chemistry Frontiers'
_journal_page_first              1365
_journal_paper_doi               10.1039/C7QI00328E
_journal_volume                  4
_journal_year                    2017
_chemical_formula_sum            'C18 H19 Ag F6 N3 O2 Sb'
_chemical_formula_weight         652.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           8
_space_group_name_Hall           'C -2y'
_space_group_name_H-M_alt        'C 1 m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/8
_audit_update_record
;
2017-04-29 deposited with the CCDC.
2017-06-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.868(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.790(9)
_cell_length_b                   17.444(7)
_cell_length_c                   7.132(3)
_cell_measurement_reflns_used    4061
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.499
_cell_measurement_theta_min      3.086
_cell_volume                     2447.5(18)
_computing_structure_refinement  'SHELXL-2014/8 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_device_type  'Bruker APEX-2 CCD'
_diffrn_measurement_method       hemispehere
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0998
_diffrn_reflns_av_unetI/netI     0.1105
_diffrn_reflns_Laue_measured_fraction_full 0.966
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            13783
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         3.086
_exptl_absorpt_coefficient_mu    1.966
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       cubic
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.421
_refine_diff_density_min         -0.808
_refine_diff_density_rms         0.154
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.17(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         4061
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1442
_refine_ls_R_factor_gt           0.0788
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1000P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1699
_refine_ls_wR_factor_ref         0.1954
_reflns_Friedel_coverage         0.997
_reflns_Friedel_fraction_full    0.967
_reflns_Friedel_fraction_max     0.968
_reflns_number_gt                2401
_reflns_number_total             4061
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7qi00328e2.cif
_cod_data_source_block           CP2
_cod_original_cell_volume        2447.6(18)
_cod_original_sg_symbol_H-M      'C m'
_cod_database_code               4349749
_shelx_shelxl_version_number     2014/8
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Ag1 Ag 0.08284(13) 0.5000 1.3919(4) 0.0663(8) Uani 1 2 d S T P
Ag2 Ag 0.06691(15) 0.0000 0.8188(4) 0.0723(9) Uani 1 2 d S T P
O1A O -0.0609(9) 0.5000 0.784(5) 0.076(9) Uani 1 2 d S T P
N1A N 0.1278(14) 0.5000 1.097(3) 0.051(6) Uani 1 2 d S T P
C1A C 0.0028(15) 0.5000 0.833(8) 0.099(16) Uani 1 2 d S T P
C2A C 0.0410(12) 0.4292(11) 0.885(3) 0.044(5) Uani 1 1 d . . .
C3A C 0.1085(12) 0.4297(10) 0.972(3) 0.051(6) Uani 1 1 d . . .
H3A1 H 0.1311 0.4294 0.8728 0.061 Uiso 1 1 calc R U .
H3A2 H 0.1224 0.3844 1.0543 0.061 Uiso 1 1 calc R U .
C1AN C 0.2098(19) 0.5000 1.194(6) 0.075(10) Uani 1 2 d S T P
N11A N 0.0487(11) 0.1236(9) 0.858(3) 0.058(5) Uani 1 1 d . . .
C11A C 0.0998(10) 0.1719(10) 0.879(3) 0.050(5) Uani 1 1 d . . .
H11A H 0.1434 0.1525 0.9039 0.060 Uiso 1 1 calc R U .
C12A C 0.0892(12) 0.2549(10) 0.866(3) 0.053(5) Uani 1 1 d . . .
H12A H 0.1248 0.2885 0.8758 0.064 Uiso 1 1 calc R U .
C13A C 0.0237(9) 0.2814(9) 0.839(3) 0.033(4) Uani 1 1 d . . .
C14A C -0.0238(18) 0.2288(14) 0.815(5) 0.082(9) Uani 1 1 d . . .
H14A H -0.0676 0.2459 0.8002 0.099 Uiso 1 1 calc R U .
C15A C -0.0147(13) 0.1526(11) 0.811(4) 0.066(7) Uani 1 1 d . . .
H15A H -0.0521 0.1200 0.7762 0.079 Uiso 1 1 calc R U .
C16A C 0.0072(10) 0.3630(9) 0.824(4) 0.060(7) Uani 1 1 d . . .
H16A H -0.0385 0.3716 0.7545 0.072 Uiso 1 1 calc R U .
