# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# 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_GaPO_c5_p6
_database_code_depnum_ccdc_archive 'CCDC 1888652'
_audit_update_record             
;
2019-01-03 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2016/6
_shelx_SHELXL_version_number     2016/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'Ga2 H12 O12 P6'
_chemical_formula_sum            'Ga2 H12 O12 P6'
_chemical_formula_weight         529.36

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0018 0.0018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.0349 0.0308 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2724 0.6060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/n'
_space_group_name_Hall           '-P 2yn'

_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.
;

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

_cell_length_a                   11.3584(6)
_cell_length_b                   11.10520(10)
_cell_length_c                   11.3265(19)
_cell_angle_alpha                90
_cell_angle_beta                 107.683(12)
_cell_angle_gamma                90
_cell_volume                     1361.2(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    2212
_cell_measurement_theta_min      2.1180
_cell_measurement_theta_max      21.2450

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.583
_exptl_crystal_F_000             1040
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    1.044
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.78969
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_pressure         '1.33 GPa'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.41112
_diffrn_radiation_type           synchrotron
_diffrn_source                   synchrotron
_diffrn_measurement_device_type  'ID15B beamline, ESRF'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 7
_diffrn_reflns_number            4568
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_av_R_equivalents  0.0279
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_theta_min         1.667
_diffrn_reflns_theta_max         22.033
_diffrn_reflns_theta_full        14.281
_diffrn_measured_fraction_theta_max 0.249
_diffrn_measured_fraction_theta_full 0.413
_diffrn_reflns_Laue_measured_fraction_max 0.249
_diffrn_reflns_Laue_measured_fraction_full 0.413
_diffrn_reflns_point_group_measured_fraction_max 0.249
_diffrn_reflns_point_group_measured_fraction_full 0.413
_reflns_number_total             2156
_reflns_number_gt                1925
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0321P)²+0.6735P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   difmap
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2156
_refine_ls_number_parameters     217
_refine_ls_number_restraints     60
_refine_ls_R_factor_all          0.0315
_refine_ls_R_factor_gt           0.0274
_refine_ls_wR_factor_ref         0.0761
_refine_ls_wR_factor_gt          0.0697
_refine_ls_goodness_of_fit_ref   1.107
_refine_ls_restrained_S_all      1.096
_refine_ls_shift/su_max          0.002
