# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_x
_database_code_depnum_ccdc_archive 'CCDC 2298406'
loop_
_audit_author_name
_audit_author_address
'Xiaoying Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H6 Al2 O20 P4, 2(C2 H8 N)'
_chemical_formula_sum            'C6 H22 Al2 N2 O20 P4'
_chemical_formula_weight         620.09
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.6163(14)
_cell_length_b                   9.7354(17)
_cell_length_c                   12.3722(18)
_cell_angle_alpha                90
_cell_angle_beta                 93.861(15)
_cell_angle_gamma                90
_cell_volume                     1035.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1860
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      28.7940
_cell_measurement_theta_min      3.2820
_shelx_estimated_absorpt_T_max   0.984
_shelx_estimated_absorpt_T_min   0.967
_exptl_absorpt_coefficient_mu    0.554
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.71253
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0431
_diffrn_reflns_av_unetI/netI     0.0656
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.843
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5714
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.816
_diffrn_reflns_theta_min         2.369
_diffrn_ambient_temperature      292(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.843
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1823
_reflns_number_total             2509
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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, 2018)'
_computing_structure_solution    ?
_refine_diff_density_max         0.572
_refine_diff_density_min         -0.522
_refine_diff_density_rms         0.108
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2509
_refine_ls_number_restraints     2
_refine_ls_R_factor_all          0.0731
_refine_ls_R_factor_gt           0.0450
_refine_ls_restrained_S_all      1.022
_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/[σ²(Fo²)+(0.0544P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0995
_refine_ls_wR_factor_ref         0.1146
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O3-H3
 0.82 with sigma of 0.01
 O6-H6
 0.82 with sigma of 0.01
2.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
2.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Al1 Al 0.48543(10) 0.26574(9) 0.02051(6) 0.0113(2) Uani 1 1 d . . . . .
P1 P 0.56496(9) 0.26158(8) 0.27253(6) 0.0157(2) Uani 1 1 d . . . . .
P2 P 0.24578(8) 0.50943(8) -0.01263(5) 0.01160(19) Uani 1 1 d . . . . .
O1 O 0.4749(2) 0.2229(2) 0.16957(15) 0.0155(4) Uani 1 1 d . . . . .
O2 O 0.4898(2) 0.2104(2) 0.37026(15) 0.0171(5) Uani 1 1 d . . . . .
O3 O 0.5707(4) 0.4226(3) 0.27889(18) 0.0432(8) Uani 1 1 d D . . . .
H3 H 0.571(5) 0.458(4) 0.2188(17) 0.052 Uiso 1 1 d D U . . .
O4 O 0.7327(3) 0.2115(4) 0.2715(2) 0.0490(9) Uani 1 1 d . . . . .
H4 H 0.770(5) 0.178(5) 0.324(4) 0.059 Uiso 1 1 d . U . . .
O5 O 0.3149(2) 0.3757(2) 0.02939(16) 0.0173(5) Uani 1 1 d . . . . .
O6 O 0.1311(2) 0.4776(2) -0.11397(16) 0.0212(5) Uani 1 1 d D . . . .
H6 H 0.044(2) 0.457(4) -0.097(3) 0.025 Uiso 1 1 d D U . . .
O7 O 0.1509(2) 0.5772(2) 0.07140(15) 0.0173(5) Uani 1 1 d . . . . .
O8 O 0.3680(2) 0.6019(2) -0.05537(15) 0.0155(4) Uani 1 1 d . . . . .
O9 O 0.3422(2) 0.1086(2) -0.00442(15) 0.0142(4) Uani 1 1 d . . . . .
O10 O 0.3546(2) -0.1217(2) -0.01511(15) 0.0142(4) Uani 1 1 d . . . . .
C1 C 0.4119(3) -0.0038(3) -0.0053(2) 0.0122(6) Uani 1 1 d . . . . .
N1 N 0.1495(3) 0.1862(4) 0.1981(2) 0.0362(8) Uani 1 1 d . . . . .
H1A H 0.158756 0.116313 0.244499 0.043 Uiso 1 1 calc R U . . .
H1B H 0.239871 0.195149 0.167923 0.043 Uiso 1 1 calc R U . . .
C2 C 0.1195(5) 0.3120(4) 0.2585(3) 0.0431(10) Uani 1 1 d . . . . .
H2A H 0.191668 0.318060 0.320869 0.065 Uiso 1 1 calc R U . . .
H2B H 0.015195 0.309974 0.281308 0.065 Uiso 1 1 calc R U . . .
H2C H 0.131866 0.390393 0.212761 0.065 Uiso 1 1 calc R U . . .
C3 C 0.0274(5) 0.1526(6) 0.1125(4) 0.0546(12) Uani 1 1 d . . . . .
H3A H 0.054028 0.068863 0.077238 0.082 Uiso 1 1 calc R U . . .
H3B H 0.019340 0.225765 0.060402 0.082 Uiso 1 1 calc R U . . .
H3C H -0.070371 0.141468 0.144342 0.082 Uiso 1 1 calc R U . . .


