#------------------------------------------------------------------------------
#$Date: 2023-01-06 11:57:50 +0200 (Fri, 06 Jan 2023) $
#$Revision: 280215 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/06/19/7061980.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_7061980
loop_
_publ_author_name
'Zhang, Xiamei'
'He, Chengying'
'Yang, Xiaohan'
'Zhang, Qian'
'Li, Yahong'
'Yao, Jinlei'
_publ_section_title
;
 FeII, CoII and NiII complexes based on
 1-chloro-3-(pyridin-2-yl)imidazo[1,5-a]pyridine: synthesis, structures,
 single-molecule magnetic and electrocatalytic properties
;
_journal_issue                   45
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              21780
_journal_page_last               21787
_journal_paper_doi               10.1039/D2NJ03328C
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C24 H16 Cl4 N6 Ni, C H2 Cl2'
_chemical_formula_sum            'C25 H18 Cl6 N6 Ni'
_chemical_formula_weight         673.86
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2022-10-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2022-10-12 deposited with the CCDC.	2022-10-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 121.604(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.4101(12)
_cell_length_b                   11.5808(7)
_cell_length_c                   15.8049(16)
_cell_measurement_reflns_used    9500
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      2.23
_cell_volume                     2714.0(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            33674
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.542
_diffrn_reflns_theta_min         2.231
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.5905
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1662 before and 0.1044 after correction.
The Ratio of minimum to maximum transmission is 0.7920.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.649
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_exptl_transmission_factor_max   0.7456
_exptl_transmission_factor_min   0.5905
_refine_diff_density_max         0.472
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     173
_refine_ls_number_reflns         3129
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0317
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0301P)²+4.7236P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0783
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2729
_reflns_number_total             3129
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d2nj03328c2.cif
_cod_data_source_block           t_CCDC1
_cod_depositor_comments
'Adding full bibliography for 7061979--7061981.cif.'
_cod_database_code               7061980
_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.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: H25A(0.5) H25B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B)
3.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C10(H10), C14(H14), C16(H16), C18(H18), C20(H20), C22(H22), C24(H24)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'
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
Ni1 Ni 0.5000 0.19356(3) 0.2500 0.01864(10) Uani 1 2 d S T P . .
Cl2 Cl 0.39018(3) 0.05202(4) 0.23034(3) 0.02728(12) Uani 1 1 d . . . . .
Cl4 Cl 0.58209(4) 0.40756(5) 0.11835(4) 0.03627(14) Uani 1 1 d . . . . .
N2 N 0.59469(10) 0.32929(13) 0.28636(11) 0.0212(3) Uani 1 1 d . . . . .
N4 N 0.56081(11) 0.20510(13) 0.40457(11) 0.0210(3) Uani 1 1 d . . . . .
N6 N 0.68965(11) 0.45264(14) 0.40094(12) 0.0226(3) Uani 1 1 d . . . . .
C2 C 0.62728(12) 0.28419(15) 0.45202(13) 0.0189(4) Uani 1 1 d . . . . .
C4 C 0.63762(12) 0.35637(15) 0.38290(13) 0.0198(4) Uani 1 1 d . . . . .
C6 C 0.67991(13) 0.28911(16) 0.55529(14) 0.0232(4) Uani 1 1 d . . . . .
H6 H 0.7269 0.3419 0.5870 0.028 Uiso 1 1 calc R . . . .
C8 C 0.67974(13) 0.48607(17) 0.31049(15) 0.0259(4) Uani 1 1 d . . . . .
C10 C 0.66065(14) 0.21354(17) 0.60958(14) 0.0276(4) Uani 1 1 d . . . . .
H10 H 0.6946 0.2156 0.6786 0.033 Uiso 1 1 calc R . . . .
C12 C 0.61992(13) 0.40725(17) 0.24247(14) 0.0240(4) Uani 1 1 d . . . . .
C14 C 0.54414(15) 0.13384(18) 0.45897(15) 0.0309(5) Uani 1 1 d . . . . .
H14 H 0.4981 0.0799 0.4263 0.037 Uiso 1 1 calc R . . . .
C16 C 0.59152(16) 0.13568(19) 0.56153(16) 0.0341(5) Uani 1 1 d . . . . .
H16 H 0.5770 0.0855 0.5970 0.041 Uiso 1 1 calc R . . . .
C18 C 0.74434(16) 0.51643(19) 0.48648(17) 0.0355(5) Uani 1 1 d . . . . .
H18 H 0.7497 0.4961 0.5463 0.043 Uiso 1 1 calc R . . . .
C20 C 0.72873(16) 0.5806(2) 0.30724(18) 0.0382(5) Uani 1 1 d . . . . .
H20 H 0.7240 0.6015 0.2479 0.046 Uiso 1 1 calc R . . . .
