#------------------------------------------------------------------------------
#$Date: 2022-05-20 12:25:47 +0300 (Fri, 20 May 2022) $
#$Revision: 275576 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/53/8105320.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_8105320
loop_
_publ_author_name
'Li, Jun-Xia'
'Du, Zhong-Xiang'
_publ_section_title
;
 The crystal structure of catena-poly[(μ2-4,4′-dipyridine-κ2
 N,N′)-bis(3,5,6-trichloropyridine-2-oxyacetato-\kO)-bis(ethanol-\kO)nickel(II)],
 C28H26Cl6N4NiO8
;
_journal_issue                   4
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              887
_journal_page_last               890
_journal_paper_doi               10.1515/ncrs-2020-0083
_journal_volume                  235
_journal_year                    2020
_chemical_formula_moiety         '0.5(C56 H52 Cl12 N8 Ni2 O16)'
_chemical_formula_sum            'C28 H26 Cl6 N4 Ni O8'
_chemical_formula_weight         817.94
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_cell_angle_alpha                90
_cell_angle_beta                 99.609(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.7577(10)
_cell_length_b                   12.6174(7)
_cell_length_c                   16.7333(10)
_cell_measurement_reflns_used    1450
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      22.7420
_cell_measurement_theta_min      3.7700
_cell_volume                     3280.3(3)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_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      291.2(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0584
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
--------------------------------------------------------------------------
  1  ω    -81.00 -38.00   1.00    2.00    --  -13.49-178.00-150.00   43
  2  ω    -11.00  25.00   1.00    2.00    --  -13.49 -99.00  90.00   36
  3  ω    -20.00  22.00   1.00    2.00    --  -13.49 -99.00 -30.00   42
  4  ω    -52.00  37.00   1.00    2.00    --   14.89 -77.00-150.00   89
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'SuperNova, Single source at offset/far, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0190633000
_diffrn_orient_matrix_UB_12      0.0308472000
_diffrn_orient_matrix_UB_13      -0.0336787000
_diffrn_orient_matrix_UB_21      0.0242587000
_diffrn_orient_matrix_UB_22      -0.0280712000
_diffrn_orient_matrix_UB_23      -0.0252124000
_diffrn_orient_matrix_UB_31      -0.0336676000
_diffrn_orient_matrix_UB_32      -0.0376844000
_diffrn_orient_matrix_UB_33      -0.0088015000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0507
_diffrn_reflns_av_unetI/netI     0.0926
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7139
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.437
_diffrn_reflns_theta_min         3.288
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.136
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.97825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_description       block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.659
_refine_diff_density_min         -0.596
_refine_diff_density_rms         0.095
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     217
_refine_ls_number_reflns         3421
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1129
_refine_ls_R_factor_gt           0.0674
_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)+(0.0505P)²+8.2614P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1665
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2154
_reflns_number_total             3421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2020-0083_suppl.cif
_cod_data_source_block           ljx191111-3
_cod_database_code               8105320
_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   0.788
_shelx_estimated_absorpt_t_min   0.734
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     25.30
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 O4-H4
 0.85 with sigma of 0.01
 C13-H4
 1.867415 with sigma of 0.02
 Ni1-H4
 2.669545 with sigma of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C13(H13A,H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C9(H9), C8(H8), C12(H12), C11(H11), C5(H5)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C)
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -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
C1 C 0.7488(3) 0.4078(4) 0.3258(3) 0.0379(12) Uani 1 1 d . . . . .
C2 C 0.7127(4) 0.3887(4) 0.2373(3) 0.0414(13) Uani 1 1 d . . . . .
H2A H 0.7416 0.3282 0.2182 0.050 Uiso 1 1 calc R . . . .
H2B H 0.6520 0.3717 0.2321 0.050 Uiso 1 1 calc R . . . .
C3 C 0.6715(3) 0.5633(4) 0.1934(3) 0.0408(13) Uani 1 1 d . . . . .
C4 C 0.6951(4) 0.6599(4) 0.1645(4) 0.0517(15) Uani 1 1 d . . . . .
C5 C 0.6454(4) 0.7480(5) 0.1724(4) 0.0599(17) Uani 1 1 d . . . . .
H5 H 0.6608 0.8144 0.1554 0.072 Uiso 1 1 calc R . . . .
