# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_1
_database_code_depnum_ccdc_archive 'CCDC 2032249'
loop_
_audit_author_name
_audit_author_address
'Zhien Lin'
;Sichuan University
China
;
_audit_update_record             
;
2020-09-16 deposited with the CCDC.	2020-10-02 downloaded from the CCDC.
;
_audit_creation_date             2020-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(H52 In16 O96 P28)'
_chemical_formula_sum            'C9 H53 In8 N3 O55 P14'
_chemical_formula_weight         2435.68
_chemical_melting_point          ?
_chemical_oxdiff_formula         'H24  In16  O108  P28  '
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'
In In 0.0822 5.0449 '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'

_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      trigonal
_space_group_IT_number           165
_space_group_name_H-M_alt        'P -3 c 1'
_space_group_name_Hall           '-P 3 2"c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   13.8685(2)
_cell_length_b                   13.8685(2)
_cell_length_c                   18.6872(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     3112.66(13)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    4218
_cell_measurement_temperature    295.3(3)
_cell_measurement_theta_max      71.4990
_cell_measurement_theta_min      3.6570
_shelx_estimated_absorpt_T_max   0.055
_shelx_estimated_absorpt_T_min   0.033
_exptl_absorpt_coefficient_mu    27.783
_exptl_absorpt_correction_T_max  0.096
_exptl_absorpt_correction_T_min  0.010
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.599
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             2340
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -3 -1 0.1494
6 3 0 0.1502
1 -2 -12 0.2615
-1 2 12 0.1250
9 -3 0 0.1532
-9 3 -1 0.1245
-1 1 12 0.1286
3 -1 11 0.1336
9 -7 -1 0.1687
-9 7 -1 0.1171
4 -4 11 0.1438
5 -9 1 0.1469
-1 -2 11 0.1464
-5 9 -2 0.1141
0 -8 1 0.1316
0 8 0 0.1332
-3 -1 11 0.1437
0 2 -12 0.2104
-7 8 0 0.0820

_exptl_crystal_size_max          0.386
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.25
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-6.0000 -3.0000 -0.9997 0.2046 0.9884 0.1588
6.0000 3.0000 -0.0003 -0.1825 -0.9736 -0.2367
1.0000 -2.0000 -12.0001 0.0793 0.2962 -0.9661
-1.0000 2.0000 12.0001 -0.0793 -0.2962 0.9661
9.0000 -3.0000 -0.0004 -0.7396 -0.6193 -0.3276
-9.0000 3.0000 -0.9996 0.7617 0.6341 0.2496
-1.0000 1.0000 12.0001 -0.1414 -0.1841 0.9698
3.0000 -1.0000 10.9999 -0.4895 -0.3697 0.7487
9.0000 -7.0000 -1.0004 -0.9660 -0.1558 -0.3909
-9.0000 7.0000 -0.9996 1.0101 0.1855 0.2349
4.0000 -4.0000 10.9999 -0.7373 -0.1394 0.7221
5.0000 -9.0000 0.9998 -0.8884 0.4636 -0.0771
-1.0000 -2.0000 11.0001 -0.3057 0.1672 0.9028
-5.0000 9.0000 -1.9998 0.9105 -0.4487 -0.0009
0.0000 -8.0000 1.0000 -0.5189 0.8824 0.1073
-0.0000 8.0000 -0.0000 0.4969 -0.8972 -0.0294
-3.0000 -1.0000 11.0002 -0.1206 0.2675 0.9744
-0.0000 2.0000 -12.0000 0.3892 -0.0462 -0.9432
-7.0000 8.0000 0.0003 0.9272 -0.1539 0.2340

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0973
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9991
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.029
_diffrn_reflns_theta_max         67.028
_diffrn_reflns_theta_min         3.680
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      295.3(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -90.00  -2.00   1.00    7.36    --  -36.29 125.00 120.00   88