_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_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 0.75640(4) 0.74125(2) 0.19158(8) 0.0177(4) Uani 1 1 d . . . . .
Ga2 Ga 0.74996(4) 0.73031(2) 0.69584(7) 0.0167(4) Uani 1 1 d . . . . .
P1 P 0.46993(10) 0.68269(6) 0.56781(19) 0.0212(9) Uani 1 1 d D U . . .
H1 H 0.467(4) 0.753(3) 0.473(6) 0.025 Uiso 1 1 d D U . . .
H1B H 0.409(4) 0.589(3) 0.515(7) 0.025 Uiso 1 1 d D U . . .
P2 P 0.50392(11) 0.63556(6) 0.2148(2) 0.0306(10) Uani 1 1 d D U . . .
H2 H 0.546(5) 0.528(3) 0.260(8) 0.037 Uiso 1 1 d D U . . .
H2B H 0.465(4) 0.595(4) 0.095(5) 0.037 Uiso 1 1 d D U . . .
P3 P 0.67642(10) 1.00760(5) 0.64237(18) 0.0221(8) Uani 1 1 d D U . . .
H3 H 0.787(5) 1.023(3) 0.641(8) 0.027 Uiso 1 1 d D U . . .
H3B H 0.597(4) 1.058(3) 0.549(6) 0.027 Uiso 1 1 d D U . . .
P4 P 0.71139(12) 0.96450(6) 0.3377(2) 0.0248(10) Uani 1 1 d D U . . .
H4 H 0.703(5) 0.903(3) 0.438(6) 0.030 Uiso 1 1 d D U . . .
H4B H 0.601(4) 0.983(3) 0.271(6) 0.030 Uiso 1 1 d D U . . .
P5 P 0.82276(11) 0.62304(6) 0.46726(19) 0.0226(9) Uani 1 1 d D U . . .
H5 H 0.751(5) 0.536(3) 0.459(7) 0.027 Uiso 1 1 d D U . . .
H5B H 0.933(4) 0.576(3) 0.543(6) 0.027 Uiso 1 1 d D U . . .
P6 P 0.62269(11) 0.77637(6) 0.9056(2) 0.0182(9) Uani 1 1 d D U . . .
H6 H 0.539(4) 0.689(3) 0.878(7) 0.022 Uiso 1 1 d D U . . .
H6B H 0.557(4) 0.865(3) 0.833(6) 0.022 Uiso 1 1 d D U . . .
O1 O 0.4097(3) 0.7453(2) 0.6523(6) 0.029(3) Uani 1 1 d D U . . .
O2 O 0.5986(3) 0.63611(15) 0.6327(5) 0.027(3) Uani 1 1 d D U . . .
O3 O 0.3968(3) 0.66920(18) 0.2597(5) 0.025(3) Uani 1 1 d D U . . .
O4 O 0.6057(3) 0.72560(19) 0.2421(6) 0.033(3) Uani 1 1 d D U . . .
O5 O 0.6471(3) 0.87494(14) 0.6424(5) 0.017(2) Uani 1 1 d D U . . .
O6 O 0.6615(3) 1.07778(16) 0.7514(5) 0.026(2) Uani 1 1 d D U . . .
O7 O 0.7708(3) 1.08363(17) 0.3896(6) 0.026(3) Uani 1 1 d D U . . .
O8 O 0.7843(3) 0.89771(17) 0.2680(6) 0.029(3) Uani 1 1 d D U . . .
O9 O 0.7871(4) 0.72214(18) 0.5414(6) 0.033(3) Uani 1 1 d D U . . .
O10 O 0.8485(3) 0.6625(2) 0.3502(6) 0.026(3) Uani 1 1 d D U . . .
O11 O 0.6575(4) 0.81688(19) 1.0389(6) 0.022(2) Uani 1 1 d D U . . .
O12 O 0.7318(3) 0.74337(18) 0.8619(6) 0.021(3) Uani 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
Ga1 O8 1.924(3) . ?
Ga1 O1 1.929(2) 4_675 ?
Ga1 O11 1.944(6) 1_554 ?
Ga1 O7 1.957(3) 2_645 ?
Ga1 O4 1.970(2) . ?
Ga1 O10 1.986(6) . ?
Ga2 O9 1.922(5) . ?
Ga2 O2 1.953(3) . ?
Ga2 O3 1.953(3) 4_676 ?
Ga2 O12 1.959(5) . ?
Ga2 O6 1.968(3) 2_646 ?
Ga2 O5 1.970(3) . ?
P1 O1 1.505(4) . ?
P1 O2 1.514(4) . ?
P1 H1 1.32(5) . ?
P1 H1B 1.29(4) . ?
P2 O4 1.489(3) . ?
P2 O3 1.502(2) . ?
P2 H2 1.33(4) . ?
P2 H2B 1.37(5) . ?
P3 O5 1.5104(17) . ?
P3 O6 1.513(4) . ?
P3 H3 1.28(4) . ?
P3 H3B 1.29(5) . ?
P4 O8 1.502(3) . ?
P4 O7 1.520(3) . ?
P4 H4 1.35(5) . ?
P4 H4B 1.27(5) . ?
P5 O10 1.507(5) . ?
P5 O9 1.512(4) . ?
P5 H5 1.25(3) . ?
P5 H5B 1.38(5) . ?
P6 O11 1.509(7) . ?
P6 O12 1.513(2) . ?
P6 H6 1.33(4) . ?
P6 H6B 1.35(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O8 Ga1 O1 89.84(13) . 4_675 ?
O8 Ga1 O11 88.9(2) . 1_554 ?
O1 Ga1 O11 94.6(2) 4_675 1_554 ?
