#------------------------------------------------------------------------------
#$Date: 2025-07-01 13:37:59 +0300 (Tue, 01 Jul 2025) $
#$Revision: 1108 $
#$URL: svn://crystallography.net/testcod/cif/1/00/00/1000004.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_1000004
loop_
_publ_author_name
'Dias, H. V. Rasika'
'Parasar, Devaborniny'
'Yakovenko, Andrey A.'
'Stephens, Peter W.'
'Muñoz-Castro, Álvaro'
'Vanga, Mukundam'
'Mykhailiuk, Pavel'
'Slobodyanyuk, Evgeniy'
_publ_section_title
;
 In situ studies of reversible solid--gas reactions of ethylene responsive
 silver pyrazolates
;
_journal_issue                   6
_journal_name_full               'Chemical Science'
_journal_page_first              2019
_journal_page_last               2025
_journal_paper_doi               10.1039/D3SC04182D
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         'Ag3 C18 F27 N6, C H2 Cl2'
_chemical_formula_sum            'C19 H2 Ag3 Cl2 F27 N6'
_chemical_formula_weight         1221.78
_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             2022-11-20
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-09-20 deposited with the CCDC.	2023-11-29 downloaded from the CCDC.
;
_cell_angle_alpha                95.547(2)
_cell_angle_beta                 98.944(2)
_cell_angle_gamma                116.476(2)
_cell_formula_units_Z            2
_cell_length_a                   9.4750(8)
_cell_length_b                   10.5097(9)
_cell_length_c                   18.0959(16)
_cell_measurement_reflns_used    9397
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.78
_cell_measurement_theta_min      2.98
_cell_volume                     1565.1(2)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 Ver. 2016.5-0 (Bruker-AXS, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type
'Bruker D8 Quest with a Photon 100 CMOS detector'
_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  0.0183
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21034
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_min         2.885
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.219
_exptl_absorpt_correction_T_max  0.3462
_exptl_absorpt_correction_T_min  0.2510
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0765 before and 0.0454 after correction. The Ratio of minimum to maximum transmission is 0.7250. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.593
_exptl_crystal_description       parallelpipeds
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.144
_refine_diff_density_min         -1.132
_refine_diff_density_rms         0.195
_refine_ls_extinction_coef       0.0160(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     515
_refine_ls_number_reflns         9480
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0267
_refine_ls_R_factor_gt           0.0253
_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)+(0.0326P)²+1.0381P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0626
_refine_ls_wR_factor_ref         0.0636
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8994
_reflns_number_total             9480
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3sc04182d2.cif
_cod_data_source_block           rad629_0m_a
_cod_database_code               1000004
_shelx_shelxl_version_number     2017/1
_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   0.860
_shelx_estimated_absorpt_t_min   0.486
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B)
;
_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 0.72079(2) 0.60670(2) 0.80921(2) 0.01702(4) Uani 1 1 d . . . . .
Ag2 Ag 0.61158(2) 0.74713(2) 0.66052(2) 0.01784(4) Uani 1 1 d . . . . .
Ag3 Ag 0.42179(2) 0.36466(2) 0.65736(2) 0.01715(4) Uani 1 1 d . . . . .
F1 F 0.96653(15) 0.78762(13) 0.94607(7) 0.0279(3) Uani 1 1 d . . . . .
F2 F 1.18516(17) 0.86257(17) 0.90416(8) 0.0338(3) Uani 1 1 d . . . . .
F3 F 1.14744(16) 1.01067(13) 0.97887(7) 0.0278(3) Uani 1 1 d . . . . .
F4 F 1.31475(14) 1.19180(13) 0.89207(8) 0.0267(2) Uani 1 1 d . . . . .
F5 F 1.15663(16) 1.27874(13) 0.91660(7) 0.0282(3) Uani 1 1 d . . . . .
F6 F 1.22975(15) 1.28948(13) 0.80961(7) 0.0275(2) Uani 1 1 d . . . . .
F7 F 0.91811(18) 1.24353(14) 0.74502(8) 0.0322(3) Uani 1 1 d . . . . .
F8 F 1.02654(17) 1.16610(15) 0.66761(7) 0.0311(3) Uani 1 1 d . . . . .
F9 F 0.76904(18) 1.05647(16) 0.65603(9) 0.0410(4) Uani 1 1 d . . . . .
F10 F 0.54261(16) 0.86518(14) 0.53294(8) 0.0321(3) Uani 1 1 d . . . . .
F11 F 0.29664(16) 0.82545(14) 0.50547(7) 0.0287(2) Uani 1 1 d . . . . .
