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_7248067
_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         'C12 H12 Cl6 Cu N8 O8'
_chemical_formula_sum            'C12 H12 Cl6 Cu N8 O8'
_chemical_formula_weight         672.54
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_block_doi                 10.5517/ccdc.csd.cc2h8756
_audit_creation_date             2023-10-18
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-10-18 deposited with the CCDC.	2024-01-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.169(3)
_cell_length_b                   9.9451(9)
_cell_length_c                   13.4069(16)
_cell_measurement_reflns_used    1947
_cell_measurement_temperature    298.15
_cell_measurement_theta_max      24.528
_cell_measurement_theta_min      2.253
_cell_volume                     4822.5(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXL 2018/3 (Sheldrick, 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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1068
_diffrn_reflns_av_unetI/netI     0.0603
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       42
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            5437
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         2.252
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.627
_exptl_absorpt_correction_T_max  0.7583
_exptl_absorpt_correction_T_min  0.6240
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.853
_exptl_crystal_density_meas      1.853
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2680
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.092
_refine_diff_density_min         -1.032
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     99
_refine_ls_number_reflns         1069
_refine_ls_number_restraints     43
_refine_ls_restrained_S_all      1.233
_refine_ls_R_factor_all          0.1081
_refine_ls_R_factor_gt           0.0930
_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^)+(0.1255P)^2^+101.8730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2395
_refine_ls_wR_factor_ref         0.2527
_reflns_Friedel_coverage         0.000
_reflns_number_gt                860
_reflns_number_total             1069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01182h2.cif
_cod_data_source_block           220621f
_cod_depositor_comments
'Adding full bibliography for 7248065--7248069.cif.'
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               7248067
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.758
_shelx_estimated_absorpt_t_min   0.624
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 Cl2-O1 = Cl2-O3 = Cl2-O2 = Cl2-O4
 1.4 with sigma of 0.01
 O1-O2 \\sim O1-O3 \\sim O1-O4 \\sim O2-O3 \\sim O2-O4 \\sim O3-O4
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Cl2 \\sim O1 \\sim O2 \\sim O3 \\sim O4: within 2A with sigma of 0.02 and sigma
for terminal atoms of 0.04 within 2A
4. Others
 Fixed Sof: O1(0.5) O2(0.5) O3(0.5) O4(0.5)
5.a Riding coordinates:
 N2(H2)
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3)
;
_olex2_submission_special_instructions 'No special instructions were received'