_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
Al1 O1 1.899(2) . ?
Al1 O2 1.876(2) 4_565 ?
Al1 O5 1.827(2) . ?
Al1 O8 1.835(2) 3_665 ?
Al1 O9 1.977(2) . ?
Al1 O10 1.971(2) 3_655 ?
P1 O1 1.4946(19) . ?
P1 O2 1.495(2) . ?
P1 O3 1.570(3) . ?
P1 O4 1.526(3) . ?
P2 O5 1.509(2) . ?
P2 O6 1.5741(19) . ?
P2 O7 1.516(2) . ?
P2 O8 1.508(2) . ?
O3 H3 0.819(10) . ?
O4 H4 0.77(5) . ?
O6 H6 0.815(10) . ?
O9 C1 1.248(3) . ?
O10 C1 1.253(3) . ?
C1 C1 1.517(5) 3_655 ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C2 1.467(5) . ?
N1 C3 1.478(5) . ?
C2 H2A 0.9600 . ?
C2 H2B 0.9600 . ?
C2 H2C 0.9600 . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?

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 Al1 O9 84.91(9) . . ?
O1 Al1 O10 87.48(9) . 3_655 ?
O2 Al1 O1 174.20(10) 4_565 . ?
O2 Al1 O9 89.72(9) 4_565 . ?
O2 Al1 O10 89.66(9) 4_565 3_655 ?
O5 Al1 O1 88.79(10) . . ?
O5 Al1 O2 93.25(10) . 4_565 ?
O5 Al1 O8 96.79(10) . 3_665 ?
O5 Al1 O9 88.10(9) . . ?
O5 Al1 O10 170.43(10) . 3_655 ?
O8 Al1 O1 90.18(9) 3_665 . ?
O8 Al1 O2 94.97(9) 3_665 4_565 ?
O8 Al1 O9 173.01(9) 3_665 . ?
O8 Al1 O10 92.04(9) 3_665 3_655 ?
O10 Al1 O9 82.80(9) 3_655 . ?
O1 P1 O2 112.13(12) . . ?
O1 P1 O3 107.88(13) . . ?
O1 P1 O4 110.53(15) . . ?
O2 P1 O3 107.83(14) . . ?
O2 P1 O4 111.24(13) . . ?
O4 P1 O3 106.99(19) . . ?
O5 P2 O6 108.45(12) . . ?
O5 P2 O7 110.96(12) . . ?
O7 P2 O6 107.06(12) . . ?
O8 P2 O5 111.55(12) . . ?
O8 P2 O6 104.71(12) . . ?
O8 P2 O7 113.69(12) . . ?
P1 O1 Al1 135.75(14) . . ?
P1 O2 Al1 142.98(14) . 4_566 ?
P1 O3 H3 112(3) . . ?
P1 O4 H4 118(4) . . ?
P2 O5 Al1 141.70(14) . . ?
P2 O6 H6 112(2) . . ?
P2 O8 Al1 145.34(13) . 3_665 ?
C1 O9 Al1 112.61(17) . . ?
C1 O10 Al1 112.55(17) . 3_655 ?
O9 C1 O10 128.1(3) . . ?
O9 C1 C1 115.8(3) . 3_655 ?
O10 C1 C1 116.0(3) . 3_655 ?
H1A N1 H1B 107.6 . . ?
C2 N1 H1A 108.7 . . ?
C2 N1 H1B 108.7 . . ?
C2 N1 C3 114.1(3) . . ?
C3 N1 H1A 108.7 . . ?
C3 N1 H1B 108.7 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O8 0.819(10) 2.20(3) 2.860(3) 138(4) 3_665 yes
O4 H4 O7 0.77(5) 1.73(5) 2.496(3) 170(5) 2_645 yes
O6 H6 O7 0.815(10) 1.765(11) 2.577(3) 174(4) 3_565 yes
N1 H1A O6 0.89 2.00 2.832(4) 154.3 4_566 yes
N1 H1B O1 0.89 2.04 2.871(4) 154.6 . yes
N1 H1B O5 0.89 2.57 3.193(4) 127.9 . yes
N1 H1B O9 0.89 2.51 3.189(4) 133.8 . yes
C2 H2A O9 0.96 2.55 3.483(4) 164.8 4_566 yes
C2 H2B O4 0.96 2.61 3.487(5) 151.9 1_455 yes
C2 H2C O7 0.96 2.54 3.490(5) 172.4 . yes
C3 H3C O4 0.96 2.49 3.365(6) 152.1 1_455 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Al1 O9 C1 O10 177.1(2) . . . . ?
Al1 O9 C1 C1 -3.7(3) . . . 3_655 ?
Al1 O10 C1 O9 176.5(2) 3_655 . . . ?
Al1 O10 C1 C1 -2.7(3) 3_655 . . 3_655 ?
O1 Al1 O5 P2 143.3(2) . . . . ?
O1 P1 O2 Al1 -162.2(2) . . . 4_566 ?
O2 Al1 O5 P2 -42.1(2) 4_565 . . . ?