F12 F 0.40190(18) 0.77362(15) 0.41767(7) 0.0305(3) Uani 1 1 d . . . . .
F13 F 0.06880(19) 0.58089(17) 0.39048(8) 0.0401(3) Uani 1 1 d . . . . .
F14 F 0.1416(2) 0.4409(2) 0.33159(7) 0.0434(4) Uani 1 1 d . . . . .
F15 F -0.04837(16) 0.35399(17) 0.39178(8) 0.0393(3) Uani 1 1 d . . . . .
F16 F 0.09885(17) 0.17557(14) 0.41355(7) 0.0313(3) Uani 1 1 d . . . . .
F17 F -0.01775(16) 0.18193(15) 0.50543(8) 0.0316(3) Uani 1 1 d . . . . .
F18 F 0.19871(18) 0.16153(14) 0.52611(9) 0.0370(3) Uani 1 1 d . . . . .
F19 F 0.27928(17) 0.05125(14) 0.64538(8) 0.0327(3) Uani 1 1 d . . . . .
F20 F 0.24872(16) -0.07184(14) 0.73562(8) 0.0326(3) Uani 1 1 d . . . . .
F21 F 0.42123(16) -0.05778(13) 0.66814(7) 0.0289(3) Uani 1 1 d . . . . .
F22 F 0.5249(2) -0.08165(13) 0.81222(8) 0.0386(3) Uani 1 1 d . . . . .
F23 F 0.53200(17) 0.02282(15) 0.92248(8) 0.0310(3) Uani 1 1 d . . . . .
F24 F 0.75139(15) 0.07460(14) 0.88465(7) 0.0261(2) Uani 1 1 d . . . . .
F25 F 0.78018(19) 0.31090(14) 0.97923(7) 0.0366(3) Uani 1 1 d . . . . .
F26 F 0.94220(16) 0.4418(2) 0.91377(9) 0.0488(5) Uani 1 1 d . . . . .
F27 F 0.78010(18) 0.50530(13) 0.95585(7) 0.0314(3) Uani 1 1 d . . . . .
N1 N 0.85820(17) 0.82869(15) 0.80627(8) 0.0153(2) Uani 1 1 d . . . . .
N2 N 0.81559(18) 0.88709(16) 0.74860(8) 0.0163(3) Uani 1 1 d . . . . .
N3 N 0.41943(18) 0.59864(17) 0.56899(8) 0.0171(3) Uani 1 1 d . . . . .
N4 N 0.34780(18) 0.45351(16) 0.56803(8) 0.0169(3) Uani 1 1 d . . . . .
N5 N 0.51155(17) 0.28303(15) 0.74512(8) 0.0156(2) Uani 1 1 d . . . . .
N6 N 0.62528(17) 0.38139(15) 0.80548(8) 0.0153(2) Uani 1 1 d . . . . .
C1 C 0.99379(19) 0.93285(17) 0.85327(9) 0.0143(3) Uani 1 1 d . . . . .
C2 C 1.04291(19) 1.06227(17) 0.82636(9) 0.0143(3) Uani 1 1 d . . . . .
C3 C 0.9253(2) 1.02720(18) 0.76018(9) 0.0159(3) Uani 1 1 d . . . . .
C4 C 1.0734(2) 0.89881(18) 0.92098(10) 0.0174(3) Uani 1 1 d . . . . .
C5 C 1.1854(2) 1.20521(18) 0.86165(10) 0.0169(3) Uani 1 1 d . . . . .
C6 C 0.9098(2) 1.1232(2) 0.70683(11) 0.0225(3) Uani 1 1 d . . . . .
C7 C 0.3412(2) 0.6218(2) 0.50752(10) 0.0175(3) Uani 1 1 d . . . . .
C8 C 0.2153(2) 0.4910(2) 0.46557(9) 0.0175(3) Uani 1 1 d . . . . .
C9 C 0.2260(2) 0.38848(19) 0.50598(9) 0.0171(3) Uani 1 1 d . . . . .
C10 C 0.3952(2) 0.7723(2) 0.49124(10) 0.0204(3) Uani 1 1 d . . . . .
C11 C 0.0944(2) 0.4668(2) 0.39493(10) 0.0235(3) Uani 1 1 d . . . . .
C12 C 0.1255(2) 0.2263(2) 0.48801(10) 0.0200(3) Uani 1 1 d . . . . .
C13 C 0.48460(19) 0.15071(17) 0.75685(9) 0.0144(3) Uani 1 1 d . . . . .
