#------------------------------------------------------------------------------
#$Date: 2020-07-22 04:34:27 +0300 (Wed, 22 Jul 2020) $
#$Revision: 254452 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/24/09/7240908.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_7240908
loop_
_publ_author_name
'Vassilyeva, Olga Yu.'
'Buvaylo, Elena A.'
'Linnik, Rostyslav P.'
'Nesterov, Dmytro S.'
'Trachevsky, Vladimir V.'
'Skelton, Brian W.'
_publ_section_title
;
 Synthetic strategy towards halometallates with
 imidazo[1,5-a]pyridinium-based counterions
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/D0CE00018C
_journal_year                    2020
_chemical_formula_moiety         '2(C8 H9 N2), Cl4 Zn'
_chemical_formula_sum            'C16 H18 Cl4 N4 Zn'
_chemical_formula_weight         473.51
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc23rlm3
_audit_creation_date             2015-01-13T10:03:30-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-12-16 deposited with the CCDC.	2020-07-21 downloaded from the CCDC.
;
_cell_angle_alpha                99.224(3)
_cell_angle_beta                 111.029(3)
_cell_angle_gamma                91.986(3)
_cell_formula_units_Z            2
_cell_length_a                   9.3908(3)
_cell_length_b                   10.6494(4)
_cell_length_c                   10.7328(3)
_cell_measurement_reflns_used    13737
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.101
_cell_measurement_theta_min      2.088
_cell_volume                     983.95(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.31 
;
_computing_molecular_graphics    'Diamond (Brandenburg, K., (1999)'
_computing_publication_material  'WinGX Farrugia, L. J. (1999)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.4738
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Oxford Diffraction Gemini diffractometer'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0769263
_diffrn_orient_matrix_UB_12      0.0150976
_diffrn_orient_matrix_UB_13      -0.0177416
_diffrn_orient_matrix_UB_21      -0.0236653
_diffrn_orient_matrix_UB_22      -0.0637737
_diffrn_orient_matrix_UB_23      0.0007104
_diffrn_orient_matrix_UB_31      0.0116937
_diffrn_orient_matrix_UB_32      0.0174422
_diffrn_orient_matrix_UB_33      0.0698264
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0285
_diffrn_reflns_av_unetI/netI     0.0376
_diffrn_reflns_Laue_measured_fraction_full 0.99
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33095
_diffrn_reflns_point_group_measured_fraction_full 0.99
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        37
_diffrn_reflns_theta_max         37.59
_diffrn_reflns_theta_min         1.947
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.798
_exptl_absorpt_correction_T_max  0.811
_exptl_absorpt_correction_T_min  0.57
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
   CrysAlisPro, Agilent Technologies

;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.598
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.14
_refine_diff_density_max         2.297
_refine_diff_density_min         -0.857
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     228
_refine_ls_number_reflns         10024
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.049
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.035
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0496P)²+0.6512P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0984
_refine_ls_wR_factor_ref         0.1062
_reflns_number_gt                8331
_reflns_number_total             10024
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0ce00018c2.cif
_cod_data_source_block           lv721
_cod_database_code               7240908
loop_
_symmetry_equiv_pos_as_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_calc_flag
_atom_site_disorder_assembly
_atom_site_disorder_group
C11 C 0.76237(16) 0.54765(13) 0.26683(15) 0.0187(2) Uani 1 d . .
H11 H 0.8364 0.5078 0.3305 0.022 Uiso 1 calc . .
N12 N 0.78854(13) 0.61749(11) 0.18290(12) 0.01682(19) Uani 1 d . .
C12 C 0.93783(17) 0.64341(16) 0.17342(18) 0.0231(3) Uani 1 d . .
H12A H 0.9977 0.5706 0.1931 0.035 Uiso 1 calc . .
H12B H 0.9927 0.7204 0.2393 0.035 Uiso 1 calc . .
H12C H 0.9231 0.6566 0.0815 0.035 Uiso 1 calc . .
C13 C 0.65592(16) 0.65998(13) 0.10480(15) 0.0179(2) Uani 1 d . .
H13 H 0.645 0.7112 0.0377 0.021 Uiso 1 calc . .
N13A N 0.54194(15) 0.61440(12) 0.14206(14) 0.0210(2) Uani 1 d . .
C14 C 0.38157(16) 0.62398(15) 0.09859(16) 0.0215(3) Uani 1 d . .