C6 C 0.5715(4) 0.7347(4) 0.2068(4) 0.0543(16) Uani 1 1 d . . . . .
C7 C 0.5525(3) 0.6362(5) 0.2317(3) 0.0466(14) Uani 1 1 d . . . . .
C8 C 0.5976(3) 0.2057(4) 0.5490(3) 0.0442(13) Uani 1 1 d . . . . .
H8 H 0.5999 0.2613 0.5858 0.053 Uiso 1 1 calc R . . . .
C9 C 0.5386(3) 0.1276(4) 0.5532(3) 0.0435(13) Uani 1 1 d . . . . .
H9 H 0.5032 0.1307 0.5924 0.052 Uiso 1 1 calc R . . . .
C10 C 0.5312(3) 0.0435(4) 0.4989(3) 0.0325(11) Uani 1 1 d . . . . .
C11 C 0.5867(4) 0.0459(4) 0.4435(3) 0.0547(16) Uani 1 1 d . . . . .
H11 H 0.5848 -0.0081 0.4055 0.066 Uiso 1 1 calc R . . . .
C12 C 0.6452(4) 0.1277(5) 0.4439(4) 0.0557(16) Uani 1 1 d . . . . .
H12 H 0.6816 0.1266 0.4056 0.067 Uiso 1 1 calc R . . . .
C13 C 0.8826(5) 0.5237(6) 0.5548(4) 0.097(3) Uani 1 1 d D . . . .
H13A H 0.9334 0.4930 0.5872 0.117 Uiso 1 1 calc R . . . .
H13B H 0.8415 0.5370 0.5908 0.117 Uiso 1 1 calc R . . . .
C14 C 0.9061(6) 0.6224(6) 0.5252(5) 0.120(3) Uani 1 1 d . . . . .
H14A H 0.8573 0.6531 0.4910 0.181 Uiso 1 1 calc GR . . . .
H14B H 0.9518 0.6121 0.4945 0.181 Uiso 1 1 calc GR . . . .
H14C H 0.9253 0.6690 0.5699 0.181 Uiso 1 1 calc GR . . . .
Cl1 Cl 0.78527(12) 0.67082(15) 0.11876(13) 0.0864(7) Uani 1 1 d . . . . .
Cl2 Cl 0.50957(14) 0.84462(14) 0.21820(14) 0.0975(7) Uani 1 1 d . . . . .
Cl3 Cl 0.46002(10) 0.61493(14) 0.27188(10) 0.0668(5) Uani 1 1 d . . . . .
N1 N 0.6018(3) 0.5516(3) 0.2259(2) 0.0412(11) Uani 1 1 d . . . . .
N2 N 0.6521(2) 0.2079(3) 0.4962(2) 0.0343(9) Uani 1 1 d . . . . .
Ni1 Ni 0.7500 0.32936(6) 0.5000 0.0262(2) Uani 1 2 d DS T P . .
O1 O 0.7342(2) 0.3337(2) 0.3724(2) 0.0397(8) Uani 1 1 d . . . . .
O2 O 0.7901(3) 0.4905(3) 0.3453(2) 0.0568(11) Uani 1 1 d . . . . .
O3 O 0.7229(2) 0.4792(3) 0.1871(2) 0.0499(10) Uani 1 1 d . . . . .
O4 O 0.8467(3) 0.4474(3) 0.4975(2) 0.0553(11) Uani 1 1 d D . . . .
H4 H 0.846(3) 0.477(3) 0.4507(8) 0.083 Uiso 1 1 d DR . . . .
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'
O O 0.0106 0.0060 '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
O1 Ni1 O1 177.05(17) 2_656 .
O1 Ni1 O4 92.19(13) 2_656 .
O1 Ni1 O4 85.76(13) . .
O1 Ni1 O4 85.75(13) 2_656 2_656
O1 Ni1 O4 92.19(13) . 2_656
O1 Ni1 N2 90.62(14) . 2_656
O1 Ni1 N2 90.62(14) 2_656 .
O1 Ni1 N2 91.46(14) . .
O1 Ni1 N2 91.46(14) 2_656 2_656
O4 Ni1 O4 91.6(2) . 2_656
O4 Ni1 N2 89.28(15) . 2_656
O4 Ni1 N2 89.28(15) 2_656 .
O4 Ni1 N2 177.13(14) . .
