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_7713738
_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         '0.5(C10 H16 N16 Ni2 O14), 2(C3 H7 N O)'
_chemical_formula_sum            'C11 H22 N10 Ni O9'
_chemical_formula_weight         497.09
_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     dual
_audit_creation_date             2023-07-24
_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                68.215(2)
_cell_angle_beta                 87.615(2)
_cell_angle_gamma                85.471(2)
_cell_formula_units_Z            4
_cell_length_a                   11.6407(7)
_cell_length_b                   12.0947(7)
_cell_length_c                   15.6754(9)
_cell_measurement_reflns_used    8183
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.23
_cell_volume                     2042.8(2)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0788
_diffrn_reflns_av_unetI/netI     0.0556
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            43296
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.048
_diffrn_reflns_theta_max         25.048
_diffrn_reflns_theta_min         2.230
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6710
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1121 before and 0.0693 after correction.
The Ratio of minimum to maximum transmission is 0.8998.
The \l/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    1.616
_exptl_crystal_description       block
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.413
_refine_diff_density_min         -0.527
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     577
_refine_ls_number_reflns         7235
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0818
_refine_ls_R_factor_gt           0.0593
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+8.5078P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1441
_refine_ls_wR_factor_ref         0.1586
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5600
_reflns_number_total             7235
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02410e2.cif
_cod_data_source_block           12octc_o_0m
_cod_database_code               7713738
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.871
_shelx_estimated_absorpt_t_min   0.822
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 Ni01-H1A \\sim Ni01-H1B
 with sigma of 0.02
 Ni02-H9A \\sim Ni02-H9B
 with sigma of 0.02
3.a Free rotating group:
 O1(H1A,H1B), O9(H9A,H9B)
3.b Rotating group:
 O2(H2A,H2B), O10(H10A,H10B), O3(H3A,H3B), O8(H8A,H8B)
3.c Aromatic/amide H refined with riding coordinates:
 N14(H14), N5(H5), C1(H1), C6(H6), C22(H22), C14(H14A), C19(H19), C13(H13)
3.d Idealised Me refined as rotating group:
 C17(H17A,H17B,H17C), C16(H16A,H16B,H16C), C20(H20A,H20B,H20C), C21(H21A,H21B,
 H21C), C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C), C12(H12A,
 H12B,H12C)
;
_shelx_res_checksum              68065
_olex2_submission_special_instructions 'No special instructions were received'