H14 H 0.3318 0.6683 0.0272 0.026 Uiso 1 calc . .
C15 C 0.30150(19) 0.56832(17) 0.1615(2) 0.0278(3) Uani 1 d . .
H15 H 0.1943 0.5746 0.1343 0.033 Uiso 1 calc . .
C16 C 0.3751(2) 0.50038(17) 0.2682(2) 0.0310(4) Uani 1 d . .
H16 H 0.3165 0.4637 0.3117 0.037 Uiso 1 calc . .
C17 C 0.5268(2) 0.48753(16) 0.30802(19) 0.0265(3) Uani 1 d . .
H17 H 0.5749 0.441 0.3778 0.032 Uiso 1 calc . .
C17A C 0.61109(15) 0.54426(12) 0.24418(13) 0.01406(19) Uani 1 d . .
C21 C 0.29077(17) 0.89766(14) 0.31680(16) 0.0214(3) Uani 1 d . .
H21 H 0.1938 0.897 0.326 0.026 Uiso 1 calc . .
N22 N 0.32633(17) 0.93710(13) 0.21516(13) 0.0226(2) Uani 1 d . .
C22 C 0.2200(3) 0.98895(19) 0.10208(18) 0.0345(4) Uani 1 d . .
H22A H 0.2765 1.0211 0.0507 0.052 Uiso 1 calc . .
H22B H 0.1723 1.059 0.138 0.052 Uiso 1 calc . .
H22C H 0.1404 0.9213 0.0422 0.052 Uiso 1 calc . .
C23 C 0.4731(2) 0.92418(14) 0.23386(15) 0.0220(3) Uani 1 d . .
H23 H 0.5243 0.9445 0.1766 0.026 Uiso 1 calc . .
N23A N 0.53514(15) 0.87718(11) 0.34851(13) 0.0178(2) Uani 1 d . .
C24 C 0.68540(18) 0.84795(15) 0.41248(18) 0.0240(3) Uani 1 d . .
H24 H 0.7613 0.8603 0.375 0.029 Uiso 1 calc . .
C25 C 0.7195(2) 0.80185(16) 0.52862(19) 0.0290(3) Uani 1 d . .
H25 H 0.8203 0.78 0.5723 0.035 Uiso 1 calc . .
C26 C 0.6073(2) 0.78527(16) 0.58727(17) 0.0286(3) Uani 1 d . .
H26 H 0.6354 0.7549 0.6705 0.034 Uiso 1 calc . .
C27 C 0.4620(2) 0.81210(15) 0.52624(16) 0.0236(3) Uani 1 d . .
H27 H 0.3875 0.7997 0.5652 0.028 Uiso 1 calc . .
C27A C 0.42217(16) 0.85923(13) 0.40275(14) 0.0168(2) Uani 1 d . .
Zn1 Zn 0.84597(2) 0.19368(2) 0.25133(2) 0.01713(4) Uani 1 d . .
Cl1 Cl 0.58795(4) 0.19015(4) 0.13678(4) 0.02242(7) Uani 1 d . .
Cl2 Cl 0.98326(4) 0.30043(4) 0.15506(4) 0.02244(7) Uani 1 d . .
Cl3 Cl 0.90087(5) -0.01249(4) 0.24417(4) 0.02630(8) Uani 1 d . .
Cl4 Cl 0.89826(5) 0.30497(4) 0.46509(4) 0.02654(8) Uani 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 0 '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'
Zn Zn 0.2839 1.4301 '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'
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 1 0 0.1154
-1 -15 2 0.1551
1 0 0 0.0459
-1 0 0 0.0943
-1 0 1 0.1355
1 0 2 0.1296
1 1 -1 0.1603
0 -1 -2 0.2503
-1 -2 0 0.1355
-2 -1 0 0.102
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
N12 C11 C17A 107.21(12) . . ?
N12 C11 H11 126.4 . . ?
C17A C11 H11 126.4 . . ?
C11 N12 C13 110.85(12) . . ?
C11 N12 C12 124.88(13) . . ?
C13 N12 C12 124.26(13) . . ?
N12 C12 H12A 109.5 . . ?
N12 C12 H12B 109.5 . . ?
H12A C12 H12B 109.5 . . ?
N12 C12 H12C 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
N12 C13 N13A 106.65(12) . . ?
N12 C13 H13 126.7 . . ?
N13A C13 H13 126.7 . . ?
C13 N13A C17A 106.65(12) . . ?
