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#$Date: 2023-11-10 01:53:36 +0200 (Fri, 10 Nov 2023) $
#$Revision: 287497 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/44/7714436.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_7714436
loop_
_publ_author_name
'Vorobyova, Anna'
'Lyssenko, Konstantin'
'Chistyakov, Gregory'
'Morozov, Igor V.'
'Ovchenkov, Yevgeny'
'Vasilchikova, Tatyana M.'
'Koo, Hyun-Joo'
'Whangbo, Mike'
'Volkova, Olga S.'
'Vasiliev, Alexander'
_publ_section_title
;
 Combination of Organic and Inorganic Cations in Synthesis of Transition
 Metal Nitrates: Preparation and Characterization of Canted Rectangular
 Ising Antiferromagnet (PyH)CsCo2(NO3)6
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT03159D
_journal_year                    2023
_chemical_formula_moiety         'Ni2 Cs N6 O18, C5 H6 N'
_chemical_formula_sum            'C5 H6 Cs N7 Ni2 O18'
_chemical_formula_weight         702.50
_space_group_crystal_system      orthorhombic
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2023-08-28 deposited with the CCDC.	2023-11-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.632(3)
_cell_length_b                   11.859(4)
_cell_length_c                   18.173(4)
_cell_measurement_reflns_used    5791
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.43
_cell_measurement_theta_min      2.45
_cell_volume                     1860.3(10)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker D8 Quest with Photon III detector'
_diffrn_measurement_method       'φ and ω shutterless scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0671
_diffrn_reflns_av_unetI/netI     0.0437
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17611
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.997
_diffrn_reflns_theta_min         2.051
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.064
_exptl_absorpt_correction_T_max  0.4983
_exptl_absorpt_correction_T_min  0.4018
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    2.508
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.558
_refine_diff_density_rms         0.121
_refine_ls_extinction_coef       0.00138(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_gt           0.0243
_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)+(0.0220P)²+0.7844P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0564
_refine_ls_wR_factor_ref         0.0588
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2266
_reflns_number_total             2581
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d3dt03159d2.cif
_cod_data_source_block           csni
_cod_original_cell_volume        1860.4(9)
_cod_database_code               7714436
_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_min   0.366
_shelx_estimated_absorpt_t_max   0.482
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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
Cs1 Cs 0.42373(2) 0.750000 0.61474(2) 0.00978(8) Uani 1 2 d S T P . .
Ni1 Ni 0.20697(3) 0.50030(3) 0.31182(2) 0.00731(9) Uani 1 1 d . . . . .
O7 O 0.1934(2) 0.65922(15) 0.26427(9) 0.0118(4) Uani 1 1 d . . . . .
O9 O 0.2350(2) 0.34052(14) 0.35353(10) 0.0119(4) Uani 1 1 d . . . . .
N4 N 0.1765(3) 0.250000 0.32831(15) 0.0093(6) Uani 1 2 d S T P . .
O4 O -0.0176(2) 0.49507(15) 0.28089(9) 0.0107(3) Uani 1 1 d . . . . .
N3 N 0.2450(3) 0.750000 0.29197(16) 0.0097(6) Uani 1 2 d S T P . .
O10 O 0.0706(3) 0.250000 0.28384(13) 0.0114(5) Uani 1 2 d S T P . .
O6 O -0.0948(2) 0.40770(16) 0.38065(9) 0.0127(4) Uani 1 1 d . . . . .
O3 O 0.3923(2) 0.59649(17) 0.48342(10) 0.0179(4) Uani 1 1 d . . . . .
O2 O 0.4122(2) 0.52241(16) 0.37367(9) 0.0115(4) Uani 1 1 d . . . . .
O5 O -0.25334(19) 0.43661(15) 0.29041(9) 0.0106(3) Uani 1 1 d . . . . .
O8 O 0.3393(3) 0.750000 0.34228(14) 0.0150(5) Uani 1 2 d S T P . .
O1 O 0.18769(19) 0.56081(16) 0.41741(9) 0.0120(4) Uani 1 1 d . . . . .
N2 N -0.1193(2) 0.44560(17) 0.31903(11) 0.0079(4) Uani 1 1 d . . . . .
N1 N 0.3338(2) 0.56118(18) 0.42740(11) 0.0107(4) Uani 1 1 d . . . . .
N1S N 0.6658(4) 0.750000 0.39519(19) 0.0338(11) Uani 1 2 d S T P . .
C4S C 0.9132(4) 0.750000 0.4833(2) 0.0186(8) Uani 1 2 d S T P . .
C3S C 0.8503(4) 0.8509(2) 0.46123(17) 0.0232(6) Uani 1 1 d . . . . .
C2S C 0.7245(3) 0.8488(3) 0.41645(18) 0.0304(8) Uani 1 1 d . . . . .
H1 H 1.003689 0.749850 0.513546 0.020(11) Uiso 1 2 d R . P . .
H2 H 0.889779 0.921630 0.477826 0.035(10) Uiso 1 1 d R . . . .
H3 H 0.685539 0.920900 0.401086 0.058(13) Uiso 1 1 d R . . . .
