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_7061666
_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 N7 O8, H2 O, H4 N'
_chemical_formula_sum            'C4 H8 N8 O9'
_chemical_formula_weight         312.157
_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
_audit_creation_date             2022-06-06
_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                 100.161(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9418(19)
_cell_length_b                   15.988(3)
_cell_length_c                   6.7678(10)
_cell_measurement_reflns_used    2137
_cell_measurement_temperature    170
_cell_measurement_theta_max      25.688
_cell_measurement_theta_min      2.281
_cell_volume                     1165.4(3)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2016)'
_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-dev (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      170.00
_diffrn_measured_fraction_theta_full 0.9881
_diffrn_measured_fraction_theta_max 0.9853
_diffrn_measurement_device_type  'D8 VENTURE'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0733
_diffrn_reflns_av_unetI/netI     0.0616
_diffrn_reflns_Laue_measured_fraction_full 0.9881
_diffrn_reflns_Laue_measured_fraction_max 0.9853
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            11341
_diffrn_reflns_point_group_measured_fraction_full 0.9881
_diffrn_reflns_point_group_measured_fraction_max 0.9853
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         26.03
_diffrn_reflns_theta_min         2.28
_exptl_absorpt_coefficient_mu    0.172
_exptl_absorpt_correction_T_max  0.7453
_exptl_absorpt_correction_T_min  0.6758
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1127 before and 0.0677 after correction. The Ratio of minimum to maximum transmission is 0.9067. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             640.681
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.4097
_refine_diff_density_min         -0.5242
_refine_diff_density_rms         0.1191
_refine_ls_d_res_high            0.8096
_refine_ls_d_res_low             8.9324
_refine_ls_goodness_of_fit_ref   1.1145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     262
_refine_ls_number_reflns         2274
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.1120
_refine_ls_R_factor_all          0.0801
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          -0.0009
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0040P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0490
_refine_ls_wR_factor_ref         0.0604
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -13
_reflns_limit_k_max              19
_reflns_limit_k_min              0
_reflns_limit_l_max              8
_reflns_limit_l_min              0
_reflns_number_gt                1542
_reflns_number_total             2274
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d2nj02078e2.cif
_cod_data_source_block           2
_cod_database_code               7061666
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 N5, H5a, H5b
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
;
_olex2_submission_special_instructions 'No special instructions were received'