Two UV Optical Crystals with Strong Optical Anisotropy, Large Band Gaps and α-BBO Type Structure
Liu, Lehui; Zhang, Lizhen; yuan, feifei; Huang, Yisheng; Lin, Zhoubin; Dalton Transactions  (2023) –; doi:10.1039/D3DT00581J

data_7712708
_publ_section_title
;
 Two UV Optical Crystals with Strong Optical Anisotropy, Large Band Gaps
 and \a-BBO Type Structure
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D3DT00581J
_journal_year                    2023
_chemical_formula_moiety         '4(C3 H6 N6), F6 P1, 1(H)'
_chemical_formula_sum            'C12 H25 F6 N24 P'
_chemical_formula_weight         650.53
_space_group_crystal_system      trigonal
_space_group_IT_number           167
_space_group_name_Hall           '-R 3 2"c'
_space_group_name_H-M_alt        'R -3 c :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2022-12-01
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2023-02-09 deposited with the CCDC.	2023-03-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   10.8117(8)
_cell_length_b                   10.8117(8)
_cell_length_c                   37.472(4)
_cell_measurement_reflns_used    1989
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      59.4850
_cell_measurement_theta_min      4.5860
_cell_volume                     3793.4(6)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_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      0.00  55.00   0.50    0.82    --   73.66 -38.00-180.00  110
  2  \w     79.00 132.00   0.50    0.82    --   73.66 125.00-150.00  106
  3  \w    113.00 149.00   0.50    0.82    --   73.66  17.00 167.00   72
  4  \w     24.00  50.00   0.50    0.21    --   -0.62  38.00-120.00   52
  5  \w   -147.00 -88.00   0.50    0.82    --  -74.91 -99.00-180.00  118
  6  \w   -139.00 -77.00   0.50    0.82    --  -74.91-166.00  24.00  124
  7  \w   -120.00 -90.00   0.50    0.82    --  -74.91 -97.00  67.00   60
  8  \w    -12.00  33.00   0.50    0.21    --   -0.62 -97.00  67.00   90
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'ROD, Synergy Custom system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0716136000
_diffrn_orient_matrix_UB_12      -0.0762993000
_diffrn_orient_matrix_UB_13      0.0286270000
_diffrn_orient_matrix_UB_21      0.1136387000
_diffrn_orient_matrix_UB_22      0.0807865000
_diffrn_orient_matrix_UB_23      0.0205994000
_diffrn_orient_matrix_UB_31      -0.0490293000
_diffrn_orient_matrix_UB_32      0.0901146000
_diffrn_orient_matrix_UB_33      0.0057720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Ga K\a'
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0377
_diffrn_reflns_av_unetI/netI     0.0343
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            4249
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         60.579
_diffrn_reflns_theta_min         4.590
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    1.229
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62855
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             2004
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.354
_refine_diff_density_min         -0.344
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0589
_refine_ls_R_factor_gt           0.0491
_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^)+(0.1007P)^2^+1.5594P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1366
_refine_ls_wR_factor_ref         0.1464
_reflns_Friedel_coverage         0.000
_reflns_number_gt                755
_reflns_number_total             955
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00581j2.cif
_cod_data_source_block           x
_cod_original_cell_volume        3793.4(7)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               7712708
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C N O P F'
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.791
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
2. Others
 Fixed Sof: F1(0.33333) F2(0.33333) F3(0.33333) H(0.16667)
;
_shelx_res_checksum              19860
_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
;
_oxdiff_exptl_absorpt_empirical_full_max 4.470
_oxdiff_exptl_absorpt_empirical_full_min 0.325