#------------------------------------------------------------------------------
#$Date: 2021-12-16 02:03:26 +0200 (Thu, 16 Dec 2021) $
#$Revision: 271456 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/91/7709104.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7709104
loop_
_publ_author_name
'Wang, Dongmei'
'Wei, Zhuangzhuang'
'Bai, Zhiyong'
'Liu, Lehui'
'Lin, Zhoubin'
'Zhang, Lizhen'
_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     32.00  68.00   0.50    0.07    --   55.97  77.00   0.00   72
  2  ω     32.00  68.00   0.50    0.07    --   55.97  77.00 -60.00   72
  3  ω     33.00  84.00   0.50    0.07    --   55.97  77.00-120.00  102
  4  ω     32.00 120.00   0.50    0.07    --   55.97  77.00-150.00  176
  5  ω     93.00 127.00   0.50    0.07    --   55.97  77.00 -90.00   68
  6  ω     87.00 128.00   0.50    0.07    --   55.97  77.00 -60.00   82
  7  ω     32.00  79.00   0.50    0.07    --   55.97  77.00 -90.00   94
  8  ω     71.00 109.00   0.50    0.07    --   55.97  77.00   0.00   76
  9  ω     32.00 124.00   0.50    0.07    --   55.97  77.00  60.00  184
 10  ω     33.00 112.00   0.50    0.07    --   55.97  77.00 138.59  158
 11  ω     32.00  70.00   0.50    0.07    --   55.97  77.00 120.00   76
 12  ω     33.00 117.00   0.50    0.07    --   55.97  77.00  30.00  168
 13  ω     87.00 128.00   0.50    0.07    --   55.97  77.00 120.00   82
 14  ω     32.00  69.00   0.50    0.07    --   55.97  77.00 -30.00   74
 15  ω     92.00 129.00   0.50    0.07    --   55.97  77.00-120.00   74
 16  ω     32.00  97.00   0.50    0.07    --   55.97  77.00-180.00  130
 17  ω    -69.00  -9.00   0.50    0.07    --  -57.22  38.00 -30.00  120
 18  ω    -73.00  -3.00   0.50    0.07    --  -57.22  57.00   0.00  140
 19  ω   -108.00 -64.00   0.50    0.07    --  -57.22 131.00 -33.00   88
 20  ω   -111.00 -41.00   0.50    0.07    --  -57.22 138.00 142.00  140
 21  ω    -76.00  10.00   0.50    0.07    --  -57.22  77.00 150.00  172
 22  ω     71.00 129.00   0.50    0.07    --   55.97 138.00 142.00  116
 23  ω     84.00 110.00   0.50    0.07    --   55.97 131.00 -33.00   52
 24  ω    -12.00  42.00   0.50    0.07    --   55.97 -77.00  90.00  108
 25  ω     50.00  80.00   0.50    0.07    --   55.97 -77.00  90.00   60
 26  ω     65.00 106.00   0.50    0.07    --   55.97-138.00  80.00   82
 27  ω     56.00  91.00   0.50    0.07    --   55.97-131.00-103.00   70
 28  ω    -38.00  17.00   0.50    0.05    --   -0.62 -77.00-180.00  110
 29  ω    -24.00  10.00   0.50    0.05    --   -0.62 -57.00 -60.00   68
 30  ω    -69.00 -27.00   0.50    0.05    --   -0.62 -57.00 -60.00   84
 31  ω   -119.00 -80.00   0.50    0.07    --  -57.22-131.00-103.00   78
 32  ω   -124.00 -99.00   0.50    0.07    --  -57.22-138.00  80.00   50
 33  ω   -128.00 -86.00   0.50    0.07    --  -57.22-125.00  90.00   84
 34  ω   -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       'ω 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+0.001xFc²λ³/sin(2θ)]^-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/[σ²(Fo²)+(0.0267P)²] where P=(Fo²+2Fc²)/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 > 2σ(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_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_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
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y, z+1/2'
'x+1/2, y+1/2, z'
'x+1/2, -y+1/2, z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
As1 As 0.52278(2) 0.64818(2) 0.56158(2) 0.01830(13) Uani 1 1 d . . . . .
