#------------------------------------------------------------------------------
#$Date: 2020-11-06 14:46:00 +0200 (Fri, 06 Nov 2020) $
#$Revision: 258911 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/05/99/7059984.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_7059984
loop_
_publ_author_name
'Dias, H. V. Rasika'
'Palehepitiya Gamage, Chammi S.'
'Jayaratna, Naleen B.'
'Hettiarachchi, Champika V.'
_publ_section_title
;
 Mixed ligand complexes of silver(i) supported by highly fluorinated
 pyrazolates, and chelating and bridging N-heterocycles
;
_journal_issue                   39
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              17079
_journal_page_last               17087
_journal_paper_doi               10.1039/D0NJ04007J
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety         'C44 H16 Ag4 Cl4 F24 N12'
_chemical_formula_sum            'C44 H16 Ag4 Cl4 F24 N12'
_chemical_formula_weight         1741.97
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-07-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-06 deposited with the CCDC.	2020-09-11 downloaded from the CCDC.
;
_cell_angle_alpha                115.4070(10)
_cell_angle_beta                 109.1150(10)
_cell_angle_gamma                96.3290(10)
_cell_formula_units_Z            1
_cell_length_a                   11.2824(10)
_cell_length_b                   11.8130(10)
_cell_length_c                   11.8889(10)
_cell_measurement_reflns_used    7878
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.21
_cell_volume                     1292.70(19)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0169
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12785
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.294
_diffrn_reflns_theta_min         1.997
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.836
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6202
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2008/1 (Bruker,2008) was used for absorption correction. wR2(int) was 0.0533 before and 0.0280 after correction. The Ratio of minimum to maximum transmission is 0.8317. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.238
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             836
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.339
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6326
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0314
_refine_ls_R_factor_gt           0.0290
_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)+(0.0440P)²+1.1192P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0746
_refine_ls_wR_factor_ref         0.0770
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5825
_reflns_number_total             6326
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj04007j2.cif
_cod_data_source_block           dias904m
_cod_depositor_comments
'Adding full bibliography for 7059979--7059984.cif.'
_cod_original_cell_volume        1292.69(19)
_cod_database_code               7059984
_shelx_shelxl_version_number     2018/3
_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.
;
_shelx_estimated_absorpt_t_max   0.838
_shelx_estimated_absorpt_t_min   0.657
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C11(H11), C12(H12), C13(H13), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22)
;
_olex2_submission_special_instructions 'No special instructions were received'
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
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ag1 Ag 0.58574(2) -0.12068(2) 0.46896(2) 0.01917(6) Uani 1 1 d . . . . .
Ag2 Ag 0.83758(2) 0.11672(2) 0.68042(2) 0.02135(6) Uani 1 1 d . . . . .
Cl1 Cl 1.07728(6) -0.31641(6) 0.56301(6) 0.02277(12) Uani 1 1 d . . . . .
Cl2 Cl 0.65985(7) 0.11701(7) 1.06247(6) 0.03108(15) Uani 1 1 d . . . . .
F1 F 0.76207(19) -0.46175(17) 0.50306(18) 0.0385(4) Uani 1 1 d . . . . .
F2 F 0.62063(16) -0.42426(17) 0.3627(2) 0.0411(5) Uani 1 1 d . . . . .
F3 F 0.77677(17) -0.49366(15) 0.31900(17) 0.0332(4) Uani 1 1 d . . . . .
F4 F 1.21996(15) -0.02535(16) 0.67609(18) 0.0345(4) Uani 1 1 d . . . . .
F5 F 1.11781(16) 0.12070(15) 0.69211(16) 0.0279(3) Uani 1 1 d . . . . .
F6 F 1.15208(16) 0.05157(17) 0.83660(15) 0.0326(4) Uani 1 1 d . . . . .
F7 F 0.59037(16) -0.23493(16) 0.05896(18) 0.0333(4) Uani 1 1 d . . . . .
F8 F 0.5481(2) -0.30850(18) 0.18266(18) 0.0409(4) Uani 1 1 d . . . . .
F9 F 0.39951(16) -0.35935(15) -0.01186(17) 0.0331(4) Uani 1 1 d . . . . .
F10 F 0.80288(17) -0.10282(18) 0.8150(2) 0.0401(4) Uani 1 1 d . . . . .
