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_7713739
_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         '2(C5 H8 N8 O7 Zn), 4(C3 H7 N O)'
_chemical_formula_sum            'C22 H44 N20 O18 Zn2'
_chemical_formula_weight         1007.51
_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
_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                68.2650(10)
_cell_angle_beta                 87.1700(10)
_cell_angle_gamma                84.8060(10)
_cell_formula_units_Z            2
_cell_length_a                   11.7885(4)
_cell_length_b                   12.0697(4)
_cell_length_c                   15.7929(6)
_cell_measurement_reflns_used    9953
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.34
_cell_measurement_theta_min      2.42
_cell_volume                     2078.44(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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.996
_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  0.0378
_diffrn_reflns_av_unetI/netI     0.0396
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            34401
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.357
_diffrn_reflns_theta_min         2.641
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.249
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1283 before and 0.0527 after correction.
The Ratio of minimum to maximum transmission is 0.9001.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear yellowish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   yellowish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.610
_exptl_crystal_description       block
_exptl_crystal_F_000             1040
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.048
_refine_diff_density_min         -0.930
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       0.0019(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     578
_refine_ls_number_reflns         10350
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0557
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+4.2169P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1253
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8721
_reflns_number_total             10350
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt02410e2.cif
_cod_data_source_block           21novb_0m_a
_cod_database_code               7713739
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.865
_shelx_estimated_absorpt_t_min   0.788
_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
 Zn2-H10A \\sim Zn2-H10B
 with sigma of 0.02
 Zn1-H2A \\sim Zn1-H2B
 with sigma of 0.02
3.a Free rotating group:
 O10(H10A,H10B), O2(H2A,H2B)
3.b Rotating group:
 O8(H8A,H8B), O1(H1A,H1B), O9(H9A,H9B), O3(H3A,H3B)
3.c Aromatic/amide H refined with riding coordinates:
 N6(H6A), N14(H14), C1(H1), C6(H6), C22(H22), C16(H16), C13(H13), C19(H19)
3.d Idealised Me refined as rotating group:
 C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C12(H12A,H12B,H12C), C21(H21A,H21B,
 H21C), C11(H11A,H11B,H11C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C14(H14A,
 H14B,H14C)
;
_shelx_res_checksum              6979
_olex2_submission_special_instructions 'No special instructions were received'