Energetic coordination compounds: self-assembled from the nitrogen-rich energetic C-C bonded pyrazole and triazole
Yadav, Abhishek Kumar; Rajak, Richa; Ghule, Vikas; Dharavath, Srinivas; Dalton Transactions  (2023) –; doi:10.1039/D3DT02410E

data_7713740
_publ_section_title
;
 Energetic coordination compounds: self-assembled from the nitrogen-rich
 energetic C-C bonded pyrazole and triazole
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT02410E
_journal_year                    2023
_chemical_formula_moiety         'C10 H20 N14 Ni2 O10, 2(N O3)'
_chemical_formula_sum            'C10 H20 N16 Ni2 O16'
_chemical_formula_weight         737.755
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_audit_creation_date             2023-07-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272)
;
_audit_update_record
;
2023-07-27 deposited with the CCDC.	2023-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.443(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.187(2)
_cell_length_b                   10.547(3)
_cell_length_c                   13.348(3)
_cell_measurement_reflns_used    8304
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.52
_cell_volume                     1219.6(5)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.9981
_diffrn_measured_fraction_theta_max 0.9981
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_unetI/netI     0.0390
_diffrn_reflns_Laue_measured_fraction_full 0.9981
_diffrn_reflns_Laue_measured_fraction_max 0.9981
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3047
_diffrn_reflns_point_group_measured_fraction_full 0.9981
_diffrn_reflns_point_group_measured_fraction_max 0.9981
_diffrn_reflns_theta_full        25.0499
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.04
_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    1.656
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2012/1 (Bruker,2012) was used for absorption correction.

Final HKLF 4 output contains 27674 reflections, Rint = 0.0665
 (17030 with I > 3sig(I), Rint = 0.0596)
;
_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    2.009
_exptl_crystal_description       block
_exptl_crystal_F_000             753.904
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   1.66
_exptl_transmission_factor_min   0.23
_refine_diff_density_max         0.6384
_refine_diff_density_min         -0.5755
_refine_diff_density_rms         0.1503
_refine_ls_d_res_high            0.8393
_refine_ls_d_res_low             6.6945
_refine_ls_goodness_of_fit_ref   1.0707
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    11
_refine_ls_number_parameters     221
_refine_ls_number_reflns         2154
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.0704
_refine_ls_R_factor_all          0.0470
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.0002
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0537P)^2^+6.5382P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1196
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              7
_reflns_limit_h_min              -10
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              -6
_reflns_number_gt                1983
_reflns_number_total             2154
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d3dt02410e2.cif
_cod_data_source_block           13augc_0m_4_a
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7713740
_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 N(H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O1_1-H1a
 0.85 with sigma of 0.02
3.a Aromatic/amide H refined with riding coordinates:
 C1(H1)
3.b X=CH2 refined with riding coordinates:
 N7(H7a,H7b)
;
_olex2_submission_special_instructions 'No special instructions were received'