O1B O 0.2023(18) 0.0000 0.367(6) 0.111(14) Uani 1 2 d S T P
N1B N 0.0169(12) 0.0000 0.467(5) 0.073(9) Uani 1 2 d S T P
C1B C 0.143(4) 0.0000 0.371(5) 0.10(2) Uani 1 2 d S T P
C2B C 0.1070(12) 0.0753(11) 0.372(3) 0.046(5) Uani 1 1 d . . .
C3B C 0.0267(10) 0.0692(11) 0.347(4) 0.055(6) Uani 1 1 d . . .
H3B1 H 0.0117 0.1155 0.3957 0.066 Uiso 1 1 calc R U .
H3B2 H 0.0002 0.0628 0.2088 0.066 Uiso 1 1 calc R U .
C1BN C -0.065(2) 0.0000 0.443(11) 0.12(2) Uani 1 2 d S T P
N11B N 0.1009(10) 0.3759(10) 0.450(3) 0.053(5) Uani 1 1 d . . .
C11B C 0.1617(10) 0.3443(11) 0.520(3) 0.053(6) Uani 1 1 d . . .
H11B H 0.1973 0.3779 0.5790 0.064 Uiso 1 1 calc R U .
C12B C 0.1797(11) 0.2683(11) 0.516(4) 0.047(5) Uani 1 1 d . . .
H12B H 0.2241 0.2515 0.5763 0.056 Uiso 1 1 calc R U .
C13B C 0.1265(11) 0.2173(10) 0.417(3) 0.046(5) Uani 1 1 d . . .
C14B C 0.0594(11) 0.2506(13) 0.340(4) 0.074(8) Uani 1 1 d . . .
H14B H 0.0221 0.2201 0.2764 0.089 Uiso 1 1 calc R U .
C15B C 0.0519(11) 0.3239(11) 0.361(3) 0.046(5) Uani 1 1 d . . .
H15B H 0.0078 0.3427 0.3098 0.055 Uiso 1 1 calc R U .
C16B C 0.1419(11) 0.1395(13) 0.400(3) 0.052(6) Uani 1 1 d . . .
H16B H 0.1872 0.1318 0.4103 0.062 Uiso 1 1 calc R U .
O1M O -0.063(4) 0.5000 1.307(6) 0.24(4) Uani 1 2 d S T P
O2M O 0.191(2) 0.0000 0.882(5) 0.141(15) Uani 1 2 d S T P
Sb1 Sb 0.32365(10) 0.26432(10) 0.1674(2) 0.0845(9) Uani 1 1 d . . .
F101 F 0.3242(11) 0.285(2) 0.372(3) 0.192(15) Uani 1 1 d . . .
F102 F 0.3905(17) 0.202(5) 0.291(16) 0.56(9) Uani 1 1 d . . .
F103 F 0.318(3) 0.209(2) -0.026(6) 0.26(2) Uani 1 1 d . . .
F104 F 0.375(3) 0.336(2) 0.090(11) 0.35(4) Uani 1 1 d . . .
F105 F 0.268(2) 0.1937(15) 0.183(10) 0.31(3) Uani 1 1 d . . .
F106 F 0.2558(15) 0.3222(18) 0.040(10) 0.34(4) Uani 1 1 d . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N11B Ag1 N11B 156.1(10) 2_566 1_556
N11B Ag1 O1M 98.2(5) 2_566 .
N11B Ag1 O1M 98.2(5) 1_556 .
N11B Ag1 N1A 93.9(5) 2_566 .
N11B Ag1 N1A 93.9(5) 1_556 .
O1M Ag1 N1A 117.7(12) . .
N11A Ag2 N11A 152.0(10) . 2
N11A Ag2 N1B 95.6(5) . .
N11A Ag2 N1B 95.6(5) 2 .
C3A N1A C3A 111(2) 2_565 .
C3A N1A C1AN 107.3(17) 2_565 .
C3A N1A C1AN 107.3(17) . .
C3A N1A Ag1 112.9(13) 2_565 .
C3A N1A Ag1 112.9(13) . .
C1AN N1A Ag1 105.2(18) . .
O1A C1A C2A 120.9(14) . 2_565
O1A C1A C2A 120.9(14) . .
C2A C1A C2A 117(3) 2_565 .