N1 N 0.6441(5) 0.36601(18) 0.7738(3) 0.0313(8) Uani 1 1 d . . . . .
H1A H 0.609710 0.324598 0.736151 0.038 Uiso 1 1 calc R . . . .
H1B H 0.706005 0.364067 0.844481 0.038 Uiso 1 1 calc R . . . .
N2 N 1.1609(5) 0.43243(16) 0.7872(2) 0.0297(7) Uani 1 1 d . . . . .
H2A H 1.136799 0.475485 0.752920 0.036 Uiso 1 1 calc R . . . .
H2B H 1.222085 0.431029 0.858038 0.036 Uiso 1 1 calc R . . . .
N3 N 1.1413(5) 0.30399(17) 0.7859(3) 0.0320(8) Uani 1 1 d . . . . .
H3A H 1.104287 0.261838 0.750720 0.038 Uiso 1 1 calc R . . . .
H3B H 1.202673 0.303604 0.856724 0.038 Uiso 1 1 calc R . . . .
O1 O 0.3973(3) 0.72871(12) 0.51309(18) 0.0263(5) Uani 1 1 d . . . . .
C1 C 1.1492(5) 0.35054(17) 0.3077(3) 0.0229(7) Uani 1 1 d . . . . .
O2 O 0.7459(4) 0.64106(12) 0.5188(2) 0.0281(6) Uani 1 1 d . . . . .
N4 N 0.6554(5) 0.49516(17) 0.7808(2) 0.0332(7) Uani 1 1 d . . . . .
H4A H 0.628465 0.538564 0.747789 0.040 Uiso 1 1 calc R . . . .
H4B H 0.717296 0.493080 0.851477 0.040 Uiso 1 1 calc R . . . .
N5 N 0.9917(5) 0.32779(19) 0.3454(3) 0.0329(7) Uani 1 1 d . . . . .
H5A H 1.014495 0.302749 0.407586 0.040 Uiso 1 1 calc R . . . .
H5B H 0.863817 0.337636 0.308345 0.040 Uiso 1 1 calc R . . . .
O3 O 0.3640(4) 0.57465(13) 0.51850(19) 0.0302(5) Uani 1 1 d . . . . .
N6 N 1.1103(5) 0.39257(15) 0.2144(2) 0.0266(6) Uani 1 1 d . . . . .
H6A H 1.213865 0.388021 0.181341 0.032 Uiso 1 1 d GR . . . .
H6B H 0.993118 0.378792 0.166232 0.032 Uiso 1 1 d GR . . . .
N7 N 1.0119(5) 0.36954(16) 0.6247(2) 0.0298(7) Uani 1 1 d . . . . .
H7A H 0.986658 0.412122 0.589191 0.036 Uiso 1 1 calc R . . . .
H7B H 0.975746 0.327395 0.589355 0.036 Uiso 1 1 calc R . . . .
C2 C 1.1043(5) 0.36889(19) 0.7314(3) 0.0241(7) Uani 1 1 d . . . . .
C3 C 0.6021(5) 0.43215(19) 0.7232(3) 0.0253(7) Uani 1 1 d . . . . .
O4 O 0.5890(4) 0.64810(11) 0.70246(19) 0.0267(6) Uani 1 1 d . . . . .
O5 O 0.5182(6) 0.26174(12) 0.5673(4) 0.0334(5) Uani 1 1 d D . . . .
H5C H 0.434(6) 0.225(2) 0.555(4) 0.050 Uiso 1 1 d DR . . . .
H5D H 0.632(5) 0.244(2) 0.557(4) 0.050 Uiso 1 1 d DR . . . .
O6 O 0.9578(5) 0.48717(15) 0.0039(2) 0.0345(6) Uani 1 1 d D . . . .
H6C H 0.888(7) 0.448(2) 0.018(4) 0.052 Uiso 1 1 d DR . . . .
N8 N 1.3470(6) 0.33749(18) 0.3598(3) 0.0373(9) Uani 1 1 d . . . . .
H8A H 1.376989 0.312657 0.422253 0.045 Uiso 1 1 calc R . . . .
