#------------------------------------------------------------------------------
#$Date: 2024-07-05 18:57:13 +0300 (Fri, 05 Jul 2024) $
#$Revision: 293003 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/61/7716145.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_7716145
loop_
_publ_author_name
'Yadav, Abhishek Kumar'
'Rajak, Richa'
'Dharavath, Srinivas'
_publ_section_title
;
 Elevating the energetic capabilities of metal coordination compounds by
 incorporating nitrate anions.
;
_journal_issue                   24
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10093
_journal_page_last               10098
_journal_paper_doi               10.1039/d4dt01467g
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'C10 H20 N12 Ni2 O12, 4(N O3), 1.3(H2 O)'
_chemical_formula_sum            'C10 H22.6 N16 Ni2 O25.3'
_chemical_formula_weight         889.26
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-01-15
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2024-01-15 deposited with the CCDC.	2024-05-23 downloaded from the CCDC.
;
_cell_angle_alpha                91.342(3)
_cell_angle_beta                 104.194(3)
_cell_angle_gamma                112.809(2)
_cell_formula_units_Z            1
_cell_length_a                   8.4655(8)
_cell_length_b                   9.6141(9)
_cell_length_c                   10.7999(10)
_cell_measurement_reflns_used    5504
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.41
_cell_measurement_theta_min      2.32
_cell_volume                     778.58(13)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0549
_diffrn_reflns_av_unetI/netI     0.0548
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8636
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.047
_diffrn_reflns_theta_max         25.047
_diffrn_reflns_theta_min         2.764
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5184
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1522 before and 0.0710 after correction.
The Ratio of minimum to maximum transmission is 0.6952.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear greenish green'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.897
_exptl_crystal_description       block
_exptl_crystal_F_000             453
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.799
_refine_diff_density_min         -0.650
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     256
_refine_ls_number_reflns         2733
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0524
_refine_ls_R_factor_gt           0.0439
_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)+(0.0390P)²+1.5855P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1038
_refine_ls_wR_factor_ref         0.1100
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2321
_reflns_number_total             2733
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4dt01467g2.cif
_cod_data_source_block           16sepb_0m_a-sr
_cod_depositor_comments          'Adding full bibliography for 7716145.cif.'
_cod_original_formula_sum        'C10 H22.60 N16 Ni2 O25.30'
_cod_database_code               7716145
_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_max   0.878
_shelx_estimated_absorpt_t_min   0.856
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Others
 Fixed Sof: O1(0.65) H1A(0.65) H1B(0.65)
3.a Free rotating group:
 O2(H2A,H2B), O1(H1A,H1B)
3.b Rotating group:
 O3(H3A,H3B), O6(H6A,H6B)
3.c Aromatic/amide H refined with riding coordinates:
 C5(H5)
3.d X=CH2 refined with riding coordinates:
 N3(H3C,H3D)
;
_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
Ni1 Ni 0.62923(6) 0.58827(5) 0.69276(4) 0.01599(16) Uani 1 1 d . . . . .
O4 O 0.6760(3) 0.2076(3) 0.5240(2) 0.0195(5) Uani 1 1 d . . . . .
O3 O 0.4121(3) 0.4459(3) 0.7477(2) 0.0229(6) Uani 1 1 d . . . . .
H3A H 0.393152 0.493243 0.811997 0.034 Uiso 1 1 d R U . . .
H3B H 0.432611 0.368663 0.783505 0.034 Uiso 1 1 d R U . . .
O13 O 0.5572(4) -0.1585(3) 0.1763(3) 0.0346(7) Uani 1 1 d . . . . .
O14 O 1.1018(4) 1.1953(3) 0.8982(3) 0.0335(7) Uani 1 1 d . . . . .
O2 O 0.7882(4) 0.5694(3) 0.8613(3) 0.0256(6) Uani 1 1 d G . . . .
H2A H 0.747966 0.535354 0.926231 0.038 Uiso 1 1 d G U . . .
H2B H 0.901072 0.624818 0.895378 0.038 Uiso 1 1 d G U . . .
O10 O 0.8518(4) 0.3311(3) 0.0311(3) 0.0301(7) Uani 1 1 d . . . . .
O8 O 0.9246(3) 1.0641(3) 0.7154(3) 0.0282(6) Uani 1 1 d . . . . .
O11 O 0.6790(4) 0.4393(3) 0.0623(3) 0.0294(7) Uani 1 1 d . . . . .
O5 O 0.6538(4) -0.0470(4) 0.3747(3) 0.0384(8) Uani 1 1 d . . . . .
O6 O 0.8522(4) 0.7256(3) 0.6479(3) 0.0415(8) Uani 1 1 d . . . . .
H6A H 0.948853 0.814735 0.688509 0.062 Uiso 1 1 d R U . . .
H6B H 0.895616 0.716221 0.573897 0.062 Uiso 1 1 d R U . . .
N2 N 0.5370(4) 0.3553(3) 0.4605(3) 0.0183(6) Uani 1 1 d . . . . .
N5 N 0.3885(4) 0.2221(3) 0.2215(3) 0.0189(7) Uani 1 1 d . . . . .