C3A C2A C16A 121.0(18) . .
C3A C2A C1A 121.2(18) . .
C16A C2A C1A 117(2) . .
C2A C3A N1A 108.9(19) . .
C11A N11A C15A 118.2(18) . .
C11A N11A Ag2 118.0(16) . .
C15A N11A Ag2 121.8(14) . .
N11A C11A C12A 122(2) . .
C13A C12A C11A 117.3(19) . .
C12A C13A C14A 116(2) . .
C12A C13A C16A 122.1(17) . .
C14A C13A C16A 121(2) . .
C15A C14A C13A 126(3) . .
C14A C15A N11A 120(2) . .
C2A C16A C13A 137(2) . .
C3B N1B C3B 104(3) 2 .
C3B N1B C1BN 105(2) 2 .
C3B N1B C1BN 105(2) . .
C3B N1B Ag2 119.7(14) 2 .
C3B N1B Ag2 119.7(14) . .
C1BN N1B Ag2 101(3) . .
O1B C1B C2B 120(3) . 2
O1B C1B C2B 120(3) . .
C2B C1B C2B 120(5) 2 .
C16B C2B C1B 119(3) . .
C16B C2B C3B 124.8(17) . .
C1B C2B C3B 116(3) . .
N1B C3B C2B 108.0(16) . .
C11B N11B C15B 112.3(18) . .
C11B N11B Ag1 124.2(14) . 1_554
C15B N11B Ag1 120.7(14) . 1_554
N11B C11B C12B 128.8(18) . .
C11B C12B C13B 116(2) . .
C12B C13B C16B 119(2) . .
C12B C13B C14B 116.0(18) . .
C16B C13B C14B 125(2) . .
C15B C14B C13B 119(2) . .
C14B C15B N11B 128(2) . .
C2B C16B C13B 135(2) . .
F101 Sb1 F104 108(3) . .
F101 Sb1 F102 84(4) . .
F104 Sb1 F102 97(3) . .
F101 Sb1 F103 158(3) . .
F104 Sb1 F103 92(3) . .
F102 Sb1 F103 83(4) . .
F101 Sb1 F106 97(3) . .
F104 Sb1 F106 84(2) . .
F102 Sb1 F106 177(4) . .
F103 Sb1 F106 95(2) . .
F101 Sb1 F105 84(3) . .
F104 Sb1 F105 167(3) . .
F102 Sb1 F105 88(2) . .
F103 Sb1 F105 77(3) . .
F106 Sb1 F105 90(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N11B 2.213(18) 2_566
Ag1 N11B 2.213(18) 1_556
Ag1 O1M 2.89(8) .
Ag1 N1A 2.56(2) .
Ag2 N11A 2.221(17) .
Ag2 N11A 2.221(17) 2
Ag2 N1B 2.39(3) .
O1A C1A 1.25(3) .
N1A C3A 1.49(2) 2_565
N1A C3A 1.49(2) .
N1A C1AN 1.62(4) .
C1A C2A 1.45(3) 2_565
C1A C2A 1.45(3) .
C2A C3A 1.34(3) .
C2A C16A 1.35(3) .
N11A C11A 1.33(3) .
N11A C15A 1.35(3) .
C11A C12A 1.46(3) .
C12A C13A 1.39(3) .
C13A C14A 1.32(4) .
C13A C16A 1.46(2) .
C14A C15A 1.34(3) .
O1B C1B 1.24(7) .
N1B C3B 1.53(3) 2
N1B C3B 1.53(3) .
N1B C1BN 1.66(5) .
C1B C2B 1.52(4) 2
C1B C2B 1.52(4) .
C2B C16B 1.31(3) .
C2B C3B 1.62(3) .
N11B C11B 1.32(3) .
N11B C15B 1.36(3) .
N11B Ag1 2.213(18) 1_554
C11B C12B 1.38(3) .
C12B C13B 1.42(3) .
C13B C16B 1.41(3) .
C13B C14B 1.45(3) .
C14B C15B 1.30(3) .
Sb1 F101 1.50(2) .
Sb1 F104 1.85(4) .
Sb1 F102 1.76(4) .
Sb1 F103 1.66(4) .
Sb1 F106 1.73(3) .
Sb1 F105 1.72(3) .
