# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_exp_10657_auto
_database_code_depnum_ccdc_archive 'CCDC 2093747'
loop_
_audit_author_name
_audit_author_address
'Dongmei Wang'
;Fujian Institute of Research on the Structure of Matter
China
;
_audit_update_record             
;
2021-07-01 deposited with the CCDC.	2021-12-06 downloaded from the CCDC.
;
_audit_creation_date             2021-06-22
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2017/1
_chemical_name_common            ?
_chemical_name_systematic        
;
 ?
;
_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
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         'As C N O'
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'

_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.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_H-M_alt        'C 1 c 1'
_space_group_name_Hall           'C -2yc'
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'

_cell_length_a                   6.5850(3)
_cell_length_b                   17.7646(7)
_cell_length_c                   12.3972(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.506(4)
_cell_angle_gamma                90
_cell_volume                     1403.99(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9541
_cell_measurement_temperature    235(30)
_cell_measurement_theta_max      51.8270
_cell_measurement_theta_min      4.3210
_shelx_estimated_absorpt_T_max   0.788
_shelx_estimated_absorpt_T_min   0.788
_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_absorpt_special_details   ?
_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_density_meas      ?
_exptl_crystal_density_method    ?
_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
_exptl_special_details           
;
 ?
;
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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_oxdiff_digest_frames     
;
01871806e5487943d0de90c679e60902f1033867a40
;
_diffrn_oxdiff_digest_hkl        
;
01bf52df22d35d88a63507c53a3e5805863efc
;
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.3405
_diffrn_source                   'micro-focus metaljet'
_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_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     50.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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)'
_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_R_factor_all          0.0188
_refine_ls_R_factor_gt           0.0183
_refine_ls_restrained_S_all      1.012
_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
_refine_special_details          ?
_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)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
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 . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
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 . ?

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 . . ?

_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