F11 F 0.6644(2) -0.16404(18) 0.88048(18) 0.0408(4) Uani 1 1 d . . . . .
F12 F 0.61793(17) -0.24541(15) 0.66535(16) 0.0312(4) Uani 1 1 d . . . . .
N1 N 0.77879(19) -0.17436(19) 0.5100(2) 0.0176(4) Uani 1 1 d . . . . .
N2 N 0.8800(2) -0.0620(2) 0.5858(2) 0.0191(4) Uani 1 1 d . . . . .
N3 N 0.48131(19) -0.08474(19) 0.3001(2) 0.0182(4) Uani 1 1 d . . . . .
N4 N 0.5642(2) -0.0216(2) 0.6705(2) 0.0191(4) Uani 1 1 d . . . . .
N5 N 0.7690(2) 0.2902(2) 0.7201(2) 0.0194(4) Uani 1 1 d . . . . .
N6 N 0.9072(2) 0.2384(2) 0.9218(2) 0.0189(4) Uani 1 1 d . . . . .
C1 C 0.8306(2) -0.2747(2) 0.4904(2) 0.0174(4) Uani 1 1 d . . . . .
C2 C 0.9672(2) -0.2275(2) 0.5543(2) 0.0173(4) Uani 1 1 d . . . . .
C3 C 0.9941(2) -0.0939(2) 0.6132(2) 0.0176(4) Uani 1 1 d . . . . .
C4 C 0.7469(2) -0.4128(2) 0.4175(2) 0.0200(5) Uani 1 1 d . . . . .
C5 C 1.1211(2) 0.0127(2) 0.7036(2) 0.0218(5) Uani 1 1 d . . . . .
C6 C 0.4573(2) -0.1433(2) 0.1666(2) 0.0178(4) Uani 1 1 d . . . . .
C7 C 0.4990(2) -0.2613(2) 0.0999(2) 0.0208(5) Uani 1 1 d . . . . .
C8 C 0.6153(2) -0.0281(2) 0.7860(2) 0.0192(4) Uani 1 1 d . . . . .
C9 C 0.6049(2) 0.0756(2) 0.8936(2) 0.0197(4) Uani 1 1 d . . . . .
C10 C 0.6743(3) -0.1344(3) 0.7873(3) 0.0235(5) Uani 1 1 d . . . . .
C11 C 0.6964(2) 0.3137(2) 0.6232(3) 0.0219(5) Uani 1 1 d . . . . .
H11 H 0.675422 0.252918 0.530265 0.026 Uiso 1 1 calc R . . . .
C12 C 0.6498(2) 0.4230(3) 0.6513(3) 0.0243(5) Uani 1 1 d . . . . .
H12 H 0.595709 0.434257 0.578879 0.029 Uiso 1 1 calc R . . . .
C13 C 0.6836(2) 0.5144(2) 0.7861(3) 0.0231(5) Uani 1 1 d . . . . .
H13 H 0.654006 0.590140 0.807553 0.028 Uiso 1 1 calc R . . . .
C14 C 0.7620(2) 0.4947(2) 0.8914(3) 0.0194(4) Uani 1 1 d . . . . .
C15 C 0.8007(2) 0.3785(2) 0.8536(2) 0.0177(4) Uani 1 1 d . . . . .
C16 C 0.8759(2) 0.3522(2) 0.9599(2) 0.0171(4) Uani 1 1 d . . . . .
C17 C 0.9136(2) 0.4465(2) 1.0989(2) 0.0185(4) Uani 1 1 d . . . . .
C18 C 0.9853(2) 0.4164(2) 1.1985(2) 0.0213(5) Uani 1 1 d . . . . .
H18 H 1.012180 0.476342 1.293042 0.026 Uiso 1 1 calc R . . . .
C19 C 1.0161(2) 0.3006(3) 1.1589(3) 0.0225(5) Uani 1 1 d . . . . .
H19 H 1.064593 0.279405 1.225352 0.027 Uiso 1 1 calc R . . . .
C20 C 0.9752(2) 0.2137(2) 1.0188(3) 0.0224(5) Uani 1 1 d . . . . .
H20 H 0.997059 0.133569 0.992021 0.027 Uiso 1 1 calc R . . . .