  2  ω   -104.00 -20.00   1.00    7.36    --  -36.29 -57.00  60.00   84
  3  ω    100.00 176.00   1.00   29.46    --  106.21 111.00  60.00   76
  4  ω     37.00 109.00   1.00   29.46    --  106.21 -94.00-150.00   72
  5  ω     88.00 173.00   1.00   29.46    --  106.21  61.00-150.00   85
  6  ω     37.00 109.00   1.00   29.46    --  106.21 -94.00-120.00   72
  7  ω     57.00 150.00   1.00   29.46    --  106.21 178.00 120.00   93
  8  ω   -104.00 -20.00   1.00    7.36    --  -36.29 -57.00 -60.00   84
  9  ω   -104.00 -10.00   1.00    7.36    --  -36.29 -77.00-150.00   94
 10  ω     37.00  78.00   1.00   29.46    --  106.21   0.00  30.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0614791000
_diffrn_orient_matrix_UB_12      0.0621068000
_diffrn_orient_matrix_UB_13      -0.0220833000
_diffrn_orient_matrix_UB_21      -0.1061904000
_diffrn_orient_matrix_UB_22      -0.1121495000
_diffrn_orient_matrix_UB_23      -0.0148403000
_diffrn_orient_matrix_UB_31      -0.0376197000
_diffrn_orient_matrix_UB_32      -0.0036690000
_diffrn_orient_matrix_UB_33      0.0779878000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1686
_reflns_number_total             1866
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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)'
_refine_diff_density_max         3.119
_refine_diff_density_min         -2.522
_refine_diff_density_rms         0.375
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         1866
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0701
_refine_ls_R_factor_gt           0.0665
_refine_ls_restrained_S_all      1.141
_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)+(0.1336P)²+6.8875P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1829
_refine_ls_wR_factor_ref         0.1903
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, All P(H) groups
2.a Riding coordinates:
 P1(H1), P2(H2), P3(H3)
2.b Rotating group:
 O8(H8A,H8B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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 0.70795(4) 0.14305(5) 0.46304(3) 0.0327(3) Uani 1 1 d . . . . .
In2 In 1.0000 0.0000 0.2500 0.0252(4) Uani 1 6 d S T P . .
In3 In 1.0000 0.0000 0.5000 0.0238(4) Uani 1 6 d S T P . .
P1 P 0.83983(16) 0.03056(17) 0.37261(11) 0.0275(5) Uani 1 1 d . . . . .
H1 H 0.7454 -0.0471 0.3473 0.041 Uiso 1 1 d R . . . .
P2 P 0.49328(16) 0.12402(17) 0.55832(12) 0.0292(5) Uani 1 1 d . . . . .
H2 H 0.4880 0.1713 0.6173 0.044 Uiso 1 1 d R . . . .
P3 P 0.6667 0.3333 0.3610(3) 0.0534(12) Uani 1 3 d S T P . .
H3 H 0.6667 0.3333 0.2914 0.00(3) Uiso 1 3 d RS T P . .
O1 O 0.8219(6) 0.1247(6) 0.3967(4) 0.0434(16) Uani 1 1 d . . . . .
O2 O 0.9298(5) 0.0747(5) 0.3164(3) 0.0348(13) Uani 1 1 d . . . . .
O3 O 0.8602(5) -0.0260(5) 0.4363(3) 0.0303(12) Uani 1 1 d . . . . .
O4 O 0.6142(5) 0.1660(6) 0.5439(4) 0.0492(18) Uani 1 1 d . . . . .
O5 O 0.4326(6) 0.1462(5) 0.4974(5) 0.049(2) Uani 1 1 d . . . . .
O6 O 0.4309(6) 0.0022(5) 0.5779(4) 0.0495(19) Uani 1 1 d . . . . .
O7 O 0.6798(8) 0.2346(7) 0.3819(5) 0.062(2) Uani 1 1 d . . . . .
O8 O 0.7477(6) 0.0532(6) 0.5478(4) 0.0398(14) Uani 1 1 d . . . . .
H8A H 0.6976 -0.0200 0.5487 0.060 Uiso 1 1 d GR . . . .
H8B H 0.7487 0.0794 0.5919 0.060 Uiso 1 1 d GR . . . .


_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 2.121(6) . ?
In1 O4 2.119(7) . ?
In1 O5 2.106(7) 2_655 ?
In1 O6 2.115(7) 7_656 ?
In1 O7 2.135(8) . ?