O2 P1 O1 Al1 172.22(17) . . . . ?
O3 P1 O1 Al1 53.6(2) . . . . ?
O3 P1 O2 Al1 -43.6(3) . . . 4_566 ?
O4 P1 O1 Al1 -63.0(2) . . . . ?
O4 P1 O2 Al1 73.5(3) . . . 4_566 ?
O5 Al1 O1 P1 -105.8(2) . . . . ?
O5 P2 O8 Al1 -87.1(2) . . . 3_665 ?
O6 P2 O5 Al1 95.1(2) . . . . ?
O6 P2 O8 Al1 155.8(2) . . . 3_665 ?
O7 P2 O5 Al1 -147.54(19) . . . . ?
O7 P2 O8 Al1 39.3(3) . . . 3_665 ?
O8 Al1 O1 P1 -9.0(2) 3_665 . . . ?
O8 Al1 O5 P2 53.3(2) 3_665 . . . ?
O8 P2 O5 Al1 -19.7(2) . . . . ?
O9 Al1 O1 P1 166.0(2) . . . . ?
O9 Al1 O5 P2 -131.7(2) . . . . ?
O10 Al1 O1 P1 83.0(2) 3_655 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_x_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2298410'
loop_
_audit_author_name
_audit_author_address
'Xiaoying Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H6 Ga2 O20 P4, 2(C2 H8 N)'
_chemical_formula_sum            'C6 H22 Ga2 N2 O20 P4'
_chemical_formula_weight         705.57
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 '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           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.5858(10)
_cell_length_b                   9.7952(13)
_cell_length_c                   12.5984(15)
_cell_angle_alpha                90
_cell_angle_beta                 94.080(12)
_cell_angle_gamma                90
_cell_volume                     1056.8(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    1721
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.4700
_cell_measurement_theta_min      4.7060
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.954
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64939
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.84a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.217
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             708
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0451
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.861
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5672
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.861
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.604
_diffrn_reflns_theta_min         2.378
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.861
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Atlas'
_diffrn_measurement_method       ?
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2066
_reflns_number_total             2566
_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       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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, 2018)'
_computing_structure_solution    ?
_refine_diff_density_max         0.580
_refine_diff_density_min         -0.763
_refine_diff_density_rms         0.151
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     165
_refine_ls_number_reflns         2566
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0572
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      1.056
_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/[σ²(Fo²)+(0.0212P)²+0.0906P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0721
_refine_ls_wR_factor_ref         0.0817
_refine_special_details          ?
_olex2_refinement_description    
;
1. Restrained distances
 O3-H3
 0.82 with sigma of 0.01
2. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B)
3.b Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
Ga1 Ga 0.48322(4) 0.26827(4) 0.02087(3) 0.00560(11) Uani 1 1 d . . . . .
P1 P 0.56266(10) 0.25504(9) 0.27319(7) 0.0074(2) Uani 1 1 d . . . . .
P2 P 0.24129(10) 0.51068(9) -0.01591(7) 0.00628(19) Uani 1 1 d . . . . .
O1 O 0.4709(3) 0.2166(2) 0.17155(17) 0.0076(5) Uani 1 1 d . . . . .
O2 O 0.4860(2) 0.2008(2) 0.36893(17) 0.0082(5) Uani 1 1 d . . . . .
O3 O 0.5688(3) 0.4154(3) 0.28094(19) 0.0179(6) Uani 1 1 d D . . . .
H3 H 0.576(5) 0.447(4) 0.2218(15) 0.021 Uiso 1 1 d D U . . .
O4 O 0.7317(3) 0.2027(3) 0.2719(2) 0.0193(6) Uani 1 1 d . . . . .
H4 H 0.775(4) 0.169(4) 0.334(3) 0.023 Uiso 1 1 d . U . . .
O5 O 0.3049(2) 0.3791(2) 0.03405(18) 0.0086(5) Uani 1 1 d . . . . .
O6 O 0.1244(3) 0.4732(3) -0.11373(18) 0.0097(5) Uani 1 1 d . . . . .
H6 H 0.044(4) 0.457(4) -0.103(3) 0.012 Uiso 1 1 d . U . . .
O7 O 0.1497(2) 0.5893(2) 0.06275(18) 0.0087(5) Uani 1 1 d . . . . .
O8 O 0.3674(3) 0.5945(2) -0.06437(17) 0.0082(5) Uani 1 1 d . . . . .
O9 O 0.3383(2) 0.1061(2) -0.00690(17) 0.0073(5) Uani 1 1 d . . . . .
O10 O 0.3524(2) -0.1217(2) -0.01488(17) 0.0088(5) Uani 1 1 d . . . . .
C1 C 0.4111(4) -0.0047(3) -0.0065(3) 0.0070(7) Uani 1 1 d . U . . .
N1 N 0.1478(3) 0.1851(3) 0.2015(2) 0.0143(7) Uani 1 1 d . . . . .
H1A H 0.149458 0.116810 0.250532 0.017 Uiso 1 1 calc R U . . .