C21 C 0.8045(2) 0.5880(2) 1.0333(3) 0.0224(5) Uani 1 1 d . . . . .
H21 H 0.780680 0.667086 1.058178 0.027 Uiso 1 1 calc R . . . .
C22 C 0.8779(2) 0.5654(2) 1.1324(3) 0.0212(5) Uani 1 1 d . . . . .
H22 H 0.906294 0.629620 1.225900 0.025 Uiso 1 1 calc R . . . .
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'
Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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
_geom_angle_publ_flag
N1 Ag1 Ag2 65.15(5) . . ?
N3 Ag1 Ag2 108.36(5) . . ?
N3 Ag1 N1 126.48(7) . . ?
N3 Ag1 N4 120.04(7) . . ?
N4 Ag1 Ag2 72.46(5) . . ?
N4 Ag1 N1 108.53(7) . . ?
N2 Ag2 Ag1 66.97(6) . . ?
N2 Ag2 N5 164.26(8) . . ?
N2 Ag2 N6 121.69(7) . . ?
N5 Ag2 Ag1 104.85(5) . . ?
N5 Ag2 N6 74.05(7) . . ?
N6 Ag2 Ag1 126.90(5) . . ?
N2 N1 Ag1 108.53(14) . . ?
C1 N1 Ag1 144.03(16) . . ?
C1 N1 N2 107.42(19) . . ?
N1 N2 Ag2 117.69(15) . . ?
C3 N2 Ag2 131.38(16) . . ?
C3 N2 N1 108.41(19) . . ?
N4 N3 Ag1 118.64(14) 2_656 . ?
C6 N3 Ag1 133.26(16) . . ?
C6 N3 N4 107.95(19) . 2_656 ?
N3 N4 Ag1 118.82(14) 2_656 . ?
C8 N4 Ag1 131.45(16) . . ?
C8 N4 N3 107.91(19) . 2_656 ?
C11 N5 Ag2 124.63(17) . . ?
C11 N5 C15 118.3(2) . . ?
C15 N5 Ag2 117.08(16) . . ?
C16 N6 Ag2 111.44(15) . . ?
C20 N6 Ag2 129.91(16) . . ?
C20 N6 C16 118.5(2) . . ?
N1 C1 C2 110.1(2) . . ?
N1 C1 C4 121.8(2) . . ?
C2 C1 C4 128.0(2) . . ?
C1 C2 Cl1 127.72(18) . . ?
C3 C2 Cl1 127.65(18) . . ?
C3 C2 C1 104.6(2) . . ?
N2 C3 C2 109.5(2) . . ?
N2 C3 C5 119.4(2) . . ?
C2 C3 C5 131.0(2) . . ?
F1 C4 C1 111.4(2) . . ?
F2 C4 F1 106.6(2) . . ?
F2 C4 F3 108.0(2) . . ?
F2 C4 C1 112.4(2) . . ?
F3 C4 F1 104.9(2) . . ?
F3 C4 C1 113.1(2) . . ?
F4 C5 F5 107.2(2) . . ?
F4 C5 F6 107.7(2) . . ?
F4 C5 C3 111.9(2) . . ?
F5 C5 F6 105.8(2) . . ?
F5 C5 C3 112.6(2) . . ?
F6 C5 C3 111.3(2) . . ?
N3 C6 C7 122.5(2) . . ?
N3 C6 C9 110.2(2) . 2_656 ?
C9 C6 C7 127.2(2) 2_656 . ?
F7 C7 C6 111.6(2) . . ?
F8 C7 F7 107.3(2) . . ?
F8 C7 F9 106.6(2) . . ?
F8 C7 C6 112.6(2) . . ?
F9 C7 F7 106.1(2) . . ?
F9 C7 C6 112.1(2) . . ?
N4 C8 C9 110.2(2) . . ?
N4 C8 C10 120.8(2) . . ?
C9 C8 C10 128.9(2) . . ?
C6 C9 Cl2 126.92(19) 2_656 . ?
C6 C9 C8 103.7(2) 2_656 . ?
C8 C9 Cl2 129.35(19) . . ?
F10 C10 C8 112.6(2) . . ?
F11 C10 F10 106.5(2) . . ?
F11 C10 F12 107.4(2) . . ?
F11 C10 C8 112.3(2) . . ?
