#------------------------------------------------------------------------------
#$Date: 2019-11-17 09:56:17 +0200 (Sun, 17 Nov 2019) $
#$Revision: 229220 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/64/7046452.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_7046452
loop_
_publ_author_name
'Suntrup, Lisa'
'Kleoff, Merlin'
'Sarkar, Biprajit'
_publ_section_title
;
 Serendipitous discoveries of new coordination modes of the
 1,5-regioisomer of 1,2,3-triazoles enroute to the attempted synthesis of
 a carbon-anchored tri-mesoionic carbene.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7992
_journal_page_last               8002
_journal_paper_doi               10.1039/c8dt01521j
_journal_volume                  47
_journal_year                    2018
_chemical_formula_sum            'C30 H22 Ag2 F6 N6 O6 S2'
_chemical_formula_weight         956.39
_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
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-15 deposited with the CCDC.
2018-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                68.090(2)
_cell_angle_beta                 84.194(2)
_cell_angle_gamma                79.220(2)
_cell_formula_units_Z            1
_cell_length_a                   6.3470(4)
_cell_length_b                   10.9429(7)
_cell_length_c                   13.4498(9)
_cell_measurement_reflns_used    3766
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.380
_cell_measurement_theta_min      3.035
_cell_volume                     850.88(10)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            17787
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.380
_diffrn_reflns_theta_min         3.035
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4888
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, 1995'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.866
_exptl_crystal_description       block
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.529
_refine_diff_density_min         -1.449
_refine_diff_density_rms         0.132
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.842
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         4218
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.842
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_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          0.1017
_refine_ls_wR_factor_ref         0.1090
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3766
_reflns_number_total             4218
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c8dt01521j2.cif
_cod_data_source_block           bip56m_a
_cod_depositor_comments
'Adding full bibliography for 7046452--7046455.cif.'
_cod_database_code               7046452
_shelx_shelxl_version_number     2014/7
_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'
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
Ag1 Ag 0.79121(3) 0.61348(2) 0.44437(2) 0.02073(10) Uani 1 1 d . .
C1 C 1.0813(4) 0.5298(3) 0.7408(2) 0.0168(5) Uani 1 1 d . .
H1 H 1.1936 0.4789 0.7881 0.020 Uiso 1 1 calc R U
N1 N 1.0616(3) 0.5279(2) 0.64309(17) 0.0162(4) Uani 1 1 d . .
C2 C 0.9134(4) 0.6171(2) 0.76160(19) 0.0153(5) Uani 1 1 d . .
N2 N 0.8874(3) 0.6108(2) 0.60005(16) 0.0150(4) Uani 1 1 d . .
C3 C 0.8580(4) 0.6566(3) 0.8551(2) 0.0181(5) Uani 1 1 d . .
N3 N 0.7959(3) 0.6658(2) 0.67157(16) 0.0137(4) Uani 1 1 d . .
C4 C 1.0045(4) 0.7138(3) 0.8884(2) 0.0255(6) Uani 1 1 d . .
H4 H 1.1408 0.7231 0.8527 0.031 Uiso 1 1 calc R U
C5 C 0.9487(5) 0.7568(3) 0.9739(3) 0.0324(7) Uani 1 1 d . .
H5 H 1.0469 0.7968 0.9958 0.039 Uiso 1 1 calc R U
C6 C 0.7518(5) 0.7421(3) 1.0275(2) 0.0305(6) Uani 1 1 d . .
H6 H 0.7156 0.7714 1.0861 0.037 Uiso 1 1 calc R U
C7 C 0.6073(5) 0.6844(3) 0.9953(2) 0.0295(6) Uani 1 1 d . .
H7 H 0.4718 0.6745 1.0319 0.035 Uiso 1 1 calc R U
C8 C 0.6600(4) 0.6411(3) 0.9100(2) 0.0241(6) Uani 1 1 d . .
H8 H 0.5612 0.6008 0.8887 0.029 Uiso 1 1 calc R U
C9 C 0.6020(4) 0.7615(2) 0.6458(2) 0.0144(5) Uani 1 1 d . .
C10 C 0.4387(4) 0.7345(2) 0.6000(2) 0.0172(5) Uani 1 1 d . .
H10 H 0.4532 0.6539 0.5868 0.021 Uiso 1 1 calc R U
C11 C 0.2525(4) 0.8288(3) 0.5739(2) 0.0221(5) Uani 1 1 d . .
H11 H 0.1405 0.8143 0.5398 0.027 Uiso 1 1 calc R U
C12 C 0.2303(5) 0.9436(3) 0.5975(2) 0.0245(6) Uani 1 1 d . .
H12 H 0.1004 1.0055 0.5824 0.029 Uiso 1 1 calc R U
C13 C 0.3954(5) 0.9687(3) 0.6429(2) 0.0251(6) Uani 1 1 d . .
H13 H 0.3794 1.0484 0.6576 0.030 Uiso 1 1 calc R U
C14 C 0.5850(4) 0.8775(3) 0.6671(2) 0.0203(5) Uani 1 1 d . .
H14 H 0.7001 0.8945 0.6975 0.024 Uiso 1 1 calc R U
C100 C 0.1881(4) 0.8385(3) 0.2206(2) 0.0244(6) Uani 1 1 d . .
S100 S 0.36059(10) 0.69128(6) 0.30589(5) 0.01849(15) Uani 1 1 d . .