In1 O8 2.248(7) . ?
In2 O2 2.138(6) 5 ?
In2 O2 2.138(6) 4_645 ?
In2 O2 2.138(6) 6_765 ?
In2 O2 2.138(6) . ?
In2 O2 2.138(6) 3_765 ?
In2 O2 2.138(6) 2_645 ?
In3 O3 2.146(6) 7_756 ?
In3 O3 2.146(6) 3_765 ?
In3 O3 2.146(6) 8_666 ?
In3 O3 2.147(6) . ?
In3 O3 2.146(6) 9_546 ?
In3 O3 2.146(6) 2_645 ?
P1 H1 1.2996 . ?
P1 O1 1.515(6) . ?
P1 O2 1.507(6) . ?
P1 O3 1.528(6) . ?
P2 H2 1.3028 . ?
P2 O4 1.499(6) . ?
P2 O5 1.535(8) . ?
P2 O6 1.508(7) . ?
P3 H3 1.3001 . ?
P3 O7 1.520(8) . ?
P3 O7 1.520(8) 2_655 ?
P3 O7 1.520(8) 3_665 ?
O5 In1 2.106(7) 3_665 ?
O6 In1 2.115(7) 7_656 ?
O8 H8A 0.8989 . ?
O8 H8B 0.8989 . ?

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 O7 91.4(3) . . ?
O1 In1 O8 86.7(3) . . ?
O4 In1 O1 170.0(3) . . ?
O4 In1 O7 96.2(4) . . ?
O4 In1 O8 85.4(3) . . ?
O5 In1 O1 82.5(3) 2_655 . ?
O5 In1 O4 90.7(3) 2_655 . ?
O5 In1 O6 175.5(3) 2_655 7_656 ?
O5 In1 O7 91.7(4) 2_655 . ?
O5 In1 O8 85.5(3) 2_655 . ?
O6 In1 O1 93.0(3) 7_656 . ?
O6 In1 O4 93.8(3) 7_656 . ?
O6 In1 O7 87.7(3) 7_656 . ?
O6 In1 O8 94.9(3) 7_656 . ?
O7 In1 O8 176.8(3) . . ?
O2 In2 O2 178.3(3) 5 3_765 ?
O2 In2 O2 91.5(4) 3_765 6_765 ?
O2 In2 O2 89.7(2) 3_765 2_645 ?
O2 In2 O2 178.3(3) 6_765 2_645 ?
O2 In2 O2 89.7(2) 4_645 6_765 ?
O2 In2 O2 89.1(3) 6_765 . ?
O2 In2 O2 91.5(4) 5 . ?
O2 In2 O2 89.7(2) 5 4_645 ?
O2 In2 O2 178.3(3) 4_645 . ?
O2 In2 O2 89.7(2) 3_765 . ?
O2 In2 O2 89.7(2) 2_645 . ?
O2 In2 O2 89.1(3) 3_765 4_645 ?
O2 In2 O2 89.1(3) 5 2_645 ?
O2 In2 O2 89.7(2) 5 6_765 ?
O2 In2 O2 91.5(4) 4_645 2_645 ?
O3 In3 O3 92.2(2) 7_756 8_666 ?
O3 In3 O3 92.2(2) 8_666 9_546 ?
O3 In3 O3 87.8(2) 8_666 3_765 ?
O3 In3 O3 180.0 9_546 3_765 ?
O3 In3 O3 87.8(2) 2_645 9_546 ?
O3 In3 O3 87.8(2) 9_546 . ?
O3 In3 O3 180.0 7_756 . ?
O3 In3 O3 87.8(2) 7_756 2_645 ?
O3 In3 O3 92.2(2) 2_645 . ?
O3 In3 O3 87.8(2) 8_666 . ?
O3 In3 O3 92.2(2) 3_765 . ?
O3 In3 O3 180.0 8_666 2_645 ?
O3 In3 O3 87.8(2) 7_756 3_765 ?
O3 In3 O3 92.2(2) 7_756 9_546 ?
O3 In3 O3 92.2(2) 2_645 3_765 ?
O1 P1 H1 106.9 . . ?
O1 P1 O3 111.3(4) . . ?
O2 P1 H1 111.7 . . ?
