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_7248069
_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 Cl4 Cu N8, 2(N O3)'
_chemical_formula_sum            'C12 H12 Cl4 Cu N10 O6'
_chemical_formula_weight         597.66
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_block_doi                 10.5517/ccdc.csd.cc2h8734
_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                 102.767(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   38.031(3)
_cell_length_b                   7.9094(8)
_cell_length_c                   14.7249(11)
_cell_measurement_reflns_used    3735
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.228
_cell_measurement_theta_min      2.197
_cell_volume                     4319.8(6)
_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    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0494
_diffrn_reflns_av_unetI/netI     0.0560
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       43
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            10045
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.018
_diffrn_reflns_theta_max         25.018
_diffrn_reflns_theta_min         2.196
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.561
_exptl_absorpt_correction_T_max  0.8228
_exptl_absorpt_correction_T_min  0.6779
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_meas      1.838
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2392
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.554
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         3800
_refine_ls_number_restraints     173
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.0916
_refine_ls_R_factor_gt           0.0759
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0522P)^2^+63.8785P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1873
_refine_ls_wR_factor_ref         0.1943
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3015
_reflns_number_total             3800
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ce01182h2.cif
_cod_data_source_block           220703f
_cod_depositor_comments
'Adding full bibliography for 7248065--7248069.cif.'
_cod_original_cell_volume        4319.8(7)
_cod_database_code               7248069
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.823
_shelx_estimated_absorpt_t_min   0.678
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
2. Restrained distances
 O1-O2' = O2'-O3' = O3'-O1 = O4'-O5' = O5'-O6 = O6-O4'
 2.15 with sigma of 0.02
 N9-O2' = N9-O3' = N10-O4' = N10-O5
 1.21 with sigma of 0.01
3. Restrained planarity
 N10, O4', O5', O6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O2' \\sim O3' \\sim O4'
\\sim O5': within 3.8A with sigma of 0.02 and sigma for terminal atoms of 0.04
within 3.8A
5. Others
 Sof(O2')=Sof(O3')=1-FVAR(1)
 Sof(O2)=Sof(O3)=FVAR(1)
 Sof(O4')=Sof(O5')=1-FVAR(2)
 Sof(O4)=Sof(O5)=FVAR(2)
6.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), N6(H6), N8(H8), C1(H1), C3(H3), C4(H4A), C6(H6A), C7(H7),
 C9(H9), C10(H10), C12(H12)
;
_olex2_submission_special_instructions 'No special instructions were received'