N1 N 0.6275(4) 0.4034(3) 0.5912(3) 0.0184(7) Uani 1 1 d . . . . .
O7 O 1.0740(4) 0.9647(3) 0.8481(3) 0.0426(9) Uani 1 1 d . . . . .
N7 N 1.0334(4) 1.0741(4) 0.8215(3) 0.0273(8) Uani 1 1 d . . . . .
O12 O 0.8176(4) 0.3596(4) 0.2230(3) 0.0468(9) Uani 1 1 d . . . . .
N6 N 0.5739(5) -0.0612(4) 0.2606(3) 0.0262(7) Uani 1 1 d . . . . .
N8 N 0.7830(4) 0.3748(4) 0.1067(3) 0.0262(8) Uani 1 1 d . . . . .
N4 N 0.3205(4) 0.1375(4) 0.1057(3) 0.0223(7) Uani 1 1 d . . . . .
N3 N 0.8080(4) 0.3063(4) 0.7374(3) 0.0268(8) Uani 1 1 d . . . . .
H3C H 0.828116 0.370424 0.804756 0.032 Uiso 1 1 calc R U . . .
H3D H 0.854388 0.238299 0.745510 0.032 Uiso 1 1 calc R U . . .
C2 C 0.5689(5) 0.2419(4) 0.4264(3) 0.0189(8) Uani 1 1 d . . . . .
C3 C 0.4894(5) 0.1621(4) 0.2961(4) 0.0180(8) Uani 1 1 d . . . . .
C4 C 0.4861(5) 0.0376(4) 0.2235(4) 0.0194(8) Uani 1 1 d . . . . .
C1 C 0.7093(5) 0.3123(4) 0.6253(4) 0.0214(8) Uani 1 1 d . . . . .
C5 C 0.3746(5) 0.0242(4) 0.1029(4) 0.0217(8) Uani 1 1 d . . . . .
H5 H 0.342493 -0.050688 0.031780 0.026 Uiso 1 1 calc R U . . .
O1 O 0.9063(7) 0.7033(6) 0.4266(4) 0.0491(15) Uani 0.65 1 d G . P . .
H1A H 0.800925 0.663602 0.371924 0.074 Uiso 0.65 1 d G U P . .
H1B H 0.962756 0.786481 0.397497 0.074 Uiso 0.65 1 d G U P . .
H4 H 0.246(8) 0.147(6) 0.041(6) 0.064(19) Uiso 1 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 0.0000 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'
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
_geom_angle_publ_flag
O3 Ni1 N2 91.31(11) . 2_666 ?
O3 Ni1 N5 90.10(11) . 2_666 ?
O3 Ni1 N1 89.56(11) . . ?
O2 Ni1 O3 88.30(11) . . ?
O2 Ni1 N2 168.51(11) . 2_666 ?
O2 Ni1 N5 91.63(11) . 2_666 ?
O2 Ni1 N1 94.48(12) . . ?
O6 Ni1 O3 176.56(12) . . ?
O6 Ni1 O2 88.30(13) . . ?
O6 Ni1 N2 92.12(13) . 2_666 ?
O6 Ni1 N5 90.49(13) . 2_666 ?
O6 Ni1 N1 90.21(13) . . ?
N5 Ni1 N2 76.89(11) 2_666 2_666 ?
N1 Ni1 N2 97.01(12) . 2_666 ?
N1 Ni1 N5 173.87(11) . 2_666 ?
C2 O4 C1 103.4(3) . . ?
Ni1 O3 H3A 111.4 . . ?
Ni1 O3 H3B 110.9 . . ?
H3A O3 H3B 102.9 . . ?
Ni1 O2 H2A 122.9 . . ?
Ni1 O2 H2B 127.5 . . ?
H2A O2 H2B 104.5 . . ?
Ni1 O6 H6A 134.3 . . ?
Ni1 O6 H6B 130.5 . . ?
H6A O6 H6B 95.2 . . ?
N1 N2 Ni1 140.0(2) . 2_666 ?
C2 N2 Ni1 113.0(2) . 2_666 ?
C2 N2 N1 106.9(3) . . ?
N4 N5 Ni1 136.5(2) . 2_666 ?
C3 N5 Ni1 116.7(2) . 2_666 ?
C3 N5 N4 106.8(3) . . ?
N2 N1 Ni1 123.0(2) . . ?
C1 N1 Ni1 131.3(3) . . ?
C1 N1 N2 105.6(3) . . ?
O14 N7 O8 119.4(3) . . ?
O7 N7 O14 121.0(3) . . ?
O7 N7 O8 119.6(3) . . ?
O13 N6 C4 117.2(3) . . ?
O5 N6 O13 125.1(3) . . ?
O5 N6 C4 117.6(3) . . ?
O10 N8 O11 118.5(3) . . ?
O12 N8 O10 121.8(3) . . ?
O12 N8 O11 119.7(3) . . ?
N5 N4 H4 127(4) . . ?
C5 N4 N5 111.8(3) . . ?