O4 Ni1 N2 177.13(14) 2_656 2_656
N2 Ni1 N2 90.0(2) 2_656 .
C1 O1 Ni1 129.8(3) . .
C3 O3 C2 116.8(4) . .
Ni1 O4 H4 114.8(16) . .
C13 O4 Ni1 132.0(4) . .
C13 O4 H4 105.1(16) . .
C8 N2 Ni1 122.0(3) . .
C12 N2 Ni1 122.5(3) . .
C12 N2 C8 115.4(4) . .
C3 N1 C7 118.6(5) . .
C9 C10 C10 122.3(5) . 5_656
C11 C10 C10 122.2(6) . 5_656
C11 C10 C9 115.5(4) . .
O1 C1 C2 114.0(4) . .
O2 C1 O1 126.9(5) . .
O2 C1 C2 119.0(5) . .
N1 C7 Cl3 116.4(4) . .
N1 C7 C6 123.3(5) . .
C6 C7 Cl3 120.3(4) . .
C10 C9 H9 119.9 . .
C8 C9 C10 120.1(4) . .
C8 C9 H9 119.9 . .
O3 C3 C4 117.7(5) . .
N1 C3 O3 119.9(5) . .
N1 C3 C4 122.4(5) . .
N2 C8 C9 124.7(5) . .
N2 C8 H8 117.6 . .
C9 C8 H8 117.6 . .
O3 C2 C1 112.5(4) . .
O3 C2 H2A 109.1 . .
O3 C2 H2B 109.1 . .
C1 C2 H2A 109.1 . .
C1 C2 H2B 109.1 . .
H2A C2 H2B 107.8 . .
C3 C4 Cl1 120.9(4) . .
C5 C4 Cl1 120.0(4) . .
C5 C4 C3 119.0(5) . .
C7 C6 Cl2 122.9(5) . .
C7 C6 C5 118.6(5) . .
C5 C6 Cl2 118.5(5) . .
N2 C12 H12 118.2 . .
N2 C12 C11 123.5(5) . .
C11 C12 H12 118.2 . .
C10 C11 C12 120.7(5) . .
C10 C11 H11 119.6 . .
C12 C11 H11 119.6 . .
C4 C5 C6 118.1(5) . .
C4 C5 H5 121.0 . .
C6 C5 H5 121.0 . .
O4 C13 H13A 107.9 . .
O4 C13 H13B 107.9 . .
O4 C13 C14 117.5(6) . .
H13A C13 H13B 107.2 . .
C14 C13 H13A 107.9 . .
C14 C13 H13B 107.9 . .
C13 C14 H14A 109.5 . .
C13 C14 H14B 109.5 . .
C13 C14 H14C 109.5 . .
H14A C14 H14B 109.5 . .
H14A C14 H14C 109.5 . .
H14B C14 H14C 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni1 O1 2.109(3) 2_656
Ni1 O1 2.109(3) .
Ni1 O4 2.136(4) .
Ni1 O4 2.136(4) 2_656
Ni1 N2 2.168(4) 2_656
Ni1 N2 2.168(4) .
Cl3 C7 1.725(5) .
Cl1 C4 1.727(6) .
Cl2 C6 1.724(5) .
O1 C1 1.263(6) .
O3 C3 1.350(6) .
O3 C2 1.442(6) .
O4 H4 0.867(10) .
O4 C13 1.409(7) .
N2 C8 1.332(6) .
N2 C12 1.330(6) .
O2 C1 1.244(6) .
N1 C7 1.333(6) .
N1 C3 1.312(6) .
C10 C10 1.478(9) 5_656
C10 C9 1.389(7) .
C10 C11 1.376(7) .
C1 C2 1.514(7) .
C7 C6 1.361(8) .
C9 H9 0.9300 .
C9 C8 1.364(7) .
C3 C4 1.385(7) .
C8 H8 0.9300 .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
C4 C5 1.379(7) .
C6 C5 1.393(8) .
C12 H12 0.9300 .
C12 C11 1.384(7) .
C11 H11 0.9300 .
C5 H5 0.9300 .
C13 H13A 0.9700 .
C13 H13B 0.9700 .
C13 C14 1.413(9) .
C14 H14A 0.9600 .
C14 H14B 0.9600 .
C14 H14C 0.9600 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O2 0.867(10) 1.843(18) 2.611(5) 147(2) .
