To improve the key properties of nonlinear optical crystals assembled with tetrahedral functional building units
Bai, Zhiyong; Liu, Lehui; Wang, Dongmei; Hu, Chun-Li; Lin, Zhoubin; Chemical Science 12 (2021) 4014–4020; doi:10.1039/D1SC00080B

data_1560198
_publ_section_title
;
 To improve the key properties of nonlinear optical crystals assembled
 with tetrahedral functional building units
;
_journal_issue                   11
_journal_name_full               'Chemical Science'
_journal_page_first              4014
_journal_page_last               4020
_journal_paper_doi               10.1039/D1SC00080B
_journal_volume                  12
_journal_year                    2021
_chemical_formula_moiety         'As B F O4, H4 N'
_chemical_formula_sum            'As B F H4 N O4'
_chemical_formula_weight         186.77
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-12-11 deposited with the CCDC.	2021-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.4453(6)
_cell_length_b                   8.1098(10)
_cell_length_c                   12.7463(18)
_cell_measurement_reflns_used    3282
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      60.2000
_cell_measurement_theta_min      6.0140
_cell_volume                     459.51(11)
_computing_cell_refinement       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.40.82a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_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 0.995
_diffrn_measured_fraction_theta_max 0.947
_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     50.00  89.00   0.50    0.08    --   70.78  77.00 120.00   78
  2  \w    115.00 142.00   0.50    0.08    --   70.78  77.00 120.00   54
  3  \w     47.00  96.00   0.50    0.08    --   70.78  77.00 -30.00   98
  4  \w     47.00 115.00   0.50    0.08    --   70.78  77.00 -90.00  136
  5  \w     47.00 119.00   0.50    0.08    --   70.78  77.00-120.00  144
  6  \w    104.00 130.00   0.50    0.08    --   70.78  77.00-150.00   52
  7  \w     96.00 140.00   0.50    0.08    --   70.78  77.00-180.00   88
  8  \w     47.00  88.00   0.50    0.08    --   70.78  77.00-180.00   82
  9  \w     49.00  82.00   0.50    0.08    --   70.78  77.00-150.00   66
 10  \w    109.00 134.00   0.50    0.08    --   70.78  77.00   0.00   50
 11  \w     92.00 134.00   0.50    0.08    --   70.78  77.00  30.00   84
 12  \w     99.00 142.00   0.50    0.08    --   70.78  77.00  60.00   86
 13  \w     47.00  84.00   0.50    0.08    --   70.78  77.00  30.00   74
 14  \w     47.00  81.00   0.50    0.08    --   70.78  77.00   0.00   68
 15  \w    107.00 143.00   0.50    0.08    --   70.78  77.00 -30.00   72
 16  \w     47.00  78.00   0.50    0.08    --   70.78  77.00  60.00   62
 17  \w     47.00  83.00   0.50    0.08    --   70.78  77.00  90.00   72
 18  \w     50.00  85.00   0.50    0.08    --   70.78  71.00 149.89   70
 19  \w     51.00 141.00   0.50    0.08    --   70.78  77.00 150.00  180
 20  \w     57.00  99.00   0.50    0.08    --   70.78  57.00 -30.00   84
 21  \w    107.00 134.00   0.50    0.08    --   70.78  57.00 -30.00   54
 22  \w    114.00 140.00   0.50    0.08    --   70.78  45.00 -94.00   52
 23  \w     60.00  86.00   0.50    0.08    --   70.78  45.00 -94.00   52
 24  \w      8.00  47.00   0.50    0.08    --   70.78 -45.00 115.00   78
 25  \w      0.00  52.00   0.50    0.08    --   70.78 -57.00  90.00  104
 26  \w     20.00 104.00   0.50    0.08    --   70.78-125.00 120.00  168
 27  \w     60.00 108.00   0.50    0.08    --   70.78-125.00 -90.00   96
 28  \w    -60.00  13.00   0.50    0.05    --   -2.81 -57.00-120.00  146
 29  \w    -75.00 -47.00   0.50    0.05    --   -2.81 -38.00  30.00   56
 30  \w    -42.00 -16.00   0.50    0.05    --   -2.81 -38.00  30.00   52
 31  \w    -65.00 -39.00   0.50    0.05    --   -2.81 -45.00 115.00   52
 32  \w   -126.00 -92.00   0.50    0.08    --  -76.40 -45.00 115.00   68
 33  \w    -54.00 -28.00   0.50    0.08    --  -76.40  77.00  60.00   52
 34  \w    -65.00 -14.00   0.50    0.08    --  -76.40  57.00  30.00  102
 35  \w    -98.00 -61.00   0.50    0.08    --  -76.40  77.00  60.00   74
 36  \w    -62.00  -5.00   0.50    0.08    --  -76.40  57.00 -30.00  114
 37  \w      1.00  68.00   0.50    0.05    --   -2.81  57.00-180.00  134
 38  \w    -13.00  20.00   0.50    0.05    --   -2.81  45.00 -94.00   66
 39  \w    -60.00  -4.00   0.50    0.08    --  -76.40  57.00-180.00  112
 40  \w    -51.00 -26.00   0.50    0.08    --  -76.40  45.00 -94.00   50
 41  \w    -65.00 -10.00   0.50    0.08    --  -76.40  77.00 -90.00  110
 42  \w   -100.00 -70.00   0.50    0.08    --  -76.40  77.00 -90.00   60
;
_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      0.2240153500
_diffrn_orient_matrix_UB_12      -0.0645733500
_diffrn_orient_matrix_UB_13      -0.0570273000
_diffrn_orient_matrix_UB_21      -0.1571599000
_diffrn_orient_matrix_UB_22      -0.1400144000
_diffrn_orient_matrix_UB_23      -0.0106531000
_diffrn_orient_matrix_UB_31      -0.1257433500
_diffrn_orient_matrix_UB_32      0.0592054500
_diffrn_orient_matrix_UB_33      -0.0875682000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.1387
_diffrn_reflns_av_unetI/netI     0.0682
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3649
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.898
_diffrn_reflns_theta_full        53.543
_diffrn_reflns_theta_max         62.219
_diffrn_reflns_theta_min         6.037
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    6.663
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45369
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.82a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    2.700
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.757
_refine_diff_density_min         -1.328
_refine_diff_density_rms         0.352
_refine_ls_abs_structure_details
;
 Flack x determined using 410 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.05(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.154
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     73
_refine_ls_number_reflns         981
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.153
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1099P)^2^+6.7729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1764
_reflns_Friedel_coverage         0.887
_reflns_Friedel_fraction_full    0.950
_reflns_Friedel_fraction_max     0.847
_reflns_number_gt                950
_reflns_number_total             981
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1sc00080b2.cif
_cod_data_source_block           abaf6-2
_cod_depositor_comments          'Adding full bibliography for 1560198.cif.'
_cod_original_cell_volume        459.51(10)
_cod_database_code               1560198
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'As B O F N'
_shelx_estimated_absorpt_t_max   0.585
_shelx_estimated_absorpt_t_min   0.478
_diffrn_oxdiff_digest_frames
;
01472c31066842c4bd022521fb0bc9d60703552600d
;
_diffrn_oxdiff_digest_hkl
;
01e1f19722a719c64ddb075bd860959445f1d3
;
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     56.82
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H,H,H) groups
2.a Riding coordinates:
 N1(H1A), N1(H1B,H1C,H1D)
;
_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 4.723
_oxdiff_exptl_absorpt_empirical_full_min 0.266