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_7237082
_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         'Cl3 Na O12, C4 H12 N2'
_chemical_formula_sum            'C4 H12 Cl3 N2 Na O12'
_chemical_formula_weight         409.49
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-20
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-10-10 deposited with the CCDC.
2018-10-19 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.993(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1689(4)
_cell_length_b                   9.7312(4)
_cell_length_c                   13.2985(6)
_cell_measurement_reflns_used    6969
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      77.0990
_cell_measurement_theta_min      4.3390
_cell_volume                     1315.16(10)
_computing_cell_refinement       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.40t (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9742
_diffrn_measured_fraction_theta_max 0.9742
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -69.00  58.00   1.00   30.00    --  -32.00   0.00-180.00  127
  2  \w    -47.00  14.00   1.00   30.00    --  -32.00  72.00  36.00   61
  3  \w    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00-180.00   60
  4  \w    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00 108.00   60
  5  \w    -79.00  17.00   1.00   30.00    --  -32.00   0.00 108.00   96
  6  \w    -47.00  15.00   1.00   30.00    --  -32.00  72.00 108.00   62
  7  \w    -78.00 -18.00   1.00   30.00    --  -32.00 -72.00  36.00   60
  8  \w   -200.00 -20.00   1.00   80.00    -- -110.00   0.00-180.00  180
  9  \w   -125.00 -34.00   1.00   80.00    -- -110.00  72.00 108.00   91
 10  \w   -114.00 -35.00   1.00   80.00    -- -110.00  72.00-180.00   79
 11  \w   -104.00 -23.00   1.00   80.00    -- -110.00  72.00 -36.00   81
 12  \w   -200.00 -38.00   1.00   80.00    -- -110.00   0.00-108.00  162
 13  \w   -200.00-105.00   1.00   80.00    -- -110.00 -72.00 -36.00   95
 14  \w    -89.00 -23.00   1.00   80.00    -- -110.00  72.00  36.00   66
 15  \w   -125.00 -64.00   1.00   80.00    -- -110.00  72.00-108.00   61
 16  \w   -169.00-109.00   1.00   80.00    -- -110.00 -72.00-180.00   60
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1357929000
_diffrn_orient_matrix_UB_12      -0.0583044000
_diffrn_orient_matrix_UB_13      -0.0251896000
_diffrn_orient_matrix_UB_21      -0.0618640000
_diffrn_orient_matrix_UB_22      -0.1428638000
_diffrn_orient_matrix_UB_23      -0.0172088000
_diffrn_orient_matrix_UB_31      -0.0265235000
_diffrn_orient_matrix_UB_32      0.0351022000
_diffrn_orient_matrix_UB_33      -0.1119021000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.1187
_diffrn_reflns_av_unetI/netI     0.0657
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11329
_diffrn_reflns_theta_full        77.3376
_diffrn_reflns_theta_max         77.34
_diffrn_reflns_theta_min         4.35
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    7.367
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.22594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.40t (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.0679
_exptl_crystal_description       block
_exptl_crystal_F_000             840.0138
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.2025
_refine_diff_density_min         -0.6800
_refine_diff_density_rms         0.2511
_refine_ls_d_res_high            0.7901
_refine_ls_d_res_low             10.1627
_refine_ls_goodness_of_fit_ref   1.0292
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    18
_refine_ls_number_parameters     199
_refine_ls_number_reflns         2722
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0292
_refine_ls_R_factor_all          0.0788
_refine_ls_R_factor_gt           0.0731
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1743P)^2^+0.0644P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2007
_refine_ls_wR_factor_ref         0.2103
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              12
_reflns_limit_h_min              -12
_reflns_limit_k_max              12
_reflns_limit_k_min              0
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                2379
_reflns_number_total             2722
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c8ce01350k2.cif
_cod_data_source_block           CSL_Cu
_cod_original_cell_volume        1315.17(9)
_cod_database_code               7237082
_reflns_odcompleteness_completeness 97.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     77.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 N00F(H00a,H00b), N00G(H00c,H00d), C00J(H00e,H00f), C00K(H00g,H00h), C00L(H00i,
 H00j), C00M(H00k,H00l)
;
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.769
_oxdiff_exptl_absorpt_empirical_full_min 0.212