C22 C 0.78280(18) 0.6410(2) 0.3913(2) 0.0501(7) Uani 1 1 d . . . . .
H22 H 0.8155 0.7037 0.3901 0.060 Uiso 1 1 calc R . . . .
C24 C 0.78947(18) 0.6082(2) 0.48148(19) 0.0486(7) Uani 1 1 d . . . . .
H24 H 0.8259 0.6512 0.5386 0.058 Uiso 1 1 calc R . . . .
Cl6 Cl 0.52850(6) 0.67967(7) 0.35435(7) 0.0659(2) Uani 1 1 d . . . . .
C25 C 0.5000 0.7640(4) 0.2500 0.0846(17) Uani 1 2 d S T P . .
H25A H 0.4494 0.8133 0.2352 0.102 Uiso 0.5 1 calc R . . . .
H25B H 0.5506 0.8133 0.2648 0.102 Uiso 0.5 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'
Cl Cl 0.1484 0.1585 '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'
Ni Ni 0.3393 1.1124 '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
Cl2 Ni1 Cl2 94.37(3) 2_655 . ?
N2 Ni1 Cl2 91.01(4) 2_655 . ?
N2 Ni1 Cl2 91.01(4) . 2_655 ?
N2 Ni1 Cl2 170.67(4) . . ?
N2 Ni1 Cl2 170.67(4) 2_655 2_655 ?
N2 Ni1 N2 84.73(8) . 2_655 ?
N4 Ni1 Cl2 90.64(5) 2_655 . ?
N4 Ni1 Cl2 90.63(4) . 2_655 ?
N4 Ni1 Cl2 94.33(4) 2_655 2_655 ?
N4 Ni1 Cl2 94.33(4) . . ?
N4 Ni1 N2 77.97(6) . . ?
N4 Ni1 N2 77.97(6) 2_655 2_655 ?
N4 Ni1 N2 96.57(6) . 2_655 ?
N4 Ni1 N2 96.56(6) 2_655 . ?
N4 Ni1 N4 172.69(8) . 2_655 ?
C4 N2 Ni1 111.84(12) . . ?
C4 N2 C12 107.01(16) . . ?
C12 N2 Ni1 140.62(13) . . ?
C2 N4 Ni1 116.86(12) . . ?
C14 N4 Ni1 124.48(13) . . ?
C14 N4 C2 118.37(16) . . ?
C4 N6 C8 107.34(15) . . ?
C4 N6 C18 132.60(17) . . ?
C18 N6 C8 120.05(17) . . ?
N4 C2 C4 112.21(15) . . ?
N4 C2 C6 121.56(16) . . ?
C6 C2 C4 126.18(17) . . ?
N2 C4 N6 109.99(16) . . ?
N2 C4 C2 120.33(16) . . ?
N6 C4 C2 129.65(16) . . ?
C10 C6 C2 118.45(17) . . ?
N6 C8 C20 119.98(19) . . ?
C12 C8 N6 104.56(16) . . ?
C12 C8 C20 135.4(2) . . ?
C16 C10 C6 119.99(18) . . ?
N2 C12 Cl4 124.00(15) . . ?
N2 C12 C8 111.09(17) . . ?
C8 C12 Cl4 124.91(15) . . ?
N4 C14 C16 123.45(19) . . ?
C10 C16 C14 118.12(19) . . ?
C24 C18 N6 119.0(2) . . ?
C22 C20 C8 119.3(2) . . ?
C20 C22 C24 119.8(2) . . ?
C18 C24 C22 121.7(2) . . ?
Cl6 C25 Cl6 112.2(3) 2_655 . ?
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
Ni1 Cl2 2.4118(5) . ?
Ni1 Cl2 2.4117(5) 2_655 ?
Ni1 N2 2.1273(16) 2_655 ?
Ni1 N2 2.1273(16) . ?
Ni1 N4 2.0967(15) . ?
Ni1 N4 2.0967(15) 2_655 ?
Cl4 C12 1.7112(19) . ?
N2 C4 1.338(2) . ?
N2 C12 1.345(2) . ?
N4 C2 1.353(2) . ?
N4 C14 1.329(2) . ?
N6 C4 1.369(2) . ?
N6 C8 1.402(2) . ?
N6 C18 1.390(3) . ?
C2 C4 1.460(2) . ?
C2 C6 1.393(3) . ?
C6 C10 1.384(3) . ?
C8 C12 1.378(3) . ?
C8 C20 1.406(3) . ?
C10 C16 1.371(3) . ?
C14 C16 1.381(3) . ?
C18 C24 1.349(3) . ?
C20 C22 1.353(4) . ?
C22 C24 1.419(4) . ?
Cl6 C25 1.750(3) . ?
C25 Cl6 1.750(3) 2_655 ?
