# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

####################################################################### 
# 
# 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. 
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#######################################################################

data_mo_21216b
_database_code_depnum_ccdc_archive 'CCDC 1000500'
_audit_update_record             
;
2015-01-08 deposited with the CCDC.
2015-01-09 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        InPCF-1
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C14 H7 In O7 P, H3 O, 2(H2 O)'
_chemical_formula_sum            'C14 H11 In O10 P'
_chemical_formula_weight         485.02

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'
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'
In In -0.7276 1.3100 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Tetragonal
_symmetry_space_group_name_H-M   P4/mnc
_space_group_name_Hall           '-P 4 2n'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'x-1/2, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z-1/2'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'

_cell_length_a                   23.474(3)
_cell_length_b                   23.474(3)
_cell_length_c                   6.6926(9)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     3687.9(8)
_cell_formula_units_Z            8
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    2191
_cell_measurement_theta_min      2.45
_cell_measurement_theta_max      25.14

_exptl_crystal_description       rod
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.747
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8155
_exptl_absorpt_correction_T_max  0.8951
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            21607
_diffrn_reflns_av_R_equivalents  0.1108
_diffrn_reflns_av_sigmaI/netI    0.0441
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_theta_min         1.23
_diffrn_reflns_theta_max         25.01
_reflns_number_total             1778
_reflns_number_gt                1362
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0805P)²+2.4258P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         1778
_refine_ls_number_parameters     157
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0462
_refine_ls_wR_factor_ref         0.1432
_refine_ls_wR_factor_gt          0.1175
_refine_ls_goodness_of_fit_ref   1.175
_refine_ls_restrained_S_all      1.175
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
In1 In 0.12300(3) 0.27548(3) 1.0000 0.0196(3) Uani 1 2 d S . .
P1 P 0.20059(11) 0.39524(10) 1.0000 0.0206(6) Uani 1 2 d S . .
C3 C 0.1237(5) 0.4850(5) 1.0000 0.079(6) Uani 1 2 d S . .
H3 H 0.0957 0.4570 1.0000 0.094 Uiso 1 2 calc SR . .
O2 O 0.1454(3) 0.3609(3) 1.0000 0.0275(15) Uani 1 2 d S . .
O6 O 0.2182(3) 0.2519(3) 1.0000 0.0340(18) Uani 1 2 d S . .
O5 O 0.1542(3) 0.1847(3) 1.0000 0.0308(17) Uani 1 2 d S . .
C2 C 0.1797(4) 0.4699(4) 1.0000 0.026(2) Uani 1 2 d S . .
C13 C 0.2057(5) 0.1999(4) 1.0000 0.028(2) Uani 1 2 d S . .
O4 O 0.0210(3) 0.2155(4) 1.0000 0.057(2) Uani 1 2 d S . .
O3 O 0.0383(3) 0.3067(4) 1.0000 0.0373(19) Uani 1 2 d S . .
C6 C 0.4138(4) 0.1477(4) 1.0000 0.027(2) Uani 1 2 d S . .
C12 C 0.3085(4) 0.1714(4) 1.0000 0.028(2) Uani 1 2 d S . .
H12 H 0.3178 0.2099 1.0000 0.033 Uiso 1 2 calc SR . .
C9 C 0.2796(4) 0.0582(4) 1.0000 0.025(2) Uani 1 2 d S . .
C7 C 0.3524(4) 0.1320(4) 1.0000 0.026(2) Uani 1 2 d S . .
C10 C 0.2374(4) 0.0986(4) 1.0000 0.027(2) Uani 1 2 d S . .
H10 H 0.1993 0.0876 1.0000 0.033 Uiso 1 2 calc SR . .
C11 C 0.2521(4) 0.1562(4) 1.0000 0.025(2) Uani 1 2 d S . .
C5 C 0.4308(4) 0.2035(4) 1.0000 0.031(3) Uani 1 2 d S . .
H5 H 0.4033 0.2320 1.0000 0.037 Uiso 1 2 calc SR . .
C14 C 0.0037(5) 0.2657(6) 1.0000 0.039(3) Uani 1 2 d S . .
C1 C 0.2189(4) 0.5113(5) 1.0000 0.040(3) Uani 1 2 d S . .
H1 H 0.2573 0.5016 1.0000 0.048 Uiso 1 2 calc SR . .
C8 C 0.3365(4) 0.0743(4) 1.0000 0.026(2) Uani 1 2 d S . .
H8 H 0.3646 0.0464 1.0000 0.032 Uiso 1 2 calc SR . .
C4 C 0.1079(5) 0.5440(5) 1.0000 0.075(6) Uani 1 2 d S . .
H4 H 0.0695 0.5537 1.0000 0.090 Uiso 1 2 calc SR . .
O1 O 0.23751(19) 0.38535(19) 0.8153(7) 0.0261(11) Uani 1 1 d . . .
O7 O 0.3608(11) 0.3381(9) 1.0000 0.221(12) Uani 1 2 d S . .
O8 O 0.3519(7) 0.4045(12) 1.0000 0.283(16) Uani 1 2 d S . .
H8A H 0.3551 0.4279 1.0961 0.340 Uiso 0.50 1 d PR . .
H8B H 0.3173 0.4033 0.9635 0.340 Uiso 0.50 1 d PR . .
O9 O 0.3768(15) 0.462(2) 0.753(6) 0.44(4) Uani 0.50 1 d P . .
H9A H 0.3484 0.4667 0.6758 0.525 Uiso 0.50 1 d PR . .
H9B H 0.3669 0.4398 0.8471 0.525 Uiso 0.50 1 d PR . .


