Preparation, crystal structure and solution-mediated phase transformation of a novel solid-state form of CL-20
Pan, Bochen; Dang, Leping; Wang, Zhanzhong; Jiang, Jun; Wei, Hongyuan; CrystEngComm 20 (2018) 1553–; doi:10.1039/C7CE02026K

data_7230122
_publ_section_title
;
 Preparation, crystal structure and solution-mediated phase transformation
 of a novel solid-state form of CL-20
;
_journal_issue                   11
_journal_name_full               CrystEngComm
_journal_page_first              1553
_journal_paper_doi               10.1039/C7CE02026K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C8 H9 N13 O12'
_chemical_formula_weight         479.28
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2018-01-17 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 130.51(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.746(6)
_cell_length_b                   7.8121(16)
_cell_length_c                   19.757(4)
_cell_measurement_reflns_used    11125
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.555
_cell_measurement_theta_min      3.205
_cell_volume                     3491(2)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'rigaku r-axis rapid IP'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0405
_diffrn_reflns_av_sigmaI/netI    0.0371
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13800
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         3.32
_exptl_absorpt_coefficient_mu    0.170
_exptl_absorpt_correction_T_max  0.9749
_exptl_absorpt_correction_T_min  0.9587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.824
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.242
_refine_diff_density_min         -0.207
_refine_diff_density_rms         0.045
_refine_ls_extinction_coef       0.0087(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     311
_refine_ls_number_reflns         3240
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0479
_refine_ls_R_factor_gt           0.0392
_refine_ls_shift/su_max          0.094
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1350
_reflns_number_gt                2714
_reflns_number_total             3240
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c7ce02026k2.cif
_cod_data_source_block           b
_cod_depositor_comments          'Adding full bibliography for 7230122.cif.'
_cod_original_cell_volume        3490.6(12)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7230122