F100 F 0.1544(3) 0.9352(2) 0.26098(19) 0.0441(5) Uani 1 1 d . .
O101 O 0.2408(4) 0.6531(2) 0.40684(18) 0.0362(5) Uani 1 1 d . .
F101 F -0.0023(3) 0.8094(2) 0.2127(2) 0.0466(5) Uani 1 1 d . .
O102 O 0.3866(3) 0.59969(19) 0.25081(17) 0.0258(4) Uani 1 1 d . .
F102 F 0.2742(3) 0.88603(19) 0.12293(16) 0.0410(5) Uani 1 1 d . .
O100 O 0.5539(3) 0.7441(2) 0.30740(18) 0.0286(5) 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'
S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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'
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
N2 Ag1 N1 127.41(7) . 2_766
N2 Ag1 O100 139.02(8) . .
N1 Ag1 O100 93.46(8) 2_766 .
N2 Ag1 Ag1 64.14(5) . 2_766
N1 Ag1 Ag1 63.32(5) 2_766 2_766
O100 Ag1 Ag1 156.07(6) . 2_766
N1 C1 C2 109.2(2) . .
N1 C1 H1 125.4 . .
C2 C1 H1 125.4 . .
N2 N1 C1 109.0(2) . .
N2 N1 Ag1 114.73(15) . 2_766
C1 N1 Ag1 134.52(17) . 2_766
N3 C2 C1 104.2(2) . .
N3 C2 C3 124.2(2) . .
C1 C2 C3 131.6(2) . .
N1 N2 N3 107.37(19) . .
N1 N2 Ag1 117.50(15) . .
N3 N2 Ag1 134.69(16) . .
C8 C3 C4 119.5(2) . .
C8 C3 C2 121.1(2) . .
C4 C3 C2 119.4(2) . .
N2 N3 C2 110.2(2) . .
N2 N3 C9 119.7(2) . .
C2 N3 C9 130.1(2) . .
C5 C4 C3 119.5(3) . .
C5 C4 H4 120.2 . .
C3 C4 H4 120.2 . .
C4 C5 C6 120.8(3) . .
C4 C5 H5 119.6 . .
C6 C5 H5 119.6 . .
C7 C6 C5 119.8(3) . .
C7 C6 H6 120.1 . .
C5 C6 H6 120.1 . .
C8 C7 C6 120.2(3) . .
C8 C7 H7 119.9 . .
C6 C7 H7 119.9 . .
C7 C8 C3 120.1(3) . .
C7 C8 H8 119.9 . .
C3 C8 H8 119.9 . .
C10 C9 C14 122.3(2) . .
C10 C9 N3 118.7(2) . .
C14 C9 N3 119.0(2) . .
C9 C10 C11 118.3(2) . .
C9 C10 H10 120.9 . .
C11 C10 H10 120.9 . .
C12 C11 C10 120.2(2) . .
C12 C11 H11 119.9 . .
C10 C11 H11 119.9 . .
C11 C12 C13 120.6(3) . .
C11 C12 H12 119.7 . .
C13 C12 H12 119.7 . .
C14 C13 C12 120.2(3) . .
C14 C13 H13 119.9 . .
C12 C13 H13 119.9 . .
C13 C14 C9 118.5(3) . .
C13 C14 H14 120.8 . .
C9 C14 H14 120.8 . .
F102 C100 F101 108.1(3) . .
F102 C100 F100 108.1(3) . .
F101 C100 F100 107.5(2) . .
F102 C100 S100 111.31(19) . .
F101 C100 S100 110.7(2) . .
F100 C100 S100 111.0(2) . .
O101 S100 O100 114.41(14) . .
O101 S100 O102 115.71(12) . .
O100 S100 O102 114.47(13) . .
O101 S100 C100 103.37(15) . .
O100 S100 C100 102.28(12) . .
O102 S100 C100 104.28(13) . .
S100 O100 Ag1 116.31(11) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ag1 N2 2.228(2) .
Ag1 N1 2.290(2) 2_766
Ag1 O100 2.344(2) .
Ag1 Ag1 3.3164(4) 2_766
C1 N1 1.341(3) .
C1 C2 1.372(4) .
C1 H1 0.9500 .
N1 N2 1.320(3) .
N1 Ag1 2.290(2) 2_766
C2 N3 1.363(3) .
C2 C3 1.467(4) .
N2 N3 1.346(3) .
C3 C8 1.397(4) .
C3 C4 1.403(4) .
N3 C9 1.437(3) .
C4 C5 1.388(4) .
C4 H4 0.9500 .
C5 C6 1.383(5) .
C5 H5 0.9500 .
C6 C7 1.389(4) .
C6 H6 0.9500 .
C7 C8 1.387(4) .
C7 H7 0.9500 .
C8 H8 0.9500 .
C9 C10 1.386(3) .
C9 C14 1.385(4) .
C10 C11 1.393(4) .
C10 H10 0.9500 .
C11 C12 1.386(4) .
C11 H11 0.9500 .
C12 C13 1.381(4) .
C12 H12 0.9500 .
C13 C14 1.392(4) .
C13 H13 0.9500 .
C14 H14 0.9500 .
C100 F102 1.321(4) .
C100 F101 1.329(3) .
C100 F100 1.335(3) .
C100 S100 1.823(3) .
S100 O101 1.443(2) .
S100 O100 1.4556(19) .
S100 O102 1.431(2) .
