Optimizing the oxygen balance by changing the A-site cations in molecular perovskite high-energetic materials
Chen, Shao-Li; Shang, Yu; He, Chun-Ting; Sun, Lin-Ying; Ye, Zi-Ming; Zhang, Wei-Xiong; Chen, Xiao-Ming; CrystEngComm 20 (2018) 7458–; doi:10.1039/C8CE01350K

data_7237079
_publ_section_title
;
 Optimizing the oxygen balance by changing the A-site cations in molecular
 perovskite high-energetic materials
;
_journal_issue                   46
_journal_name_full               CrystEngComm
_journal_page_first              7458
_journal_paper_doi               10.1039/C8CE01350K
_journal_volume                  20
_journal_year                    2018
_chemical_formula_moiety         '0.25(Cl12 K4 O48), 1(C6 H14 N2 O)'
_chemical_formula_sum            'C6 H14 Cl3 K N2 O13'
_chemical_formula_weight         467.64
_chemical_name_systematic        DAP-O12
_space_group_crystal_system      cubic
_space_group_IT_number           226
_space_group_name_Hall           '-F 4a 2 3'
_space_group_name_H-M_alt        'F m -3 c'
_atom_sites_solution_hydrogens   mixed
_audit_block_doi                 10.5517/ccdc.csd.cc20gf75
_audit_creation_date             2018-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-08 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   14.745(3)
_cell_length_b                   14.745(3)
_cell_length_c                   14.745(3)
_cell_measurement_reflns_used    650
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      27.375
_cell_measurement_theta_min      3.909
_cell_volume                     3205.8(11)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.910
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_Laue_measured_fraction_full 0.910
_diffrn_reflns_Laue_measured_fraction_max 0.917
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            650
_diffrn_reflns_point_group_measured_fraction_full 0.910
_diffrn_reflns_point_group_measured_fraction_max 0.917
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.375
_diffrn_reflns_theta_min         3.909
_exptl_absorpt_coefficient_mu    0.904
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.8
_exptl_crystal_colour            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.938
_exptl_crystal_description       block
_exptl_crystal_F_000             1904
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.233
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     38
_refine_ls_number_reflns         165
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0412
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0755P)^2^+3.0868P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1251
_reflns_Friedel_coverage         0.000
_reflns_number_gt                102
_reflns_number_total             165
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ce01350k2.cif
_cod_data_source_block           c
_cod_original_cell_volume        3206(2)
_cod_original_sg_symbol_Hall     '-F 4c 2 3'
_cod_database_code               7237079
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.915
_shelx_estimated_absorpt_t_min   0.915
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C3-C4 = C6-C5 = C1-C2
 1.52 with sigma of 0.02
 O2-N1
 1.37 with sigma of 0.02
 C2-C4 = C4-C6 = C6-C2 = C1-C3 = C3-C5 = C5-C1
 2.42 with sigma of 0.02
 O2-O1_$1
 2.45 with sigma of 0.01
 N2-C2 \\sim N2-C6 \\sim N2-C4 \\sim N1-C1 \\sim N1-C5 \\sim N1-C3
 with sigma of 0.01
 O2-C1 \\sim O2-C3 \\sim O2-C5
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uiso(O2) = Uiso(N1) = Uiso(N2) = Uiso(C1) = Uiso(C2) = Uiso(C3) = Uiso(C4) =
Uiso(C5) = Uiso(C6)
4. Others
 Fixed Sof: O2(0.04167) H2(0.04167) N1(0.04167) N2(0.04167) H2A(0.04167)
 C1(0.04167) H1A(0.04167) H1B(0.04167) C2(0.04167) H2B(0.04167) H2C(0.04167)
 C3(0.04167) H3A(0.04167) H3B(0.04167) C4(0.04167) H4A(0.04167) H4B(0.04167)
 C5(0.04167) H5A(0.04167) H5B(0.04167) C6(0.04167) H6A(0.04167) H6B(0.04167)
5.a Riding coordinates:
 N2(H2A), C1(H1A,H1B), C2(H2B,H2C), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B),
 C6(H6A,H6B)
5.b Tetrahedral OH refined with riding coordinates:
 O2(H2)
;
_shelx_res_checksum              67217
_olex2_submission_special_instructions 'No special instructions were received'