_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 O2 2.072(6) . ?
In1 O3 2.119(7) . ?
In1 O1 2.141(5) 8_556 ?
In1 O1 2.141(5) 15_666 ?
In1 O5 2.254(7) . ?
In1 O6 2.302(7) . ?
In1 C13 2.630(10) . ?
P1 O2 1.527(7) . ?
P1 O1 1.528(5) 10_557 ?
P1 O1 1.528(5) . ?
P1 C2 1.821(10) . ?
C3 C2 1.360(15) . ?
C3 C4 1.433(17) . ?
O6 C13 1.255(12) . ?
O5 C13 1.261(12) . ?
C2 C1 1.339(14) . ?
C13 C11 1.496(14) . ?
O4 C14 1.245(14) . ?
O3 C14 1.259(14) . ?
C6 C4 1.362(16) 3_655 ?
C6 C5 1.367(13) . ?
C6 C7 1.490(13) . ?
C12 C11 1.372(13) . ?
C12 C7 1.383(13) . ?
C9 C10 1.370(13) . ?
C9 C8 1.388(14) . ?
C9 C14 1.490(13) 11_557 ?
C7 C8 1.404(13) . ?
C10 C11 1.396(13) . ?
C5 C1 1.405(14) 3_655 ?
C14 C9 1.490(13) 3 ?
C1 C5 1.405(14) 11_567 ?
C4 C6 1.362(16) 11_567 ?
O1 In1 2.141(5) 15_665 ?
O7 O8 1.57(3) . ?