C14 C 0.58245(19) 0.16126(17) 0.82552(9) 0.0141(3) Uani 1 1 d . . . . .
C15 C 0.66794(19) 0.30931(17) 0.85375(9) 0.0144(3) Uani 1 1 d . . . . .
C16 C 0.3581(2) 0.01774(19) 0.70111(10) 0.0196(3) Uani 1 1 d . . . . .
C17 C 0.5967(2) 0.04474(19) 0.86176(10) 0.0188(3) Uani 1 1 d . . . . .
C18 C 0.7935(2) 0.39178(19) 0.92585(10) 0.0182(3) Uani 1 1 d . . . . .
Cl1 Cl 0.50001(8) 0.64152(8) 0.91424(3) 0.03900(13) Uani 1 1 d . . . . .
Cl2 Cl 0.33031(7) 0.58559(5) 0.75539(3) 0.02990(10) Uani 1 1 d . . . . .
C19 C 0.3236(3) 0.6179(2) 0.85326(13) 0.0274(4) Uani 1 1 d . . . . .
H19A H 0.310158 0.705586 0.864024 0.033 Uiso 1 1 calc R . . . .
H19B H 0.228843 0.535125 0.863243 0.033 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
N6 Ag1 N1 167.87(6) . . ?
N2 Ag2 N3 174.98(6) . . ?
N5 Ag3 N4 176.13(6) . . ?
N2 N1 Ag1 120.82(11) . . ?
C1 N1 Ag1 131.01(11) . . ?
C1 N1 N2 108.15(13) . . ?
N1 N2 Ag2 117.70(10) . . ?
C3 N2 Ag2 134.15(12) . . ?
C3 N2 N1 108.04(14) . . ?
N4 N3 Ag2 121.37(11) . . ?
C7 N3 Ag2 130.62(13) . . ?
C7 N3 N4 107.91(14) . . ?
N3 N4 Ag3 121.83(11) . . ?
C9 N4 Ag3 130.08(12) . . ?
C9 N4 N3 108.00(14) . . ?
N6 N5 Ag3 117.03(10) . . ?
C13 N5 Ag3 135.02(11) . . ?
C13 N5 N6 107.95(13) . . ?
N5 N6 Ag1 121.96(11) . . ?
C15 N6 Ag1 129.82(11) . . ?
C15 N6 N5 108.00(13) . . ?
N1 C1 C2 110.12(15) . . ?
N1 C1 C4 120.29(15) . . ?
C2 C1 C4 129.52(15) . . ?
C1 C2 C3 103.64(14) . . ?
C1 C2 C5 127.81(15) . . ?
C3 C2 C5 128.54(15) . . ?
N2 C3 C2 110.06(14) . . ?
N2 C3 C6 121.05(15) . . ?
C2 C3 C6 128.88(15) . . ?
F1 C4 F2 107.07(15) . . ?
F1 C4 C1 111.58(14) . . ?
F2 C4 C1 111.29(15) . . ?
F3 C4 F1 107.33(15) . . ?
F3 C4 F2 107.16(15) . . ?
F3 C4 C1 112.13(14) . . ?
F4 C5 F5 107.24(15) . . ?
F4 C5 F6 106.28(14) . . ?
F4 C5 C2 112.11(14) . . ?
F5 C5 F6 106.98(14) . . ?
F5 C5 C2 112.78(14) . . ?
F6 C5 C2 111.07(14) . . ?
F7 C6 C3 111.00(16) . . ?
F8 C6 F7 107.02(15) . . ?
F8 C6 C3 112.56(16) . . ?
F9 C6 F7 107.46(17) . . ?
F9 C6 F8 107.02(17) . . ?
F9 C6 C3 111.49(15) . . ?
N3 C7 C8 110.16(16) . . ?
N3 C7 C10 120.71(16) . . ?
C8 C7 C10 129.11(16) . . ?
C7 C8 C11 128.21(17) . . ?
C9 C8 C7 103.73(15) . . ?
C9 C8 C11 128.04(17) . . ?
N4 C9 C8 110.20(16) . . ?
N4 C9 C12 120.64(16) . . ?
C8 C9 C12 129.16(15) . . ?
F10 C10 F12 107.25(16) . . ?
F10 C10 C7 111.73(15) . . ?
F11 C10 F10 106.96(16) . . ?
F11 C10 F12 107.24(15) . . ?
F11 C10 C7 112.78(15) . . ?
F12 C10 C7 110.59(15) . . ?
F13 C11 F14 106.87(17) . . ?
F13 C11 C8 111.95(16) . . ?
F14 C11 C8 112.21(16) . . ?