C5 N4 H4 121(4) . . ?
H3C N3 H3D 120.0 . . ?
C1 N3 H3C 120.0 . . ?
C1 N3 H3D 120.0 . . ?
O4 C2 C3 126.4(3) . . ?
N2 C2 O4 112.7(3) . . ?
N2 C2 C3 120.9(3) . . ?
N5 C3 C2 112.5(3) . . ?
N5 C3 C4 108.9(3) . . ?
C4 C3 C2 138.6(3) . . ?
C3 C4 N6 129.6(3) . . ?
C5 C4 N6 124.4(3) . . ?
C5 C4 C3 106.0(3) . . ?
N1 C1 O4 111.3(3) . . ?
N3 C1 O4 118.4(3) . . ?
N3 C1 N1 130.3(3) . . ?
N4 C5 C4 106.5(3) . . ?
N4 C5 H5 126.8 . . ?
C4 C5 H5 126.8 . . ?
H1A O1 H1B 104.5 . . ?
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 O3 2.056(3) . ?
Ni1 O2 2.039(3) . ?
Ni1 O6 2.021(3) . ?
Ni1 N2 2.122(3) 2_666 ?
Ni1 N5 2.099(3) 2_666 ?
Ni1 N1 2.060(3) . ?
O4 C2 1.349(4) . ?
O4 C1 1.366(4) . ?
O3 H3A 0.9008 . ?
O3 H3B 0.9008 . ?
O13 N6 1.232(4) . ?
O14 N7 1.255(4) . ?
O2 H2A 0.8699 . ?
O2 H2B 0.8697 . ?
O10 N8 1.260(4) . ?
O8 N7 1.256(4) . ?
O11 N8 1.273(4) . ?
O5 N6 1.227(4) . ?
O6 H6A 0.9272 . ?
O6 H6B 0.9741 . ?
N2 N1 1.399(4) . ?
N2 C2 1.287(5) . ?
N5 N4 1.339(4) . ?
N5 C3 1.333(5) . ?
N1 C1 1.321(5) . ?
O7 N7 1.246(4) . ?
O12 N8 1.243(4) . ?
N6 C4 1.427(5) . ?
N4 C5 1.337(5) . ?
N4 H4 0.85(6) . ?
N3 H3C 0.8800 . ?
N3 H3D 0.8800 . ?
N3 C1 1.308(5) . ?
C2 C3 1.451(5) . ?
C3 C4 1.403(5) . ?
C4 C5 1.378(5) . ?
C5 H5 0.9500 . ?
O1 H1A 0.8701 . ?
O1 H1B 0.8698 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ni1 N2 N1 Ni1 -2.0(5) 2_666 . . . ?
Ni1 N2 N1 C1 -179.2(3) 2_666 . . . ?
Ni1 N2 C2 O4 179.4(2) 2_666 . . . ?
Ni1 N2 C2 C3 -2.2(4) 2_666 . . . ?
Ni1 N5 N4 C5 -179.0(3) 2_666 . . . ?
Ni1 N5 C3 C2 0.3(4) 2_666 . . . ?
Ni1 N5 C3 C4 -179.9(2) 2_666 . . . ?
Ni1 N1 C1 O4 -177.1(2) . . . . ?
Ni1 N1 C1 N3 5.0(6) . . . . ?
O4 C2 C3 N5 179.4(3) . . . . ?
O4 C2 C3 C4 -0.2(7) . . . . ?
O13 N6 C4 C3 -176.2(4) . . . . ?
O13 N6 C4 C5 4.8(6) . . . . ?
O5 N6 C4 C3 6.7(6) . . . . ?
O5 N6 C4 C5 -172.2(4) . . . . ?
N2 N1 C1 O4 -0.3(4) . . . . ?
N2 N1 C1 N3 -178.2(4) . . . . ?
N2 C2 C3 N5 1.3(5) . . . . ?
N2 C2 C3 C4 -178.3(4) . . . . ?
N5 N4 C5 C4 -0.8(4) . . . . ?
N5 C3 C4 N6 179.4(3) . . . . ?
N5 C3 C4 C5 -1.5(4) . . . . ?
N1 N2 C2 O4 -0.2(4) . . . . ?
N1 N2 C2 C3 178.1(3) . . . . ?
N6 C4 C5 N4 -179.5(3) . . . . ?
N4 N5 C3 C2 -178.8(3) . . . . ?
N4 N5 C3 C4 0.9(4) . . . . ?
C2 O4 C1 N1 0.1(4) . . . . ?
C2 O4 C1 N3 178.3(3) . . . . ?
C2 N2 N1 Ni1 177.5(2) . . . . ?
C2 N2 N1 C1 0.3(4) . . . . ?
C2 C3 C4 N6 -0.9(7) . . . . ?
C2 C3 C4 C5 178.2(4) . . . . ?
C3 N5 N4 C5 -0.1(4) . . . . ?
C3 C4 C5 N4 1.4(4) . . . . ?
C1 O4 C2 N2 0.1(4) . . . . ?
C1 O4 C2 C3 -178.2(3) . . . . ?