H1B H 0.243495 0.188076 0.174898 0.017 Uiso 1 1 calc R U . . .
C2 C 0.1206(4) 0.3152(4) 0.2554(3) 0.0169(8) Uani 1 1 d . . . . .
H2A H 0.194037 0.323731 0.318237 0.025 Uiso 1 1 calc R U . . .
H2B H 0.013415 0.317542 0.277272 0.025 Uiso 1 1 calc R U . . .
H2C H 0.136393 0.390986 0.206511 0.025 Uiso 1 1 calc R U . . .
C3 C 0.0291(4) 0.1513(4) 0.1133(3) 0.0200(9) Uani 1 1 d . . . . .
H3A H 0.054055 0.062615 0.082726 0.030 Uiso 1 1 calc R U . . .
H3B H 0.029870 0.221798 0.058148 0.030 Uiso 1 1 calc R U . . .
H3C H -0.074573 0.147215 0.141018 0.030 Uiso 1 1 calc R U . . .


_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
Ga1 O1 1.975(2) . ?
Ga1 O2 1.940(2) 4_565 ?
Ga1 O5 1.894(2) . ?
Ga1 O8 1.911(2) 3_665 ?
Ga1 O9 2.032(2) . ?
Ga1 O10 2.019(2) 3_655 ?
P1 O1 1.503(2) . ?
P1 O2 1.511(2) . ?
P1 O3 1.574(3) . ?
P1 O4 1.541(3) . ?
P2 O5 1.519(2) . ?
P2 O6 1.577(2) . ?
P2 O7 1.518(2) . ?
P2 O8 1.521(2) . ?
O3 H3 0.814(10) . ?
O4 H4 0.90(4) . ?
O6 H6 0.73(4) . ?
O9 C1 1.253(4) . ?
O10 C1 1.253(4) . ?
C1 C1 1.527(6) 3_655 ?
N1 H1A 0.9100 . ?
N1 H1B 0.9100 . ?
N1 C2 1.470(5) . ?
N1 C3 1.491(5) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?

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 Ga1 O9 83.76(9) . . ?
O1 Ga1 O10 86.51(9) . 3_655 ?
O2 Ga1 O1 173.67(10) 4_565 . ?
O2 Ga1 O9 90.15(9) 4_565 . ?
O2 Ga1 O10 90.96(9) 4_565 3_655 ?
O5 Ga1 O1 87.92(9) . . ?
O5 Ga1 O2 93.64(9) . 4_565 ?
O5 Ga1 O8 95.85(10) . 3_665 ?
O5 Ga1 O9 88.54(9) . . ?
O5 Ga1 O10 169.38(9) . 3_655 ?
O8 Ga1 O1 89.16(9) 3_665 . ?
O8 Ga1 O2 96.78(10) 3_665 4_565 ?
O8 Ga1 O9 171.53(9) 3_665 . ?
O8 Ga1 O10 93.10(10) 3_665 3_655 ?
O10 Ga1 O9 81.88(9) 3_655 . ?
O1 P1 O2 111.11(13) . . ?
O1 P1 O3 108.42(14) . . ?
O1 P1 O4 110.15(14) . . ?
O2 P1 O3 108.42(14) . . ?
O2 P1 O4 110.84(14) . . ?
O4 P1 O3 107.80(16) . . ?
O5 P2 O6 108.45(14) . . ?
O5 P2 O8 112.29(13) . . ?
O7 P2 O5 110.35(13) . . ?
O7 P2 O6 107.34(13) . . ?
O7 P2 O8 113.84(14) . . ?
O8 P2 O6 104.12(13) . . ?
P1 O1 Ga1 133.96(14) . . ?
P1 O2 Ga1 140.27(15) . 4_566 ?
P1 O3 H3 109(3) . . ?
P1 O4 H4 116(2) . . ?
P2 O5 Ga1 136.00(14) . . ?
P2 O6 H6 118(3) . . ?
P2 O8 Ga1 138.34(14) . 3_665 ?
C1 O9 Ga1 112.2(2) . . ?
C1 O10 Ga1 112.0(2) . 3_655 ?
O9 C1 O10 126.5(3) . . ?
O9 C1 C1 116.2(3) . 3_655 ?
O10 C1 C1 117.3(4) . 3_655 ?
H1A N1 H1B 107.6 . . ?
C2 N1 H1A 108.6 . . ?
C2 N1 H1B 108.6 . . ?
C2 N1 C3 114.5(3) . . ?
C3 N1 H1A 108.6 . . ?
C3 N1 H1B 108.6 . . ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O3 H3 O8 0.814(10) 2.12(3) 2.823(3) 145(4) 3_665 yes
O4 H4 O7 0.90(4) 1.62(4) 2.511(3) 172(4) 2_645 yes
O6 H6 O7 0.73(4) 1.83(4) 2.557(3) 174(4) 3_565 yes
N1 H1A O6 0.91 1.95 2.816(4) 158.5 4_566 yes
N1 H1B O1 0.91 1.98 2.843(4) 158.8 . yes
N1 H1B O5 0.91 2.66 3.207(4) 119.7 . yes
N1 H1B O9 0.91 2.61 3.284(4) 131.3 . yes
C2 H2A O9 0.98 2.54 3.502(4) 165.6 4_566 yes
C3 H3C O4 0.98 2.48 3.389(4) 153.6 1_455 yes

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ga1 O9 C1 O10 175.4(3) . . . . ?