O2 P1 O1 108.4(4) . . ?
O2 P1 O3 115.1(4) . . ?
O3 P1 H1 103.1 . . ?
O4 P2 H2 106.9 . . ?
O4 P2 O5 114.1(5) . . ?
O4 P2 O6 112.5(5) . . ?
O5 P2 H2 110.6 . . ?
O6 P2 H2 102.3 . . ?
O6 P2 O5 109.8(4) . . ?
O7 P3 H3 104.9 . . ?
O7 P3 H3 104.9 3_665 . ?
O7 P3 H3 104.9 2_655 . ?
O7 P3 O7 113.6(3) 2_655 3_665 ?
O7 P3 O7 113.6(3) . 2_655 ?
O7 P3 O7 113.6(3) . 3_665 ?
P1 O1 In1 136.9(4) . . ?
P1 O2 In2 133.8(4) . . ?
P1 O3 In3 136.8(4) . . ?
P2 O4 In1 136.2(4) . . ?
P2 O5 In1 132.2(4) . 3_665 ?
P2 O6 In1 136.0(5) . 7_656 ?
P3 O7 In1 149.1(6) . . ?
In1 O8 H8A 111.9 . . ?
In1 O8 H8B 112.3 . . ?
H8A O8 H8B 106.7 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.242 0.214 0.250 506.1 88.4 ?
2 -0.322 -0.856 0.750 506.1 93.4 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.842
_oxdiff_exptl_absorpt_empirical_full_min 0.601
####################################################################### 
# 
# 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_1_CCDC1
_database_code_depnum_ccdc_archive 'CCDC 2032250'
loop_
_audit_author_name
_audit_author_address
'Zhien Lin'
;Sichuan University
China
;
_audit_update_record             
;
2020-09-16 deposited with the CCDC.	2020-10-02 downloaded from the CCDC.
;
_audit_creation_date             2020-09-14
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(H52 In18 O114 P34)'
_chemical_formula_sum            'C22.50 H90.50 In9 N4.50 O68.50 P17'
_chemical_formula_weight         3080.36
_chemical_melting_point          ?
_chemical_oxdiff_formula         'In18  O114  P34  '
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'
In In 0.0822 5.0449 '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'

_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      trigonal
_space_group_IT_number           163
_space_group_name_H-M_alt        'P -3 1 c'
_space_group_name_Hall           '-P 3 2c'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-y, -x, -z+1/2'
'-x+y, y, -z+1/2'
'x, x-y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'y, x, z-1/2'
'x-y, -y, z-1/2'
'-x, -x+y, z-1/2'

_cell_length_a                   13.80944(16)
_cell_length_b                   13.80944(16)
_cell_length_c                   28.5199(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     4710.12(12)
_cell_formula_units_Z            2.00004
_cell_measurement_reflns_used    7036
_cell_measurement_temperature    293.0(4)
_cell_measurement_theta_max      71.6850
_cell_measurement_theta_min      3.9940
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    21.004
_exptl_absorpt_correction_T_max  0.259
_exptl_absorpt_correction_T_min  0.007
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.172
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             3002
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
9 -5 -2 0.1881
-8 8 1 0.1645
3 -9 0 0.2147
1 7 -1 0.3592
-6 6 10 0.1412
7 -5 -11 0.1882
1 -8 -4 0.2252
-5 -1 14 0.1897
-1 -7 -1 0.2496
2 -7 -12 0.2030
4 -3 16 0.0917
-4 4 -16 0.1634
3 -5 15 0.1028
-5 -2 -11 0.2511
2 -2 -18 0.1083
-2 2 18 0.0665
1 -1 -18 0.0931
-1 1 18 0.0494
1 -1 18 0.0250
-8 0 4 0.2637

_exptl_crystal_size_max          0.691
_exptl_crystal_size_mid          0.404
_exptl_crystal_size_min          0.143
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
8.9945 -4.9991 -2.0084 0.2203 0.9697 -0.1853
-7.9963 7.9959 1.0187 -0.2087 -0.9703 -0.2814
3.0011 -8.9931 -0.0251 0.1500 0.5401 0.8538
0.9965 6.9932 -0.9779 -0.0496 -0.1163 -0.9644
-6.0021 5.9994 10.0055 -0.6495 -0.6634 -0.1660
