Putting the squeeze on energetic materials—structural characterisation of a high-pressure phase of CL-20
Millar, David I. A.; Maynard-Casely, Helen E.; Kleppe, Annette K.; Marshall, William G.; Pulham, Colin R.; Cumming, Adam S.; CrystEngComm 12 (2010) 2524–; doi:10.1039/c002701d

data_7212612
_publ_section_title
;
 Putting the squeeze on energetic materials---structural characterisation
 of a high-pressure phase of CL-20
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              2524
_journal_paper_doi               10.1039/c002701d
_journal_volume                  12
_journal_year                    2010
_chemical_formula_moiety         'C6 H6 N12 O12'
_chemical_formula_sum            'C6 H6 N12 O12'
_chemical_formula_weight         438.19
_chemical_name_common            'Zeta CL-20 at 3.3 GPa'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 111.218(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.579(2)
_cell_length_b                   7.7219(19)
_cell_length_c                   14.1260(15)
_cell_measurement_reflns_used    676
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.250
_cell_measurement_theta_min      3.094
_cell_volume                     1279.1(4)
_computing_cell_refinement       'Apex2 (Bruker AXS, 2006)'
_computing_data_collection       'Apex2 (Bruker AXS, 2006)'
_computing_data_reduction        'Apex2 (Bruker AXS, 2006)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.636
_diffrn_measured_fraction_theta_max 0.503
_diffrn_measurement_device       'Bruker Kappa Apex2'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.128
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5107
_diffrn_reflns_theta_full        17.508
_diffrn_reflns_theta_max         23.345
_diffrn_reflns_theta_min         3.094
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.218
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.99
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.275
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.54
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1244
_refine_ls_hydrogen_treatment    none
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         515
_refine_ls_number_restraints     18
_refine_ls_R_factor_all          0.1673
_refine_ls_R_factor_gt           0.0877
_refine_ls_shift/su_max          0.0000906
_refine_ls_shift/su_mean         2.5068915
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ are:
1.17 0.787 0.789
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1665
_refine_ls_wR_factor_gt          0.0885
_refine_ls_wR_factor_ref         0.0885
_reflns_limit_h_max              10
_reflns_limit_h_min              -13
_reflns_limit_k_max              5
_reflns_limit_k_min              0
_reflns_limit_l_max              15
_reflns_limit_l_min              0
_reflns_number_gt                515
_reflns_number_total             935
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.07
_oxford_diffrn_Wilson_scale      53.98
_oxford_refine_ls_r_factor_ref   0.0877
_oxford_refine_ls_scale          0.1689(17)
_oxford_reflns_number_all        929
_oxford_reflns_threshold_expression_ref I>2.0\s(I)
_cod_data_source_file            c002701d.txt
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7212612