Ga1 O9 C1 C1 -4.1(4) . . . 3_655 ?
Ga1 O10 C1 O9 175.7(3) 3_655 . . . ?
Ga1 O10 C1 C1 -4.7(4) 3_655 . . 3_655 ?
O1 Ga1 O5 P2 149.8(2) . . . . ?
O1 P1 O2 Ga1 -160.1(2) . . . 4_566 ?
O2 Ga1 O5 P2 -36.4(2) 4_565 . . . ?
O2 P1 O1 Ga1 171.18(17) . . . . ?
O3 P1 O1 Ga1 52.1(2) . . . . ?
O3 P1 O2 Ga1 -41.0(3) . . . 4_566 ?
O4 P1 O1 Ga1 -65.6(2) . . . . ?
O4 P1 O2 Ga1 77.1(3) . . . 4_566 ?
O5 P2 O8 Ga1 -88.1(2) . . . 3_665 ?
O6 P2 O5 Ga1 93.8(2) . . . . ?
O6 P2 O8 Ga1 154.7(2) . . . 3_665 ?
O7 P2 O5 Ga1 -148.86(18) . . . . ?
O7 P2 O8 Ga1 38.2(3) . . . 3_665 ?
O8 Ga1 O5 P2 60.8(2) 3_665 . . . ?
O8 P2 O5 Ga1 -20.7(3) . . . . ?
O9 Ga1 O5 P2 -126.4(2) . . . . ?
O10 Ga1 O5 P2 -151.9(4) 3_655 . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_x_CCDC2
_database_code_depnum_ccdc_archive 'CCDC 2298424'
loop_
_audit_author_name
_audit_author_address
'Xiaoying Huang'
;Fujian Institute of Research on the Structure of Matter, Chinese Academy of Sciences
China
;
_audit_update_record             
;
2023-09-29 deposited with the CCDC.	2023-12-26 downloaded from the CCDC.
;
_audit_creation_date             2023-09-26
_audit_creation_method           
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H6 In2 O20 P4, 2(C2 H8 N), H2 O'
_chemical_formula_sum            'C6 H24 In2 N2 O21 P4'
_chemical_formula_weight         813.79
_chemical_absolute_configuration ?
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
In In 0.0822 5.0449 '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           4
_space_group_name_H-M_alt        'P 1 21 1'
_space_group_name_Hall           'P 2yb'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'

_cell_length_a                   8.95360(10)
_cell_length_b                   10.26900(10)
_cell_length_c                   13.16290(10)
_cell_angle_alpha                90
_cell_angle_beta                 95.5430(10)
_cell_angle_gamma                90
_cell_volume                     1204.60(2)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8951
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      74.7310
_cell_measurement_theta_min      3.3560
_shelx_estimated_absorpt_T_max   0.603
_shelx_estimated_absorpt_T_min   0.316
_exptl_absorpt_coefficient_mu    18.729
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.28099
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.42.90a (Rigaku Oxford Diffraction, 2023)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_density_diffrn    2.244
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0374
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11935
_diffrn_reflns_point_group_measured_fraction_full 0.938
_diffrn_reflns_point_group_measured_fraction_max 0.895
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         75.170
_diffrn_reflns_theta_min         3.373
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       ?
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_source                   ?
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_full    0.869
_reflns_Friedel_fraction_max     0.807
_reflns_number_gt                4368
_reflns_number_total             4430
_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. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_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, 2018)'
_computing_structure_solution    ?
_refine_diff_density_max         1.179
_refine_diff_density_min         -1.638
_refine_diff_density_rms         0.165
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.000(8)
_refine_ls_extinction_coef       0.00041(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         4430
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0308
_refine_ls_R_factor_gt           0.0305
_refine_ls_restrained_S_all      1.045
_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)+(0.0548P)²+0.1034P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0788
_refine_ls_wR_factor_ref         0.0791
_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.9997
 0.0003
2. Restrained distances
 O21-H21A = O21-H21B
 0.82 with sigma of 0.01
 O14-H14 = O11-H11
 0.82 with sigma of 0.01
 H21B-H2A
 2.1 with sigma of 0.01
 H21A-H21B
 1.39 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B)
3.b Tetrahedral OH refined with riding coordinates:
 O2(H2C), O3(H3D), O7(H7A), O8(H8A)
3.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_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
In1 In 0.49703(5) 0.41310(4) 0.22627(3) 0.01448(13) Uani 1 1 d . . . . .
In2 In 0.52231(5) 0.46229(4) 0.73141(3) 0.01522(13) Uani 1 1 d . . . . .
P1 P 0.4448(2) 0.5217(2) -0.02035(13) 0.0225(4) Uani 1 1 d . . . . .