7.0012 -5.0009 -11.0012 0.6917 0.7207 -0.0520
1.0047 -7.9944 -4.0195 0.3396 0.2969 0.8871
-5.0021 -0.9937 13.9817 -0.7516 -0.3398 0.6358
-0.9954 -6.9938 -1.0203 0.1561 0.1024 0.9546
2.0075 -6.9978 -12.0087 0.7548 0.3056 0.6351
3.9890 -2.9943 15.9785 -0.7904 0.5709 0.0968
-3.9894 3.9935 -15.9756 0.7751 -0.5999 -0.2212
2.9913 -4.9925 14.9730 -0.7106 0.5286 0.4293
-4.9884 -1.9996 -10.9984 0.5962 -0.4847 0.6383
2.0085 -2.0038 -17.9884 0.9982 0.1191 -0.0162
-2.0085 2.0038 17.9884 -0.9982 -0.1191 0.0162
1.0090 -1.0043 -17.9860 0.9788 -0.0030 -0.0520
-1.0090 1.0043 17.9860 -0.9788 0.0030 0.0520
0.9899 -0.9946 17.9811 -0.9399 0.2473 0.1236
-7.9943 0.0037 3.9923 -0.2463 -0.7179 0.7285

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0755
_diffrn_reflns_av_unetI/netI     0.0394
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15776
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.035
_diffrn_reflns_theta_max         67.035
_diffrn_reflns_theta_min         3.696
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      293.0(4)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -89.00   0.00   1.00    4.11    --  -36.42 123.00  32.00   89
  2  ω    -55.00  33.00   1.00    4.11    --  -36.42  38.00-120.00   88
  3  ω     20.00 104.00   1.00    4.11    --   36.42  57.00-150.00   84
  4  ω    100.00 176.00   1.00   16.44    --  106.21 111.00 -60.00   76
  5  ω     88.00 173.00   1.00   16.44    --  106.21  61.00 -30.00   85
  6  ω     85.00 176.00   1.00   16.44    --  106.21  30.00  90.00   91
  7  ω     36.00 113.00   1.00   16.44    --  106.21-111.00  30.00   77
  8  ω     39.00 125.00   1.00   16.44    --  106.21 -62.00  18.00   86
  9  ω     10.00 104.00   1.00    4.11    --   36.42  77.00  90.00   94
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0041638000
_diffrn_orient_matrix_UB_12      -0.0151375000
_diffrn_orient_matrix_UB_13      -0.0533398000
_diffrn_orient_matrix_UB_21      0.0932907000
_diffrn_orient_matrix_UB_22      -0.0289437000
_diffrn_orient_matrix_UB_23      0.0070175000
_diffrn_orient_matrix_UB_31      -0.0887540000
_diffrn_orient_matrix_UB_32      -0.1245728000
_diffrn_orient_matrix_UB_33      0.0048674000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2680
_reflns_number_total             2823
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_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)'
_refine_diff_density_max         2.285
_refine_diff_density_min         -1.212
_refine_diff_density_rms         0.202
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     128
_refine_ls_number_reflns         2823
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0591
_refine_ls_restrained_S_all      1.087
_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)+(0.0904P)²+37.8306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1605
_refine_ls_wR_factor_ref         0.1619
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups, All P(H) groups
2. Rigid bond restraints
 O9, P4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Riding coordinates:
 P1(H1), P2(H2), P3(H3)
4.b Rotating group:
 O10(H10A,H10B)
;
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     dual
_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 0.70632(4) 0.14471(4) 0.47485(2) 0.0313(2) Uani 1 1 d . . . . .
In2 In 1.0000 0.0000 0.5000 0.0235(3) Uani 1 6 d S T P . .
In3 In 1.0000 0.0000 0.33620(3) 0.0332(3) Uani 1 3 d S T P . .
P1 P 0.49350(16) 0.12404(15) 0.53823(7) 0.0285(4) Uani 1 1 d . . . . .
H1 H 0.4971 0.1799 0.5756 0.043 Uiso 1 1 d R . . . .