H8B H 1.447285 0.353736 0.331592 0.045 Uiso 1 1 calc R . . . .
N9 N 0.5084(5) 0.43537(17) 0.6162(2) 0.0323(7) Uani 1 1 d . . . . .
H9A H 0.473843 0.394060 0.578336 0.039 Uiso 1 1 calc R . . . .
H9B H 0.481149 0.478798 0.583312 0.039 Uiso 1 1 calc R . . . .
H6D H 1.072(7) 0.466(2) 0.000(4) 0.048(14) Uiso 1 1 d . . . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0150 0.0070 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -1.3050 0.8170 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0250 0.0140 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0410 0.0250 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 As1 O2 109.81(11) . . ?
O1 As1 O4 110.22(10) . . ?
O2 As1 O4 107.77(12) . . ?
O3 As1 O1 109.70(12) . . ?
O3 As1 O2 111.38(11) . . ?
O3 As1 O4 107.92(11) . . ?
H1A N1 H1B 120.0 . . ?
C3 N1 H1A 120.0 . . ?
C3 N1 H1B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
C2 N2 H2A 120.0 . . ?
C2 N2 H2B 120.0 . . ?
H3A N3 H3B 120.0 . . ?
C2 N3 H3A 120.0 . . ?
C2 N3 H3B 120.0 . . ?
N5 C1 N6 118.9(3) . . ?
N5 C1 N8 123.1(3) . . ?
N8 C1 N6 118.0(3) . . ?
H4A N4 H4B 120.0 . . ?
C3 N4 H4A 120.0 . . ?
C3 N4 H4B 120.0 . . ?
C1 N5 H5A 120.0 . . ?
C1 N5 H5B 120.0 . . ?
H5A N5 H5B 120.0 . . ?
C1 N6 H6A 110.2 . . ?
C1 N6 H6B 111.9 . . ?
H6A N6 H6B 107.8 . . ?
H7A N7 H7B 120.0 . . ?
C2 N7 H7A 120.0 . . ?
C2 N7 H7B 120.0 . . ?
N2 C2 N3 118.8(3) . . ?
N7 C2 N2 121.1(3) . . ?
N7 C2 N3 120.1(3) . . ?
N1 C3 N4 119.8(3) . . ?
N9 C3 N1 120.2(3) . . ?
N9 C3 N4 119.9(3) . . ?
H5C O5 H5D 105(4) . . ?
H6C O6 H6D 101(4) . . ?
C1 N8 H8A 120.0 . . ?
C1 N8 H8B 120.0 . . ?
H8A N8 H8B 120.0 . . ?
C3 N9 H9A 120.0 . . ?
C3 N9 H9B 120.0 . . ?
H9A N9 H9B 120.0 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
As1 O1 1.686(2) . ?
As1 O2 1.687(2) . ?
As1 O3 1.675(2) . ?
As1 O4 1.691(2) . ?
N1 H1A 0.8700 . ?
N1 H1B 0.8700 . ?
N1 C3 1.328(5) . ?
N2 H2A 0.8700 . ?
N2 H2B 0.8700 . ?
N2 C2 1.328(5) . ?
N3 H3A 0.8700 . ?
N3 H3B 0.8700 . ?
N3 C2 1.327(5) . ?
C1 N5 1.304(5) . ?
C1 N6 1.346(4) . ?
C1 N8 1.322(5) . ?
N4 H4A 0.8700 . ?
N4 H4B 0.8700 . ?
N4 C3 1.326(5) . ?
N5 H5A 0.8700 . ?
N5 H5B 0.8700 . ?
N6 H6A 0.8831 . ?
N6 H6B 0.8840 . ?
N7 H7A 0.8700 . ?
N7 H7B 0.8700 . ?
N7 C2 1.311(5) . ?
C3 N9 1.317(4) . ?
O5 H5C 0.85(2) . ?
O5 H5D 0.85(3) . ?
O6 H6C 0.87(3) . ?
O6 H6D 0.85(5) . ?
N8 H8A 0.8700 . ?
N8 H8B 0.8700 . ?
N9 H9A 0.8700 . ?
N9 H9B 0.8700 . ?