P2 P 0.4297(2) 0.4328(2) 0.47814(12) 0.0240(4) Uani 1 1 d . . . . .
P3 P 0.75683(17) 0.18156(18) 0.27442(13) 0.0143(3) Uani 1 1 d . . . . .
P4 P 0.78142(18) 0.69247(19) 0.75499(14) 0.0175(4) Uani 1 1 d . . . . .
O1 O 0.5065(6) 0.4344(6) 0.0642(4) 0.0265(13) Uani 1 1 d . . . . .
O2 O 0.2759(6) 0.4885(7) -0.0455(4) 0.0430(17) Uani 1 1 d . . . . .
H2C H 0.243181 0.527247 -0.097468 0.064 Uiso 1 1 calc R U . . .
O3 O 0.4446(9) 0.6645(7) 0.0166(4) 0.0478(17) Uani 1 1 d . . . . .
H3D H 0.530868 0.692112 0.023481 0.072 Uiso 1 1 calc R U . . .
O4 O 0.5278(6) 0.5102(7) -0.1128(3) 0.0300(13) Uani 1 1 d . . . . .
O5 O 0.5053(6) 0.3936(6) 0.3864(3) 0.0275(13) Uani 1 1 d . . . . .
O6 O 0.5248(6) 0.4027(6) 0.5755(3) 0.0239(11) Uani 1 1 d . . . . .
O7 O 0.2769(8) 0.3671(11) 0.4809(5) 0.084(4) Uani 1 1 d . . . . .
H7A H 0.247049 0.341428 0.423507 0.127 Uiso 1 1 calc R U . . .
O8 O 0.4014(11) 0.5829(8) 0.4718(5) 0.074(3) Uani 1 1 d . . . . .
H8A H 0.387076 0.610714 0.528433 0.111 Uiso 1 1 calc R U . . .
O9 O 0.6933(6) 0.3030(5) 0.2204(4) 0.0238(11) Uani 1 1 d . . . . .
O10 O 0.6350(5) 0.1059(5) 0.3225(4) 0.0216(11) Uani 1 1 d . . . . .
O11 O 0.8702(5) 0.2234(6) 0.3676(4) 0.0264(12) Uani 1 1 d D . . . .
H11 H 0.954(4) 0.236(10) 0.349(6) 0.032 Uiso 1 1 d D U . . .
O12 O 0.8413(6) 0.1000(6) 0.2029(4) 0.0259(11) Uani 1 1 d . . . . .
O13 O 0.6688(6) 0.7751(6) 0.8054(4) 0.0257(12) Uani 1 1 d . . . . .
O14 O 0.8978(6) 0.6545(7) 0.8471(4) 0.0359(15) Uani 1 1 d D . . . .
H14 H 0.976(6) 0.630(10) 0.825(7) 0.043 Uiso 1 1 d D U . . .
O15 O 0.8629(5) 0.7676(5) 0.6770(4) 0.0265(11) Uani 1 1 d . . . . .
O16 O 0.7125(6) 0.5708(6) 0.7066(4) 0.0300(13) Uani 1 1 d . . . . .
O17 O 0.3653(6) 0.3030(5) 0.7501(4) 0.0250(11) Uani 1 1 d . . . . .
O18 O 0.3558(6) 0.0863(5) 0.7552(4) 0.0234(11) Uani 1 1 d . . . . .
O19 O 0.6683(6) 0.2915(5) 0.7615(4) 0.0221(11) Uani 1 1 d . . . . .
O20 O 0.6596(6) 0.0763(5) 0.7725(4) 0.0213(11) Uani 1 1 d . . . . .
C1 C 0.4256(7) 0.1931(8) 0.7549(5) 0.0170(14) Uani 1 1 d . . . . .
C2 C 0.5995(8) 0.1862(8) 0.7636(5) 0.0174(14) Uani 1 1 d . . . . .
N1 N 0.8390(9) 0.3900(12) 0.5398(6) 0.062(3) Uani 1 1 d . . . . .
H1A H 0.754117 0.403133 0.568325 0.075 Uiso 1 1 calc R U . . .
H1B H 0.822314 0.326729 0.493926 0.075 Uiso 1 1 calc R U . . .
C3 C 0.8766(14) 0.5086(14) 0.4872(9) 0.067(3) Uani 1 1 d . . . . .
H3A H 0.801831 0.524836 0.431327 0.100 Uiso 1 1 calc R U . . .
H3B H 0.972816 0.498693 0.461728 0.100 Uiso 1 1 calc R U . . .
H3C H 0.879798 0.580595 0.533947 0.100 Uiso 1 1 calc R U . . .
C4 C 0.9538(13) 0.3467(17) 0.6184(9) 0.079(4) Uani 1 1 d . . . . .
H4A H 0.924769 0.264624 0.645299 0.119 Uiso 1 1 calc R U . . .
H4B H 0.964783 0.409976 0.672252 0.119 Uiso 1 1 calc R U . . .
H4C H 1.047463 0.336957 0.589334 0.119 Uiso 1 1 calc R U . . .