P2 P 0.6667 0.3333 0.40843(14) 0.0368(8) Uani 1 3 d S T P . .
H2 H 0.6667 0.3333 0.3628 0.055 Uiso 1 3 d RS T P . .
P3 P 0.83561(16) 0.02686(17) 0.41666(7) 0.0294(4) Uani 1 1 d . . . . .
H3 H 0.7513 -0.0586 0.3969 0.044 Uiso 1 1 d R . . . .
P4 P 0.8015(4) -0.0993(2) 0.2500 0.108(3) Uani 1 2 d S TU P . .
O1 O 0.6151(5) 0.1701(5) 0.5282(2) 0.0417(14) Uani 1 1 d . . . . .
O2 O 0.4339(5) 0.0027(5) 0.5509(2) 0.0413(14) Uani 1 1 d . . . . .
O3 O 0.4328(6) 0.1454(5) 0.4982(3) 0.0483(17) Uani 1 1 d . . . . .
O4 O 0.6790(7) 0.2369(6) 0.4224(3) 0.0553(18) Uani 1 1 d . . . . .
O5 O 0.8203(5) 0.1230(5) 0.4313(2) 0.0386(13) Uani 1 1 d . . . . .
O6 O 0.8579(5) -0.0290(5) 0.45789(19) 0.0334(12) Uani 1 1 d . . . . .
O7 O 0.9203(6) 0.0668(6) 0.3787(2) 0.0444(15) Uani 1 1 d . . . . .
O8 O 0.8552(7) -0.0928(8) 0.2924(3) 0.076(3) Uani 1 1 d . . . . .
O9 O 0.6905(19) -0.1548(9) 0.2500 0.177(10) Uani 1 2 d S TU P . .
O10 O 0.7441(5) 0.0525(5) 0.5301(2) 0.0348(12) Uani 1 1 d . . . . .
H10A H 0.6849 -0.0100 0.5364 0.052 Uiso 1 1 d GR . . . .
H10B H 0.7601 0.0886 0.5562 0.052 Uiso 1 1 d GR . . . .


_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 2.113(6) . ?
In1 O2 2.119(6) 7_656 ?
In1 O3 2.117(6) 2_655 ?
In1 O4 2.116(7) . ?
In1 O5 2.139(6) . ?
In1 O10 2.246(5) . ?
In2 O6 2.161(5) 7_756 ?
In2 O6 2.161(5) . ?
In2 O6 2.161(5) 3_765 ?
In2 O6 2.161(5) 8_666 ?
In2 O6 2.161(5) 2_645 ?
In2 O6 2.161(5) 9_546 ?
In3 O7 2.133(6) . ?
In3 O7 2.133(6) 3_765 ?
In3 O7 2.133(6) 2_645 ?
In3 O8 2.154(7) . ?
In3 O8 2.154(7) 2_645 ?
In3 O8 2.154(7) 3_765 ?
P1 H1 1.3013 . ?
P1 O1 1.497(6) . ?
P1 O2 1.496(6) . ?
P1 O3 1.530(7) . ?
P2 H2 1.3002 . ?
P2 O4 1.479(6) 3_665 ?
P2 O4 1.479(7) 2_655 ?
P2 O4 1.479(6) . ?
P3 H3 1.3003 . ?
P3 O5 1.505(6) . ?
P3 O6 1.520(6) . ?
P3 O7 1.483(7) . ?
P4 O8 1.398(8) 6_545 ?
P4 O8 1.398(8) . ?
P4 O9 1.33(2) . ?
O2 In1 2.119(5) 7_656 ?
O3 In1 2.117(6) 3_665 ?
O10 H10A 0.8605 . ?
O10 H10B 0.8607 . ?

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 O2 94.3(2) . 7_656 ?
O1 In1 O3 89.9(2) . 2_655 ?
O1 In1 O4 96.2(3) . . ?
O1 In1 O5 169.1(2) . . ?
O1 In1 O10 85.2(2) . . ?
O2 In1 O5 92.7(3) 7_656 . ?
O2 In1 O10 93.3(2) 7_656 . ?
O3 In1 O2 175.4(3) 2_655 7_656 ?