F12 C10 F10 105.3(2) . . ?
F12 C10 C8 112.2(2) . . ?
N5 C11 H11 118.3 . . ?
N5 C11 C12 123.4(2) . . ?
C12 C11 H11 118.3 . . ?
C11 C12 H12 120.6 . . ?
C13 C12 C11 118.8(2) . . ?
C13 C12 H12 120.6 . . ?
C12 C13 H13 120.2 . . ?
C12 C13 C14 119.6(2) . . ?
C14 C13 H13 120.2 . . ?
C13 C14 C15 117.9(2) . . ?
C13 C14 C21 122.3(2) . . ?
C15 C14 C21 119.8(2) . . ?
N5 C15 C14 122.0(2) . . ?
N5 C15 C16 118.9(2) . . ?
C14 C15 C16 119.1(2) . . ?
N6 C16 C15 118.4(2) . . ?
N6 C16 C17 122.7(2) . . ?
C17 C16 C15 119.0(2) . . ?
C16 C17 C22 119.9(2) . . ?
C18 C17 C16 117.1(2) . . ?
C18 C17 C22 123.0(2) . . ?
C17 C18 H18 120.1 . . ?
C19 C18 C17 119.8(2) . . ?
C19 C18 H18 120.1 . . ?
C18 C19 H19 120.5 . . ?
C18 C19 C20 119.0(2) . . ?
C20 C19 H19 120.5 . . ?
N6 C20 C19 122.9(2) . . ?
N6 C20 H20 118.6 . . ?
C19 C20 H20 118.6 . . ?
C14 C21 H21 119.5 . . ?
C22 C21 C14 121.1(2) . . ?
C22 C21 H21 119.5 . . ?
C17 C22 H22 119.5 . . ?
C21 C22 C17 121.0(2) . . ?
C21 C22 H22 119.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ag1 Ag2 3.1263(3) . ?
Ag1 N1 2.2931(19) . ?
Ag1 N3 2.211(2) . ?
Ag1 N4 2.282(2) . ?
Ag2 N2 2.119(2) . ?
Ag2 N5 2.187(2) . ?
Ag2 N6 2.378(2) . ?
Cl1 C2 1.718(2) . ?
Cl2 C9 1.712(2) . ?
F1 C4 1.347(3) . ?
F2 C4 1.321(3) . ?
F3 C4 1.329(3) . ?
F4 C5 1.333(3) . ?
F5 C5 1.344(3) . ?
F6 C5 1.346(3) . ?
F7 C7 1.336(3) . ?
F8 C7 1.329(3) . ?
F9 C7 1.335(3) . ?
F10 C10 1.347(3) . ?
F11 C10 1.329(3) . ?
F12 C10 1.344(3) . ?
N1 N2 1.358(3) . ?
N1 C1 1.344(3) . ?
N2 C3 1.357(3) . ?
N3 N4 1.359(3) 2_656 ?
N3 C6 1.345(3) . ?
N4 C8 1.344(3) . ?
N5 C11 1.334(3) . ?
N5 C15 1.363(3) . ?
N6 C16 1.350(3) . ?
N6 C20 1.327(3) . ?
C1 C2 1.395(3) . ?
C1 C4 1.488(3) . ?
C2 C3 1.371(3) . ?
C3 C5 1.492(3) . ?
C6 C7 1.494(3) . ?
C6 C9 1.389(3) 2_656 ?
C8 C9 1.391(3) . ?
C8 C10 1.488(3) . ?
C11 H11 0.9500 . ?
C11 C12 1.397(4) . ?
C12 H12 0.9500 . ?
C12 C13 1.379(4) . ?
C13 H13 0.9500 . ?
C13 C14 1.405(4) . ?
C14 C15 1.417(3) . ?
C14 C21 1.432(4) . ?
C15 C16 1.452(3) . ?
C16 C17 1.418(3) . ?
C17 C18 1.407(3) . ?
C17 C22 1.430(3) . ?
C18 H18 0.9500 . ?
C18 C19 1.369(4) . ?
C19 H19 0.9500 . ?
C19 C20 1.402(4) . ?
C20 H20 0.9500 . ?
C21 H21 0.9500 . ?
C21 C22 1.351(4) . ?
C22 H22 0.9500 . ?
