Simple methods for the introduction of nitrate ester, amino and diazo-oxide substituents into dinitromethylpyrazole
Zhang, Xiya; Lin, Xiangyang; New Journal of Chemistry 46 (2022) 14186–14191; doi:10.1039/D2NJ02078E

data_7061665
_publ_section_title
;
 Simple methods for the introduction of nitrate ester, amino and
 diazo-oxide substituents into dinitromethylpyrazole
;
_journal_issue                   29
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14186
_journal_page_last               14191
_journal_paper_doi               10.1039/D2NJ02078E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety         'C4 H2 Cl K N6 O9'
_chemical_formula_sum            'C4 H2 Cl K N6 O9'
_chemical_formula_weight         352.646
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-21
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2022-06-06 deposited with the CCDC.	2022-06-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.99(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.100(3)
_cell_length_b                   15.461(3)
_cell_length_c                   6.9205(19)
_cell_measurement_reflns_used    1796
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.16
_cell_measurement_theta_min      2.30
_cell_volume                     1157.3(5)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.9990
_diffrn_measured_fraction_theta_max 0.9939
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0849
_diffrn_reflns_av_unetI/netI     0.0855
_diffrn_reflns_Laue_measured_fraction_full 0.9990
_diffrn_reflns_Laue_measured_fraction_max 0.9939
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            7926
_diffrn_reflns_point_group_measured_fraction_full 0.9990
_diffrn_reflns_point_group_measured_fraction_max 0.9939
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         25.44
_diffrn_reflns_theta_min         1.88
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.755
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6468
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1322 before and 0.0751 after correction.
The Ratio of minimum to maximum transmission is 0.8680.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.024
_exptl_crystal_description       needle
_exptl_crystal_F_000             705.915
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.7131
_refine_diff_density_min         -0.8166
_refine_diff_density_rms         0.1989
_refine_ls_d_res_high            0.8274
_refine_ls_d_res_low             10.8160
_refine_ls_goodness_of_fit_ref   1.1287
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     198
_refine_ls_number_reflns         2128
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.1282
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0501
_refine_ls_shift/su_max          -0.0007
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+0.7005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0804
_refine_ls_wR_factor_ref         0.1027
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -13
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1419
_reflns_number_total             2128
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj02078e2.cif
_cod_data_source_block           K
_cod_database_code               7061665
_olex2_refinement_description
;
1. Restrained distances
 O9-H9a
 0.87 with sigma of 0.02
 O9-H9b
 0.87 with sigma of 0.02
;
_olex2_submission_special_instructions 'No special instructions were received'