O3 In1 O5 82.9(2) 2_655 . ?
O3 In1 O10 85.2(3) 2_655 . ?
O4 In1 O2 88.9(3) . 7_656 ?
O4 In1 O3 92.5(3) . 2_655 ?
O4 In1 O5 92.3(3) . . ?
O4 In1 O10 177.3(3) . . ?
O5 In1 O10 86.1(2) . . ?
O6 In2 O6 92.1(2) 7_756 8_666 ?
O6 In2 O6 180.0 9_546 3_765 ?
O6 In2 O6 87.9(2) 9_546 . ?
O6 In2 O6 87.9(2) 7_756 2_645 ?
O6 In2 O6 87.9(2) 8_666 . ?
O6 In2 O6 180.0(2) 8_666 2_645 ?
O6 In2 O6 92.1(2) 2_645 3_765 ?
O6 In2 O6 92.1(2) 7_756 9_546 ?
O6 In2 O6 180.0 7_756 . ?
O6 In2 O6 92.1(2) 8_666 9_546 ?
O6 In2 O6 92.1(2) 2_645 . ?
O6 In2 O6 87.9(2) 7_756 3_765 ?
O6 In2 O6 92.1(2) 3_765 . ?
O6 In2 O6 87.9(2) 8_666 3_765 ?
O6 In2 O6 87.9(2) 2_645 9_546 ?
O7 In3 O7 90.9(2) . 3_765 ?
O7 In3 O7 90.9(2) . 2_645 ?
O7 In3 O7 90.9(2) 3_765 2_645 ?
O7 In3 O8 93.5(4) . . ?
O7 In3 O8 93.5(3) 2_645 2_645 ?
O7 In3 O8 174.8(4) . 2_645 ?
O7 In3 O8 174.8(4) 3_765 . ?
O7 In3 O8 86.1(3) . 3_765 ?
O7 In3 O8 86.1(3) 3_765 2_645 ?
O7 In3 O8 93.5(4) 3_765 3_765 ?
O7 In3 O8 174.8(4) 2_645 3_765 ?
O7 In3 O8 86.1(3) 2_645 . ?
O8 In3 O8 89.8(3) 3_765 2_645 ?
O8 In3 O8 89.8(3) . 2_645 ?
O8 In3 O8 89.8(3) 3_765 . ?
O1 P1 H1 101.7 . . ?
O1 P1 O3 112.5(4) . . ?
O2 P1 H1 107.6 . . ?
O2 P1 O1 113.3(4) . . ?
O2 P1 O3 110.4(3) . . ?
O3 P1 H1 111.0 . . ?
O4 P2 H2 105.7 . . ?
O4 P2 H2 105.7 3_665 . ?
O4 P2 H2 105.7 2_655 . ?
O4 P2 O4 113.0(3) . 2_655 ?
O4 P2 O4 113.0(3) . 3_665 ?
O4 P2 O4 113.0(3) 2_655 3_665 ?
O5 P3 H3 117.7 . . ?
O5 P3 O6 112.7(3) . . ?
O6 P3 H3 101.0 . . ?
O7 P3 H3 101.7 . . ?
O7 P3 O5 107.9(4) . . ?
O7 P3 O6 115.6(3) . . ?
O8 P4 O8 125.3(8) 6_545 . ?
O9 P4 O8 117.3(4) . . ?
O9 P4 O8 117.3(4) . 6_545 ?
P1 O1 In1 134.6(4) . . ?
P1 O2 In1 135.9(4) . 7_656 ?
P1 O3 In1 131.5(4) . 3_665 ?
P2 O4 In1 150.2(5) . . ?
P3 O5 In1 136.3(4) . . ?
P3 O6 In2 137.0(4) . . ?
P3 O7 In3 137.3(4) . . ?
P4 O8 In3 147.6(6) . . ?
In1 O10 H10A 110.0 . . ?
In1 O10 H10B 110.0 . . ?
H10A O10 H10B 103.9 . . ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 -0.739 -0.984 0.250 1190.5 426.2 ?
2 -0.704 -0.694 0.750 1190.5 424.2 ?

_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.849
_oxdiff_exptl_absorpt_empirical_full_min 0.661
