Hybrid organic-inorganic triguanidine arsenate dihydrate for ultraviolet nonlinear optical application
Wang, Dongmei; Wei, Zhuangzhuang; Bai, Zhiyong; Liu, Lehui; Lin, Zhoubin; Zhang, Lizhen; Dalton Transactions  (2021) –; doi:10.1039/D1DT03323A

data_7709104
_publ_section_title
;
 Hybrid organic-inorganic triguanidine arsenate dihydrate for ultraviolet
 nonlinear optical application
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT03323A
_journal_year                    2021
_chemical_formula_moiety         'As O4, 3(C H6 N3), 2(H2 O)'
_chemical_formula_sum            'C3 H22 As N9 O6'
_chemical_formula_weight         355.21
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-01 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.506(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.5850(3)
_cell_length_b                   17.7646(7)
_cell_length_c                   12.3972(5)
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    235(30)
_cell_measurement_theta_max      51.8270
_cell_measurement_theta_min      4.3210
_cell_volume                     1403.99(10)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      235(30)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_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     32.00  68.00   0.50    0.07    --   55.97  77.00   0.00   72
  2  \w     32.00  68.00   0.50    0.07    --   55.97  77.00 -60.00   72
  3  \w     33.00  84.00   0.50    0.07    --   55.97  77.00-120.00  102
  4  \w     32.00 120.00   0.50    0.07    --   55.97  77.00-150.00  176
  5  \w     93.00 127.00   0.50    0.07    --   55.97  77.00 -90.00   68
  6  \w     87.00 128.00   0.50    0.07    --   55.97  77.00 -60.00   82
  7  \w     32.00  79.00   0.50    0.07    --   55.97  77.00 -90.00   94
  8  \w     71.00 109.00   0.50    0.07    --   55.97  77.00   0.00   76
  9  \w     32.00 124.00   0.50    0.07    --   55.97  77.00  60.00  184
 10  \w     33.00 112.00   0.50    0.07    --   55.97  77.00 138.59  158
 11  \w     32.00  70.00   0.50    0.07    --   55.97  77.00 120.00   76
 12  \w     33.00 117.00   0.50    0.07    --   55.97  77.00  30.00  168
 13  \w     87.00 128.00   0.50    0.07    --   55.97  77.00 120.00   82
 14  \w     32.00  69.00   0.50    0.07    --   55.97  77.00 -30.00   74
 15  \w     92.00 129.00   0.50    0.07    --   55.97  77.00-120.00   74
 16  \w     32.00  97.00   0.50    0.07    --   55.97  77.00-180.00  130
 17  \w    -69.00  -9.00   0.50    0.07    --  -57.22  38.00 -30.00  120
 18  \w    -73.00  -3.00   0.50    0.07    --  -57.22  57.00   0.00  140
 19  \w   -108.00 -64.00   0.50    0.07    --  -57.22 131.00 -33.00   88
 20  \w   -111.00 -41.00   0.50    0.07    --  -57.22 138.00 142.00  140
 21  \w    -76.00  10.00   0.50    0.07    --  -57.22  77.00 150.00  172
 22  \w     71.00 129.00   0.50    0.07    --   55.97 138.00 142.00  116
 23  \w     84.00 110.00   0.50    0.07    --   55.97 131.00 -33.00   52
 24  \w    -12.00  42.00   0.50    0.07    --   55.97 -77.00  90.00  108
 25  \w     50.00  80.00   0.50    0.07    --   55.97 -77.00  90.00   60
 26  \w     65.00 106.00   0.50    0.07    --   55.97-138.00  80.00   82
 27  \w     56.00  91.00   0.50    0.07    --   55.97-131.00-103.00   70
 28  \w    -38.00  17.00   0.50    0.05    --   -0.62 -77.00-180.00  110
 29  \w    -24.00  10.00   0.50    0.05    --   -0.62 -57.00 -60.00   68
 30  \w    -69.00 -27.00   0.50    0.05    --   -0.62 -57.00 -60.00   84
 31  \w   -119.00 -80.00   0.50    0.07    --  -57.22-131.00-103.00   78
 32  \w   -124.00 -99.00   0.50    0.07    --  -57.22-138.00  80.00   50
 33  \w   -128.00 -86.00   0.50    0.07    --  -57.22-125.00  90.00   84
 34  \w   -119.00 -81.00   0.50    0.07    --  -57.22-125.00 150.00   76
;
_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      -0.0816539000
_diffrn_orient_matrix_UB_12      -0.0273443000
_diffrn_orient_matrix_UB_13      -0.1023476000
_diffrn_orient_matrix_UB_21      -0.0373989000
_diffrn_orient_matrix_UB_22      0.0702132000
_diffrn_orient_matrix_UB_23      -0.0392289000
_diffrn_orient_matrix_UB_31      0.1898705000
_diffrn_orient_matrix_UB_32      0.0020713000
_diffrn_orient_matrix_UB_33      -0.0209124000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11259
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        51.803
_diffrn_reflns_theta_max         51.803
_diffrn_reflns_theta_min         4.328
_diffrn_source                   'micro-focus metaljet'
_exptl_absorpt_coefficient_mu    2.497
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45641
_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            'clear whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.680
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.149
_refine_diff_density_min         -0.175
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 1094 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.003(13)
_refine_ls_extinction_coef       0.00169(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2341
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0183
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0267P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0431
_refine_ls_wR_factor_ref         0.0433
_reflns_Friedel_coverage         0.962
_reflns_Friedel_fraction_full    0.969
_reflns_Friedel_fraction_max     0.969
_reflns_number_gt                2300
_reflns_number_total             2341
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt03323a2.cif
_cod_data_source_block           exp_10657_auto
_cod_original_cell_volume        1403.99(11)
_cod_database_code               7709104
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'As C N O'
_shelx_estimated_absorpt_t_max   0.788
_shelx_estimated_absorpt_t_min   0.788
_diffrn_oxdiff_digest_frames
;
01871806e5487943d0de90c679e60902f1033867a40
;
_diffrn_oxdiff_digest_hkl
;
01bf52df22d35d88a63507c53a3e5805863efc
;
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All N(H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5C = O5-H5D
 0.86 with sigma of 0.02
 O6-H6C
 0.86 with sigma of 0.02
 H5C-H5D
 1.36 with sigma of 0.04
3.a Rotating group:
 N6(H6A,H6B)
3.b X=CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N7(H7A,H7B),
 N8(H8A,H8B), N9(H9A,H9B)
;
_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 4.912
_oxdiff_exptl_absorpt_empirical_full_min 0.544