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
O2 In1 O3 84.5(3) . . ?
O2 In1 O1 99.27(12) . 8_556 ?
O3 In1 O1 87.90(13) . 8_556 ?
O2 In1 O1 99.27(12) . 15_666 ?
O3 In1 O1 87.90(13) . 15_666 ?
O1 In1 O1 160.5(2) 8_556 15_666 ?
O2 In1 O5 146.4(2) . . ?
O3 In1 O5 129.2(3) . . ?
O1 In1 O5 83.97(12) 8_556 . ?
O1 In1 O5 83.97(12) 15_666 . ?
O2 In1 O6 89.3(2) . . ?
O3 In1 O6 173.7(3) . . ?
O1 In1 O6 93.13(12) 8_556 . ?
O1 In1 O6 93.13(12) 15_666 . ?
O5 In1 O6 57.1(2) . . ?
O2 In1 C13 117.8(3) . . ?
O3 In1 C13 157.8(3) . . ?
O1 In1 C13 88.37(13) 8_556 . ?
O1 In1 C13 88.37(13) 15_666 . ?
O5 In1 C13 28.6(3) . . ?
O6 In1 C13 28.5(3) . . ?
O2 P1 O1 113.7(2) . 10_557 ?
O2 P1 O1 113.7(2) . . ?
O1 P1 O1 108.1(4) 10_557 . ?
O2 P1 C2 106.3(4) . . ?
O1 P1 C2 107.4(3) 10_557 . ?
O1 P1 C2 107.4(3) . . ?
C2 C3 C4 120.1(11) . . ?
P1 O2 In1 136.6(4) . . ?
C13 O6 In1 90.4(6) . . ?
C13 O5 In1 92.5(6) . . ?
C1 C2 C3 118.4(10) . . ?
C1 C2 P1 120.9(8) . . ?
C3 C2 P1 120.7(8) . . ?
O6 C13 O5 120.0(9) . . ?
O6 C13 C11 119.8(9) . . ?
O5 C13 C11 120.2(9) . . ?
O6 C13 In1 61.1(5) . . ?
O5 C13 In1 58.9(5) . . ?
C11 C13 In1 179.2(7) . . ?
C14 O3 In1 109.9(7) . . ?
C4 C6 C5 116.3(10) 3_655 . ?
C4 C6 C7 122.3(10) 3_655 . ?
C5 C6 C7 121.4(9) . . ?
C11 C12 C7 123.0(9) . . ?
C10 C9 C8 120.5(9) . . ?
C10 C9 C14 121.0(10) . 11_557 ?
C8 C9 C14 118.4(10) . 11_557 ?
C12 C7 C8 116.6(9) . . ?
C12 C7 C6 123.6(9) . . ?
C8 C7 C6 119.8(9) . . ?
C9 C10 C11 119.4(9) . . ?
C12 C11 C10 119.3(9) . . ?
C12 C11 C13 121.7(9) . . ?
C10 C11 C13 119.0(9) . . ?
C6 C5 C1 122.0(9) . 3_655 ?
O4 C14 O3 120.8(10) . . ?
O4 C14 C9 121.7(11) . 3 ?
O3 C14 C9 117.5(10) . 3 ?
C2 C1 C5 121.6(10) . 11_567 ?
C9 C8 C7 121.1(9) . . ?
C6 C4 C3 121.7(11) 11_567 . ?
P1 O1 In1 137.0(3) . 15_665 ?

