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_7712709
_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         'C3 H7 N6, 2(C3 H6 N6), F6 P, H2 O'
_chemical_formula_sum            'C9 H21 F6 N18 O P'
_chemical_formula_weight         542.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2022-10-24
_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                 103.770(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.9123(3)
_cell_length_b                   10.9021(2)
_cell_length_c                   15.2051(4)
_cell_measurement_reflns_used    6623
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      75.0720
_cell_measurement_theta_min      5.1230
_cell_volume                     2078.92(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_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 2018/2 (Sheldrick, 2018)'
_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 0.997
_diffrn_measured_fraction_theta_max 0.956
_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   -116.00 -43.00   0.50    1.27    --  -46.63 -31.00   5.00  146
  2  \w    -25.00  25.00   0.50    1.27    --  -46.63  31.00 165.00  100
  3  \w     50.00 111.00   0.50    1.27    --   49.76  31.00 165.00  122
  4  \w    -16.00   9.00   0.50    1.27    --   49.76 -31.00   5.00   50
  5  \w   -175.00 -90.00   0.50    5.07    -- -105.55 -31.00   5.00  170
  6  \w     93.00 121.00   0.50    5.07    --  108.68  31.00 165.00   56
  7  \w    -14.00  29.00   0.50    1.27    --  -46.63  19.00 -60.00   86
  8  \w    -23.00  42.00   0.50    1.27    --   49.76 -38.00-150.00  130
  9  \w    -65.00 -33.00   0.50    5.07    -- -105.55 125.00-150.00   64
 10  \w    -67.00 -33.00   0.50    5.07    -- -105.55  61.00 150.00   68
 11  \w    -69.00 -44.00   0.50    5.07    -- -105.55  61.00   0.00   50
 12  \w    -70.00 -33.00   0.50    5.07    -- -105.55  61.00  30.00   74
 13  \w    -65.00 -34.00   0.50    5.07    -- -105.55  61.00 -60.00   62
 14  \w    -62.00 -36.00   0.50    5.07    -- -105.55  61.00 -30.00   52
 15  \w   -110.00 -81.00   0.50    5.07    -- -105.55 125.00-150.00   58
 16  \w    -63.00 -37.00   0.50    5.07    -- -105.55  61.00-120.00   52
 17  \w     40.00  65.00   0.50    5.07    --  108.68 -61.00 120.00   50
 18  \w     36.00  67.00   0.50    5.07    --  108.68 -61.00   0.00   62
 19  \w     64.00 105.00   0.50    5.07    --  108.68 -77.00  60.00   82
 20  \w     49.00  93.00   0.50    5.07    --  108.68 -77.00  30.00   88
 21  \w     36.00  85.00   0.50    5.07    --  108.68 -95.00-120.00   98
 22  \w     36.00  61.00   0.50    5.07    --  108.68 -61.00  90.00   50
 23  \w     36.00  61.00   0.50    5.07    --  108.68 -61.00 -90.00   50
 24  \w     44.00  74.00   0.50    5.07    --  108.68 -95.00  30.00   60
 25  \w     46.00 105.00   0.50    5.07    --  108.68 -77.00 -90.00  118
 26  \w     37.00  68.00   0.50    5.07    --  108.68 -61.00 150.00   62
 27  \w     37.00  67.00   0.50    5.07    --  108.68 -61.00  60.00   60
 28  \w     36.00  71.00   0.50    5.07    --  108.68 -61.00  30.00   70
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1208990000
_diffrn_orient_matrix_UB_12      0.0040353000
_diffrn_orient_matrix_UB_13      -0.0422133000
_diffrn_orient_matrix_UB_21      0.0211524000
_diffrn_orient_matrix_UB_22      0.0567497000
_diffrn_orient_matrix_UB_23      -0.0868065000
_diffrn_orient_matrix_UB_31      0.0055291000
_diffrn_orient_matrix_UB_32      -0.1294040000
_diffrn_orient_matrix_UB_33      -0.0394160000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0918
_diffrn_reflns_av_unetI/netI     0.0998
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14828
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.167
_diffrn_reflns_theta_min         2.992
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.137
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44009
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
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    1.733
_exptl_crystal_description       block
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.878
_refine_diff_density_min         -1.081
_refine_diff_density_rms         0.205
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         4266
_refine_ls_number_restraints     108
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1453
_refine_ls_R_factor_gt           0.0978
_refine_ls_shift/su_max          0.760
_refine_ls_shift/su_mean         0.020
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1833P)^2^+3.6393P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2683
_refine_ls_wR_factor_ref         0.2898
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3389
_reflns_number_total             4266
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00581j2.cif
_cod_data_source_block           x_CCDC1
_cod_database_code               7712709
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.674
_shelx_estimated_absorpt_t_min   0.482
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.9992(4)
 0.0008(4)
2. Fixed Uiso
 At 1.2 times of:
  All N(H) groups, All N(H,H) groups
3. Restrained distances
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.02
 F1-F2 \\sim F3-F4 \\sim F5-F6
 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
F1 \\sim F3 \\sim F2 \\sim F4 \\sim F5 \\sim F6: within 3.8A with sigma of 0.06
and sigma for terminal atoms of 0.12 within 3.8A
5.a Free rotating group:
 O2(H2C,H2D)
5.b Aromatic/amide H refined with riding coordinates:
 N16(H16)
5.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B), N3(H3A,H3B), N5(H5A,H5B), N7(H7A,H7B), N9(H9A,H9B), N11(H11A,
 H11B), N13(H13A,H13B), N15(H15A,H15B), N17(H17A,H17B)
;
_shelx_res_checksum              77368
_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 1.783
_oxdiff_exptl_absorpt_empirical_full_min 0.597