H1SA H 0.585619 0.749850 0.368136 0.06(2) Uiso 1 2 d R . P . .
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'
N N 0.0061 0.0033 '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'
Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cs Cs -0.3680 2.1192 '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
O3 Cs1 O3 74.32(8) 7_575 . ?
O3 Cs1 O10 142.48(4) 7_575 2_565 ?
O3 Cs1 O10 142.48(4) . 2_565 ?
O3 Cs1 O5 88.11(5) 7_575 3_556 ?
O3 Cs1 O5 144.21(5) . 3_556 ?
O10 Cs1 O5 57.54(4) 2_565 3_556 ?
O3 Cs1 O5 144.21(5) 7_575 5_566 ?
O3 Cs1 O5 88.11(5) . 5_566 ?
O10 Cs1 O5 57.54(4) 2_565 5_566 ?
O5 Cs1 O5 88.65(7) 3_556 5_566 ?
O3 Cs1 O9 91.32(5) 7_575 3_656 ?
O3 Cs1 O9 115.46(5) . 3_656 ?
O10 Cs1 O9 78.72(5) 2_565 3_656 ?
O5 Cs1 O9 95.48(5) 3_556 3_656 ?
O5 Cs1 O9 124.47(4) 5_566 3_656 ?
O3 Cs1 O9 115.46(5) 7_575 5_666 ?
O3 Cs1 O9 91.32(5) . 5_666 ?
O10 Cs1 O9 78.72(5) 2_565 5_666 ?
O5 Cs1 O9 124.47(4) 3_556 5_666 ?
O5 Cs1 O9 95.48(5) 5_566 5_666 ?
O9 Cs1 O9 39.36(6) 3_656 5_666 ?
O3 Cs1 O6 106.05(5) 7_575 5_566 ?
O3 Cs1 O6 67.18(5) . 5_566 ?
O10 Cs1 O6 89.35(5) 2_565 5_566 ?
O5 Cs1 O6 89.03(5) 3_556 5_566 ?
O5 Cs1 O6 38.25(4) 5_566 5_566 ?
O9 Cs1 O6 162.21(4) 3_656 5_566 ?
O9 Cs1 O6 125.58(5) 5_666 5_566 ?
O3 Cs1 O6 67.18(5) 7_575 3_556 ?
O3 Cs1 O6 106.05(5) . 3_556 ?
O10 Cs1 O6 89.35(5) 2_565 3_556 ?
O5 Cs1 O6 38.25(4) 3_556 3_556 ?
O5 Cs1 O6 89.03(5) 5_566 3_556 ?
O9 Cs1 O6 125.58(5) 3_656 3_556 ?
O9 Cs1 O6 162.21(4) 5_666 3_556 ?
O6 Cs1 O6 66.72(7) 5_566 3_556 ?
O3 Cs1 O2 62.03(5) 7_575 3_656 ?
O3 Cs1 O2 129.46(5) . 3_656 ?
O10 Cs1 O2 86.22(3) 2_565 3_656 ?
O5 Cs1 O2 60.98(5) 3_556 3_656 ?
O5 Cs1 O2 142.42(4) 5_566 3_656 ?
O9 Cs1 O2 46.45(4) 3_656 3_656 ?
O9 Cs1 O2 85.80(5) 5_666 3_656 ?
O6 Cs1 O2 146.71(4) 5_566 3_656 ?
O6 Cs1 O2 80.24(5) 3_556 3_656 ?
O3 Cs1 O2 129.46(5) 7_575 5_666 ?
O3 Cs1 O2 62.03(5) . 5_666 ?
O10 Cs1 O2 86.22(3) 2_565 5_666 ?
O5 Cs1 O2 142.42(4) 3_556 5_666 ?
O5 Cs1 O2 60.98(5) 5_566 5_666 ?
O9 Cs1 O2 85.80(5) 3_656 5_666 ?
O9 Cs1 O2 46.45(4) 5_666 5_666 ?
O6 Cs1 O2 80.24(5) 5_566 5_666 ?
O6 Cs1 O2 146.71(4) 3_556 5_666 ?
O2 Cs1 O2 132.19(6) 3_656 5_666 ?
O3 Cs1 N4 108.28(5) 7_575 5_666 ?
O3 Cs1 N4 108.28(5) . 5_666 ?
O10 Cs1 N4 72.39(7) 2_565 5_666 ?
O5 Cs1 N4 106.77(4) 3_556 5_666 ?
O5 Cs1 N4 106.77(4) 5_566 5_666 ?
O9 Cs1 N4 20.43(3) 3_656 5_666 ?
O9 Cs1 N4 20.43(3) 5_666 5_666 ?
O6 Cs1 N4 142.43(4) 5_566 5_666 ?
O6 Cs1 N4 142.43(4) 3_556 5_666 ?
O2 Cs1 N4 66.36(3) 3_656 5_666 ?
O2 Cs1 N4 66.36(3) 5_666 5_666 ?
O4 Ni1 O5 84.04(7) . 6_656 ?
O4 Ni1 O9 100.80(7) . . ?