N2 N 0.8578(9) 0.4656(11) 0.0850(8) 0.068(3) Uani 1 1 d . . . . .
H2A H 0.804004 0.534839 0.063269 0.081 Uiso 1 1 calc DR U . . .
H2B H 0.805486 0.422636 0.128437 0.081 Uiso 1 1 calc R U . . .
C5 C 0.8765(14) 0.3802(13) -0.0036(9) 0.069(4) Uani 1 1 d . . . . .
H5A H 0.787346 0.383522 -0.050295 0.103 Uiso 1 1 calc R U . . .
H5B H 0.893534 0.292348 0.019581 0.103 Uiso 1 1 calc R U . . .
H5C H 0.960680 0.409484 -0.037380 0.103 Uiso 1 1 calc R U . . .
C6 C 0.9976(14) 0.5107(16) 0.1401(12) 0.081(4) Uani 1 1 d . . . . .
H6A H 0.975346 0.567170 0.194749 0.122 Uiso 1 1 calc R U . . .
H6B H 1.055215 0.557414 0.094155 0.122 Uiso 1 1 calc R U . . .
H6C H 1.054178 0.437189 0.167480 0.122 Uiso 1 1 calc R U . . .
O21 O 0.7529(15) 0.7167(11) 0.0294(7) 0.094(4) Uani 1 1 d D . . . .
H21A H 0.762(18) 0.760(13) -0.023(6) 0.141 Uiso 1 1 d D U . . .
H21B H 0.812(13) 0.7383(19) 0.079(7) 0.141 Uiso 1 1 d D U . . .


_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
In1 O1 2.154(5) . ?
In1 O5 2.111(4) . ?
In1 O9 2.097(5) . ?
In1 O13 2.065(5) 2_646 ?
In1 O18 2.213(6) 2_656 ?
In1 O20 2.186(6) 2_656 ?
In2 O4 2.105(5) 1_556 ?
In2 O6 2.143(5) . ?
In2 O10 2.114(5) 2_656 ?
In2 O16 2.087(5) . ?
In2 O17 2.186(6) . ?
In2 O19 2.201(5) . ?
P1 O1 1.493(6) . ?
P1 O2 1.554(6) . ?
P1 O3 1.545(7) . ?
P1 O4 1.490(5) . ?
P2 O5 1.496(5) . ?
P2 O6 1.501(5) . ?
P2 O7 1.529(7) . ?
P2 O8 1.563(8) . ?
P3 O9 1.519(5) . ?
P3 O10 1.525(5) . ?
P3 O11 1.575(5) . ?
P3 O12 1.516(5) . ?
P4 O13 1.519(6) . ?
P4 O14 1.569(5) . ?
P4 O15 1.526(5) . ?
P4 O16 1.507(6) . ?
O2 H2C 0.8200 . ?
O3 H3D 0.8200 . ?
O7 H7A 0.8200 . ?
O8 H8A 0.8200 . ?
O11 H11 0.821(14) . ?
O14 H14 0.823(14) . ?
O17 C1 1.249(9) . ?
O18 C1 1.262(10) . ?
O19 C2 1.247(9) . ?
O20 C2 1.251(9) . ?
C1 C2 1.552(9) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C3 1.456(17) . ?
N1 C4 1.455(15) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 C5 1.482(16) . ?
N2 C6 1.460(15) . ?
C5 H5A 0.9600 . ?
C5 H5B 0.9600 . ?
C5 H5C 0.9600 . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?
O21 H21A 0.826(14) . ?
O21 H21B 0.829(14) . ?

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 In1 O18 87.0(2) . 2_656 ?
O1 In1 O20 90.9(2) . 2_656 ?
O5 In1 O1 175.72(18) . . ?
O5 In1 O18 90.2(2) . 2_656 ?
O5 In1 O20 91.5(2) . 2_656 ?
O9 In1 O1 84.5(2) . . ?
O9 In1 O5 92.1(2) . . ?
O9 In1 O18 86.9(2) . 2_656 ?
O9 In1 O20 162.51(19) . 2_656 ?
O13 In1 O1 88.1(2) 2_646 . ?
O13 In1 O5 95.3(2) 2_646 . ?
O13 In1 O9 102.2(2) 2_646 . ?
O13 In1 O18 169.2(2) 2_646 2_656 ?
O13 In1 O20 94.5(2) 2_646 2_656 ?
O20 In1 O18 76.0(2) 2_656 2_656 ?
O4 In2 O6 176.4(2) 1_556 . ?
O4 In2 O10 96.7(2) 1_556 2_656 ?
O4 In2 O17 91.1(2) 1_556 . ?
O4 In2 O19 93.1(2) 1_556 . ?
O6 In2 O17 87.7(2) . . ?
O6 In2 O19 83.3(2) . . ?
O10 In2 O6 86.9(2) 2_656 . ?
O10 In2 O17 98.3(2) 2_656 . ?
O10 In2 O19 168.95(19) 2_656 . ?
O16 In2 O4 94.9(2) . 1_556 ?
