Synthesis of energetic coordination compounds based on pyrazole and 4-chloropyrazole via co-melting crystallization method
Lu, Zu-Jia; Wang, Ting-Wei; Sun, Mou; Xu, Mei-Qi; Zhang, Chao; Yi, Zhen-Xin; Zhang, Jian-Guo; CrystEngComm 26 (2024) 1178–1188; doi:10.1039/D3CE01182H

data_7248068
_publ_section_title
;
 Synthesis of energetic coordination compounds based on pyrazole and
 4-chloropyrazole via co-melting crystallization method
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1178
_journal_page_last               1188
_journal_paper_doi               10.1039/D3CE01182H
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C27 H33 Cu3 N18 O1, N1 O3'
_chemical_formula_sum            'C27 H33 Cu3 N19 O4'
_chemical_formula_weight         878.34
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2h8767
_audit_creation_date             2022-07-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6226)
;
_audit_update_record
;
2023-10-18 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.1710(13)
_cell_length_b                   12.1710(13)
_cell_length_c                   43.960(4)
_cell_measurement_reflns_used    3734
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.175
_cell_measurement_theta_min      2.675
_cell_volume                     5639.5(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      298.15
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0606
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       52
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            9447
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         1.99
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.742
_exptl_absorpt_correction_T_max  0.7925
_exptl_absorpt_correction_T_min  0.6056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_meas      1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2682
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.461
_refine_diff_density_min         -0.753
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     160
_refine_ls_number_reflns         2223
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0560
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1062P)^2^+0.7254P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1606
_refine_ls_wR_factor_ref         0.1678
_reflns_number_gt                1712
_reflns_number_total             2223
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d3ce01182h2.cif
_cod_data_source_block           220703g
_cod_depositor_comments
'Adding full bibliography for 7248065--7248069.cif.'
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7248068
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N6(H6), C1(H1), C2(H2), C3(H3), C4(H4a), C5(H5), C6(H6a), C7(H7),
 C8(H8), C9(H9)
;
_olex2_submission_special_instructions 'No special instructions were received'