O5 Ni1 O9 88.55(7) 6_656 . ?
O4 Ni1 O1 101.12(7) . . ?
O5 Ni1 O1 174.70(7) 6_656 . ?
O9 Ni1 O1 89.26(7) . . ?
O4 Ni1 O7 81.83(7) . . ?
O5 Ni1 O7 88.08(7) 6_656 . ?
O9 Ni1 O7 175.49(7) . . ?
O1 Ni1 O7 93.84(7) . . ?
O4 Ni1 O2 162.96(7) . . ?
O5 Ni1 O2 112.98(7) 6_656 . ?
O9 Ni1 O2 79.61(7) . . ?
O1 Ni1 O2 61.85(7) . . ?
O7 Ni1 O2 98.97(7) . . ?
N3 O7 Ni1 125.81(16) . . ?
N4 O9 Ni1 126.77(16) . . ?
N4 O9 Cs1 98.50(15) . 5_666 ?
Ni1 O9 Cs1 119.07(7) . 5_666 ?
O10 N4 O9 122.42(14) . 7_565 ?
O10 N4 O9 122.42(14) . . ?
O9 N4 O9 115.2(3) 7_565 . ?
O10 N4 Cs1 155.2(2) . 5_666 ?
O9 N4 Cs1 61.07(14) 7_565 5_666 ?
O9 N4 Cs1 61.07(14) . 5_666 ?
N2 O4 Ni1 121.94(14) . . ?
O8 N3 O7 121.97(14) . . ?
O8 N3 O7 121.97(14) . 7_575 ?
O7 N3 O7 116.1(3) . 7_575 ?
N4 O10 Cs1 130.6(2) . 2_564 ?
N2 O6 Cs1 94.57(13) . 5_566 ?
N1 O3 Cs1 155.77(16) . . ?
N1 O2 Ni1 90.39(13) . . ?
N1 O2 Cs1 119.82(14) . 5_666 ?
Ni1 O2 Cs1 104.72(7) . 5_666 ?
N2 O5 Ni1 119.68(14) . 6_556 ?
N2 O5 Cs1 104.96(13) . 5_566 ?
Ni1 O5 Cs1 132.70(7) 6_556 5_566 ?
N1 O1 Ni1 93.10(13) . . ?
O6 N2 O4 123.5(2) . . ?
O6 N2 O5 120.00(19) . . ?
O4 N2 O5 116.53(19) . . ?
O6 N2 Cs1 66.18(12) . 5_566 ?
O4 N2 Cs1 164.12(14) . 5_566 ?
O5 N2 Cs1 55.66(11) . 5_566 ?
O3 N1 O1 122.3(2) . . ?
O3 N1 O2 123.2(2) . . ?
O1 N1 O2 114.56(19) . . ?
C2S N1S C2S 122.9(4) . 7_575 ?
C2S N1S H1SA 118.6 . . ?
C2S N1S H1SA 118.4 7_575 . ?
C3S C4S C3S 121.2(4) 7_575 . ?
C3S C4S H1 119.3 7_575 . ?
C3S C4S H1 119.5 . . ?
C2S C3S C4S 118.4(3) . . ?
C2S C3S H2 119.4 . . ?
C4S C3S H2 122.2 . . ?
N1S C2S C3S 119.6(3) . . ?
N1S C2S H3 124.4 . . ?
C3S C2S H3 116.0 . . ?
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
Cs1 O3 3.0139(19) 7_575 ?
Cs1 O3 3.0139(19) . ?
Cs1 O10 3.074(3) 2_565 ?
Cs1 O5 3.1674(18) 3_556 ?
Cs1 O5 3.1674(18) 5_566 ?
Cs1 O9 3.188(2) 3_656 ?
Cs1 O9 3.188(2) 5_666 ?
Cs1 O6 3.401(2) 5_566 ?
Cs1 O6 3.401(2) 3_556 ?
Cs1 O2 3.534(2) 3_656 ?
Cs1 O2 3.534(2) 5_666 ?
Cs1 N4 3.603(3) 5_666 ?
Ni1 O4 2.0190(18) . ?
Ni1 O5 2.0345(17) 6_656 ?
Ni1 O9 2.0551(18) . ?
Ni1 O1 2.0556(18) . ?
Ni1 O7 2.0767(19) . ?
Ni1 O2 2.1145(18) . ?
O7 N3 1.269(2) . ?
O9 N4 1.272(2) . ?
N4 O10 1.220(4) . ?
O4 N2 1.263(3) . ?
N3 O8 1.224(4) . ?
O6 N2 1.225(2) . ?
O3 N1 1.211(3) . ?
O2 N1 1.274(3) . ?
O5 N2 1.273(3) . ?
O1 N1 1.274(3) . ?
N1S C2S 1.334(4) . ?
N1S C2S 1.334(4) 7_575 ?
N1S H1SA 0.8489 . ?
C4S C3S 1.373(4) 7_575 ?
C4S C3S 1.373(3) . ?
C4S H1 0.9554 . ?
C3S C2S 1.358(5) . ?
C3S H2 0.9546 . ?
C2S H3 0.9601 . ?