O16 In2 O6 85.3(2) . . ?
O16 In2 O10 95.9(2) . 2_656 ?
O16 In2 O17 163.8(2) . . ?
O16 In2 O19 88.5(2) . . ?
O17 In2 O19 76.2(2) . . ?
O1 P1 O2 108.1(3) . . ?
O1 P1 O3 110.3(4) . . ?
O3 P1 O2 104.2(4) . . ?
O4 P1 O1 112.5(3) . . ?
O4 P1 O2 111.1(3) . . ?
O4 P1 O3 110.4(4) . . ?
O5 P2 O6 111.8(3) . . ?
O5 P2 O7 112.1(4) . . ?
O5 P2 O8 107.8(4) . . ?
O6 P2 O7 108.9(4) . . ?
O6 P2 O8 108.9(4) . . ?
O7 P2 O8 107.2(6) . . ?
O9 P3 O10 111.2(3) . . ?
O9 P3 O11 108.9(3) . . ?
O10 P3 O11 104.4(3) . . ?
O12 P3 O9 110.5(3) . . ?
O12 P3 O10 113.3(3) . . ?
O12 P3 O11 108.2(3) . . ?
O13 P4 O14 102.8(3) . . ?
O13 P4 O15 113.1(3) . . ?
O15 P4 O14 108.7(3) . . ?
O16 P4 O13 112.7(3) . . ?
O16 P4 O14 109.6(4) . . ?
O16 P4 O15 109.7(3) . . ?
P1 O1 In1 138.7(4) . . ?
P1 O2 H2C 109.5 . . ?
P1 O3 H3D 109.5 . . ?
P1 O4 In2 147.9(3) . 1_554 ?
P2 O5 In1 143.7(3) . . ?
P2 O6 In2 134.6(3) . . ?
P2 O7 H7A 109.5 . . ?
P2 O8 H8A 109.5 . . ?
P3 O9 In1 134.6(3) . . ?
P3 O10 In2 134.1(3) . 2_646 ?
P3 O11 H11 110(6) . . ?
P4 O13 In1 142.2(3) . 2_656 ?
P4 O14 H14 109(7) . . ?
P4 O16 In2 133.1(3) . . ?
C1 O17 In2 113.7(5) . . ?
C1 O18 In1 114.2(4) . 2_646 ?
C2 O19 In2 114.1(4) . . ?
C2 O20 In1 114.9(5) . 2_646 ?
O17 C1 O18 125.0(6) . . ?
O17 C1 C2 118.1(6) . . ?
O18 C1 C2 116.9(6) . . ?
O19 C2 O20 125.1(6) . . ?
O19 C2 C1 116.9(6) . . ?
O20 C2 C1 117.9(6) . . ?
H1A N1 H1B 107.6 . . ?
C3 N1 H1A 108.6 . . ?
C3 N1 H1B 108.6 . . ?
C4 N1 H1A 108.6 . . ?
C4 N1 H1B 108.6 . . ?
C4 N1 C3 114.4(10) . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
H2A N2 H2B 107.5 . . ?
C5 N2 H2A 108.5 . . ?
C5 N2 H2B 108.5 . . ?
C6 N2 H2A 108.5 . . ?
C6 N2 H2B 108.5 . . ?
C6 N2 C5 114.9(10) . . ?
N2 C5 H5A 109.5 . . ?
N2 C5 H5B 109.5 . . ?
N2 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
N2 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
H21A O21 H21B 114(3) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2C O12 0.82 1.69 2.507(7) 174.2 2_655 yes
O3 H3D O21 0.82 2.00 2.801(15) 166.3 . yes
O7 H7A O15 0.82 1.74 2.535(8) 161.5 2_646 yes
O8 H8A O10 0.82 1.99 2.769(8) 157.9 2_656 yes
O11 H11 O15 0.821(14) 1.738(18) 2.556(7) 174(9) 2_746 yes
O14 H14 O12 0.823(14) 1.74(3) 2.550(7) 169(10) 2_756 yes
N1 H1A O6 0.89 2.06 2.900(9) 155.9 . yes
N1 H1A O16 0.89 2.56 3.167(10) 126.2 . yes
N1 H1B O11 0.89 2.05 2.875(10) 153.2 . yes
C4 H4C O7 0.96 2.63 3.564(14) 164.1 1_655 yes
N2 H2A O21 0.89 1.96 2.816(16) 159.9 . yes
N2 H2B O9 0.89 2.05 2.939(11) 173.0 . yes
O21 H21A O13 0.826(14) 2.34(7) 3.032(11) 142(10) 1_554 yes
O21 H21A O14 0.826(14) 2.44(17) 2.907(11) 116(15) 1_554 yes

_olex2_submission_special_instructions 'No special instructions were received'
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.9997
2 0.0003

# start Validation Reply Form
_vrf_PLAT420_x                   
;
PROBLEM: D-H Bond Without Acceptor  O21      --H21B     .     Please Check 
RESPONSE: This is probably due to the statistical distribution of water molecule over two orientations.
;
# end Validation Reply Form