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
O1 P1 O2 In1 -62.1(2) 10_557 . . . ?
O1 P1 O2 In1 62.1(2) . . . . ?
C2 P1 O2 In1 180.0 . . . . ?
O3 In1 O2 P1 180.0 . . . . ?
O1 In1 O2 P1 -93.05(13) 8_556 . . . ?
O1 In1 O2 P1 93.05(13) 15_666 . . . ?
O5 In1 O2 P1 0.0 . . . . ?
O6 In1 O2 P1 0.0 . . . . ?
C13 In1 O2 P1 0.0 . . . . ?
O2 In1 O6 C13 180.0 . . . . ?
O3 In1 O6 C13 180.0 . . . . ?
O1 In1 O6 C13 -80.76(12) 8_556 . . . ?
O1 In1 O6 C13 80.76(12) 15_666 . . . ?
O5 In1 O6 C13 0.0 . . . . ?
O2 In1 O5 C13 0.0 . . . . ?
O3 In1 O5 C13 180.0 . . . . ?
O1 In1 O5 C13 97.68(12) 8_556 . . . ?
O1 In1 O5 C13 -97.68(12) 15_666 . . . ?
O6 In1 O5 C13 0.0 . . . . ?
C4 C3 C2 C1 0.0 . . . . ?
C4 C3 C2 P1 180.0 . . . . ?
O2 P1 C2 C1 180.0 . . . . ?
O1 P1 C2 C1 58.0(2) 10_557 . . . ?
O1 P1 C2 C1 -58.0(2) . . . . ?
O2 P1 C2 C3 0.0 . . . . ?
O1 P1 C2 C3 -122.0(2) 10_557 . . . ?
O1 P1 C2 C3 122.0(2) . . . . ?
In1 O6 C13 O5 0.0 . . . . ?
In1 O6 C13 C11 180.0 . . . . ?
In1 O5 C13 O6 0.0 . . . . ?
In1 O5 C13 C11 180.0 . . . . ?
O2 In1 C13 O6 0.0 . . . . ?
O3 In1 C13 O6 180.0 . . . . ?
O1 In1 C13 O6 99.61(12) 8_556 . . . ?
O1 In1 C13 O6 -99.61(12) 15_666 . . . ?
O5 In1 C13 O6 180.0 . . . . ?
O2 In1 C13 O5 180.0 . . . . ?
O3 In1 C13 O5 0.0 . . . . ?
O1 In1 C13 O5 -80.39(12) 8_556 . . . ?
O1 In1 C13 O5 80.39(12) 15_666 . . . ?
O6 In1 C13 O5 180.0 . . . . ?
O2 In1 C13 C11 180.0 . . . . ?
O3 In1 C13 C11 0.0 . . . . ?
O1 In1 C13 C11 -80.39(12) 8_556 . . . ?
O1 In1 C13 C11 80.39(12) 15_666 . . . ?
O5 In1 C13 C11 0.0 . . . . ?
O6 In1 C13 C11 180.0 . . . . ?
O2 In1 O3 C14 180.0 . . . . ?
O1 In1 O3 C14 80.48(12) 8_556 . . . ?
O1 In1 O3 C14 -80.48(12) 15_666 . . . ?
O5 In1 O3 C14 0.0 . . . . ?
O6 In1 O3 C14 180.0 . . . . ?
C13 In1 O3 C14 0.0 . . . . ?
C11 C12 C7 C8 0.0 . . . . ?
C11 C12 C7 C6 180.0 . . . . ?
C4 C6 C7 C12 180.0 3_655 . . . ?
C5 C6 C7 C12 0.0 . . . . ?
C4 C6 C7 C8 0.0 3_655 . . . ?
C5 C6 C7 C8 180.0 . . . . ?
C8 C9 C10 C11 0.0 . . . . ?
C14 C9 C10 C11 180.0 11_557 . . . ?
C7 C12 C11 C10 0.0 . . . . ?
C7 C12 C11 C13 180.0 . . . . ?
C9 C10 C11 C12 0.0 . . . . ?
C9 C10 C11 C13 180.0 . . . . ?
O6 C13 C11 C12 0.0 . . . . ?
O5 C13 C11 C12 180.0 . . . . ?
In1 C13 C11 C12 180.0 . . . . ?
O6 C13 C11 C10 180.0 . . . . ?
O5 C13 C11 C10 0.0 . . . . ?
In1 C13 C11 C10 0.0 . . . . ?
C4 C6 C5 C1 0.0 3_655 . . 3_655 ?
C7 C6 C5 C1 180.0 . . . 3_655 ?
In1 O3 C14 O4 0.0 . . . . ?
In1 O3 C14 C9 180.0 . . . 3 ?
C3 C2 C1 C5 0.0 . . . 11_567 ?
P1 C2 C1 C5 180.0 . . . 11_567 ?
C10 C9 C8 C7 0.0 . . . . ?
C14 C9 C8 C7 180.0 11_557 . . . ?
C12 C7 C8 C9 0.0 . . . . ?
C6 C7 C8 C9 180.0 . . . . ?
C2 C3 C4 C6 0.0 . . . 11_567 ?
O2 P1 O1 In1 42.3(5) . . . 15_665 ?
O1 P1 O1 In1 169.42(14) 10_557 . . 15_665 ?
C2 P1 O1 In1 -75.0(5) . . . 15_665 ?

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
O8 H8A O9 0.85 1.39 2.21(4) 163.3 10_557
O8 H8B O1 0.85 2.16 2.991(18) 165.4 .
O9 H9A O4 0.85 1.93 2.78(3) 179.0 15_665
O9 H9B O8 0.85 1.36 2.21(4) 178.9 .

_diffrn_measured_fraction_theta_max 1.000
_diffrn_reflns_theta_full        25.01
_diffrn_measured_fraction_theta_full 1.000
_refine_diff_density_max         1.075
_refine_diff_density_min         -0.692
_refine_diff_density_rms         0.174
_exptl_crystal_recrystallization_method Hydrothermal
_exptl_crystal_preparation       Luminescent
