Strong intermolecular interaction induced methylene-bridged asymmetric heterocyclic explosives
Wang, Yu; Ye, Jin; Yang, Na; Ma, Haixia; Zhang, Yazhou; Guo, Zhaoqi; CrystEngComm 23 (2021) 7635–7642; doi:10.1039/D1CE01083B

data_7243554
_publ_section_title
;
 Strong intermolecular interaction induced methylene-bridged asymmetric
 heterocyclic explosives
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              7635
_journal_page_last               7642
_journal_paper_doi               10.1039/D1CE01083B
_journal_volume                  23
_journal_year                    2021
_chemical_formula_moiety         'C4 H2 K2 N10 O5'
_chemical_formula_sum            'C4 H2 K2 N10 O5'
_chemical_formula_weight         348.36
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2021-01-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-14 deposited with the CCDC.	2021-09-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1233(4)
_cell_length_b                   8.2762(3)
_cell_length_c                   11.5289(4)
_cell_measurement_reflns_used    5821
_cell_measurement_temperature    298.0
_cell_measurement_theta_max      27.122
_cell_measurement_theta_min      2.992
_cell_volume                     1142.27(7)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_diffrn_ambient_temperature      298.0
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_unetI/netI     0.0536
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            11250
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.144
_diffrn_reflns_theta_min         2.992
_exptl_absorpt_coefficient_mu    0.877
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4479
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0946 before and 0.0669 after correction. The Ratio of minimum to maximum transmission is 0.9127. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.026
_exptl_crystal_description       plate
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.7
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.600
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         2527
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      5.248
_refine_ls_R_factor_all          0.0566
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0560P)^2^+2.1583P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1196
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2162
_reflns_number_total             2527
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01083b2.cif
_cod_data_source_block           22019513kno2nh_0m
_cod_depositor_comments
'Adding full bibliography for 7243554--7243556.cif.'
_cod_database_code               7243554
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.917
_shelx_estimated_absorpt_t_min   0.579
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2. Restrained distances
 O3-N2
 2.9 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B)
;
_shelx_res_checksum              53766
_shelx_hkl_checksum              10898
_olex2_submission_special_instructions 'No special instructions were received'