C13 N13A C14 133.89(14) . . ?
C17A N13A C14 119.46(13) . . ?
C15 C14 N13A 118.30(15) . . ?
C15 C14 H14 120.8 . . ?
N13A C14 H14 120.8 . . ?
C14 C15 C16 121.29(15) . . ?
C14 C15 H15 119.4 . . ?
C16 C15 H15 119.4 . . ?
C17 C16 C15 121.04(16) . . ?
C17 C16 H16 119.5 . . ?
C15 C16 H16 119.5 . . ?
C16 C17 C17A 118.41(16) . . ?
C16 C17 H17 120.8 . . ?
C17A C17 H17 120.8 . . ?
C11 C17A C17 129.90(14) . . ?
C11 C17A N13A 108.64(12) . . ?
C17 C17A N13A 121.43(13) . . ?
N22 C21 C27A 106.73(13) . . ?
N22 C21 H21 126.6 . . ?
C27A C21 H21 126.6 . . ?
C23 N22 C21 110.58(13) . . ?
C23 N22 C22 124.08(16) . . ?
C21 N22 C22 125.33(16) . . ?
N22 C22 H22A 109.5 . . ?
N22 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
N22 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
N22 C23 N23A 107.45(13) . . ?
N22 C23 H23 126.3 . . ?
N23A C23 H23 126.3 . . ?
C23 N23A C24 129.71(14) . . ?
C23 N23A C27A 108.90(13) . . ?
C24 N23A C27A 121.39(13) . . ?
C25 C24 N23A 118.25(15) . . ?
C25 C24 H24 120.9 . . ?
N23A C24 H24 120.9 . . ?
C24 C25 C26 121.36(16) . . ?
C24 C25 H25 119.3 . . ?
C26 C25 H25 119.3 . . ?
C27 C26 C25 120.97(16) . . ?
C27 C26 H26 119.5 . . ?
C25 C26 H26 119.5 . . ?
C26 C27 C27A 118.90(15) . . ?
C26 C27 H27 120.5 . . ?
C27A C27 H27 120.5 . . ?
C21 C27A N23A 106.34(13) . . ?
C21 C27A C27 134.55(14) . . ?
N23A C27A C27 119.09(13) . . ?
Cl3 Zn1 Cl4 113.959(17) . . ?
Cl3 Zn1 Cl1 107.146(17) . . ?
Cl4 Zn1 Cl1 106.697(16) . . ?
Cl3 Zn1 Cl2 110.222(16) . . ?
Cl4 Zn1 Cl2 107.423(16) . . ?
Cl1 Zn1 Cl2 111.392(15) . . ?
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
C11 N12 1.3364(19) . ?
C11 C17A 1.3507(19) . ?
C11 H11 0.95 . ?
N12 C13 1.3674(18) . ?
N12 C12 1.4618(19) . ?
C12 H12A 0.98 . ?
C12 H12B 0.98 . ?
C12 H12C 0.98 . ?
C13 N13A 1.369(2) . ?
C13 H13 0.95 . ?
N13A C17A 1.4021(19) . ?
N13A C14 1.4205(19) . ?
C14 C15 1.355(2) . ?
C14 H14 0.95 . ?
C15 C16 1.430(3) . ?
C15 H15 0.95 . ?
C16 C17 1.351(3) . ?
C16 H16 0.95 . ?
C17 C17A 1.396(2) . ?
C17 H17 0.95 . ?
C21 N22 1.370(2) . ?
C21 C27A 1.371(2) . ?
C21 H21 0.95 . ?
N22 C23 1.335(2) . ?
N22 C22 1.469(2) . ?
C22 H22A 0.98 . ?
C22 H22B 0.98 . ?
C22 H22C 0.98 . ?
C23 N23A 1.344(2) . ?
C23 H23 0.95 . ?
N23A C24 1.401(2) . ?
N23A C27A 1.4021(18) . ?
C24 C25 1.348(3) . ?
C24 H24 0.95 . ?
C25 C26 1.427(3) . ?
C25 H25 0.95 . ?
C26 C27 1.348(3) . ?
C26 H26 0.95 . ?
C27 C27A 1.421(2) . ?
C27 H27 0.95 . ?
Zn1 Cl3 2.2682(4) . ?
Zn1 Cl4 2.2779(4) . ?
Zn1 Cl1 2.2858(4) . ?
Zn1 Cl2 2.2920(4) . ?