F15 C11 F13 106.89(17) . . ?
F15 C11 F14 106.77(17) . . ?
F15 C11 C8 111.79(16) . . ?
F16 C12 C9 110.84(15) . . ?
F17 C12 F16 107.16(15) . . ?
F17 C12 F18 106.77(17) . . ?
F17 C12 C9 112.75(15) . . ?
F18 C12 F16 107.33(16) . . ?
F18 C12 C9 111.70(15) . . ?
N5 C13 C14 110.14(14) . . ?
N5 C13 C16 120.52(15) . . ?
C14 C13 C16 129.29(15) . . ?
C13 C14 C17 129.58(15) . . ?
C15 C14 C13 103.53(14) . . ?
C15 C14 C17 126.89(15) . . ?
N6 C15 C14 110.38(14) . . ?
N6 C15 C18 119.51(15) . . ?
C14 C15 C18 130.11(15) . . ?
F19 C16 F20 107.70(16) . . ?
F19 C16 F21 106.85(15) . . ?
F19 C16 C13 111.58(14) . . ?
F20 C16 C13 111.09(15) . . ?
F21 C16 F20 106.93(15) . . ?
F21 C16 C13 112.41(15) . . ?
F22 C17 C14 111.13(15) . . ?
F23 C17 F22 107.70(16) . . ?
F23 C17 F24 106.77(15) . . ?
F23 C17 C14 113.28(15) . . ?
F24 C17 F22 105.89(16) . . ?
F24 C17 C14 111.66(14) . . ?
F25 C18 C15 111.94(15) . . ?
F26 C18 F25 108.32(17) . . ?
F26 C18 F27 106.97(16) . . ?
F26 C18 C15 111.50(15) . . ?
F27 C18 F25 106.13(15) . . ?
F27 C18 C15 111.68(15) . . ?
Cl1 C19 Cl2 111.67(11) . . ?
Cl1 C19 H19A 109.3 . . ?
Cl1 C19 H19B 109.3 . . ?
Cl2 C19 H19A 109.3 . . ?
Cl2 C19 H19B 109.3 . . ?
H19A C19 H19B 107.9 . . ?
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 N1 2.1162(14) . ?
Ag1 N6 2.1142(14) . ?
Ag2 N2 2.1199(15) . ?
Ag2 N3 2.1267(15) . ?
Ag3 N4 2.1212(15) . ?
Ag3 N5 2.1156(14) . ?
F1 C4 1.337(2) . ?
F2 C4 1.340(2) . ?
F3 C4 1.330(2) . ?
F4 C5 1.336(2) . ?
F5 C5 1.3356(19) . ?
F6 C5 1.342(2) . ?
F7 C6 1.344(2) . ?
F8 C6 1.339(2) . ?
F9 C6 1.333(2) . ?
F10 C10 1.337(2) . ?
F11 C10 1.328(2) . ?
F12 C10 1.344(2) . ?
F13 C11 1.332(2) . ?
F14 C11 1.340(2) . ?
F15 C11 1.331(2) . ?
F16 C12 1.341(2) . ?
F17 C12 1.325(2) . ?
F18 C12 1.335(2) . ?
F19 C16 1.329(2) . ?
F20 C16 1.340(2) . ?
F21 C16 1.337(2) . ?
F22 C17 1.344(2) . ?
F23 C17 1.330(2) . ?
F24 C17 1.340(2) . ?
F25 C18 1.331(2) . ?
F26 C18 1.329(2) . ?
F27 C18 1.329(2) . ?
N1 N2 1.3574(19) . ?
N1 C1 1.341(2) . ?
N2 C3 1.342(2) . ?
N3 N4 1.362(2) . ?
N3 C7 1.343(2) . ?
N4 C9 1.344(2) . ?
N5 N6 1.3584(19) . ?
N5 C13 1.342(2) . ?
N6 C15 1.338(2) . ?
C1 C2 1.392(2) . ?
C1 C4 1.496(2) . ?
C2 C3 1.395(2) . ?
C2 C5 1.492(2) . ?
C3 C6 1.500(2) . ?
C7 C8 1.394(2) . ?
C7 C10 1.505(3) . ?
C8 C9 1.390(2) . ?
C8 C11 1.494(2) . ?
C9 C12 1.505(3) . ?
C13 C14 1.393(2) . ?
C13 C16 1.505(2) . ?
C14 C15 1.390(2) . ?
C14 C17 1.491(2) . ?
C15 C18 1.500(2) . ?
Cl1 C19 1.754(2) . ?
Cl2 C19 1.787(2) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