O8 Ga1 O7 178.59(18) . 2_645 ?
O1 Ga1 O7 89.17(13) 4_675 2_645 ?
O11 Ga1 O7 90.1(2) 1_554 2_645 ?
O8 Ga1 O4 89.31(11) . . ?
O1 Ga1 O4 176.6(3) 4_675 . ?
O11 Ga1 O4 88.76(19) 1_554 . ?
O7 Ga1 O4 91.74(12) 2_645 . ?
O8 Ga1 O10 91.2(2) . . ?
O1 Ga1 O10 88.8(2) 4_675 . ?
O11 Ga1 O10 176.67(9) 1_554 . ?
O7 Ga1 O10 89.7(2) 2_645 . ?
O4 Ga1 O10 87.92(19) . . ?
O9 Ga2 O2 93.1(2) . . ?
O9 Ga2 O3 88.0(2) . 4_676 ?
O2 Ga2 O3 177.40(8) . 4_676 ?
O9 Ga2 O12 173.50(18) . . ?
O2 Ga2 O12 93.07(18) . . ?
O3 Ga2 O12 85.93(18) 4_676 . ?
O9 Ga2 O6 90.13(16) . 2_646 ?
O2 Ga2 O6 87.82(13) . 2_646 ?
O3 Ga2 O6 94.55(13) 4_676 2_646 ?
O12 Ga2 O6 88.02(16) . 2_646 ?
O9 Ga2 O5 91.87(16) . . ?
O2 Ga2 O5 87.16(12) . . ?
O3 Ga2 O5 90.44(12) 4_676 . ?
O12 Ga2 O5 90.51(16) . . ?
O6 Ga2 O5 174.69(9) 2_646 . ?
O1 P1 O2 114.1(3) . . ?
O1 P1 H1 109.8(17) . . ?
O2 P1 H1 112.2(19) . . ?
O1 P1 H1B 112.7(18) . . ?
O2 P1 H1B 104(2) . . ?
H1 P1 H1B 103(4) . . ?
O4 P2 O3 114.91(18) . . ?
O4 P2 H2 111(2) . . ?
O3 P2 H2 109(2) . . ?
O4 P2 H2B 115.2(18) . . ?
O3 P2 H2B 111.3(19) . . ?
H2 P2 H2B 93(3) . . ?
O5 P3 O6 115.0(2) . . ?
O5 P3 H3 110.4(15) . . ?
O6 P3 H3 107(3) . . ?
O5 P3 H3B 108.7(18) . . ?
O6 P3 H3B 103(2) . . ?
H3 P3 H3B 112(4) . . ?
O8 P4 O7 112.47(15) . . ?
O8 P4 H4 112.6(16) . . ?
O7 P4 H4 104(2) . . ?
O8 P4 H4B 112(2) . . ?
O7 P4 H4B 109.2(17) . . ?
H4 P4 H4B 106(3) . . ?
O10 P5 O9 115.7(2) . . ?
O10 P5 H5 117(3) . . ?
O9 P5 H5 109(2) . . ?
O10 P5 H5B 106(2) . . ?
O9 P5 H5B 106(2) . . ?
H5 P5 H5B 102(3) . . ?
O11 P6 O12 114.1(3) . . ?
O11 P6 H6 114(3) . . ?
O12 P6 H6 110.5(17) . . ?
O11 P6 H6B 109(3) . . ?
O12 P6 H6B 109.5(18) . . ?
H6 P6 H6B 99(3) . . ?
P1 O1 Ga1 143.0(3) . 4_576 ?
P1 O2 Ga2 127.41(11) . . ?
P2 O3 Ga2 134.9(3) . 4_575 ?
P2 O4 Ga1 133.4(2) . . ?
P3 O5 Ga2 133.3(2) . . ?
P3 O6 Ga2 121.16(14) . 2_656 ?
P4 O7 Ga1 127.5(4) . 2_655 ?
P4 O8 Ga1 129.84(13) . . ?
P5 O9 Ga2 135.2(2) . . ?
P5 O10 Ga1 137.24(17) . . ?
P6 O11 Ga1 131.81(13) . 1_556 ?
P6 O12 Ga2 131.9(3) . . ?

_refine_diff_density_max         0.412
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.072



# start Validation Reply Form
_vrf_PLAT029_GaPO_c5_p6          
;
PROBLEM: _diffrn_measured_fraction_theta_full value Low .      0.413 Why?  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT911_GaPO_c5_p6          
;
PROBLEM: Missing FCF Refl Between Thmin & STh/L=    0.600       1417 Report  
RESPONSE: The use of a diamond anvil cell significantly reduces the fraction
of reciprocal space from which reflection data can be acquired.
;
_vrf_PLAT088_GaPO_c5_p6          
;
PROBLEM: Poor Data / Parameter Ratio ....................       9.94 Note  
RESPONSE: There are no suitable AFIX contraints for the hydrogen atoms of the
O2PH2 group, and so additional positional parameters are present for the 12 
hydrogen atoms. Distance and angle restraints are used to maintain sensible 
H atom position refinement.
;
_vrf_PLAT430_GaPO_c5_p6          
;
PROBLEM: Short Inter D...A Contact  O3       ..O6       .       2.88 Ang.  
RESPONSE: These O-O distances are from the GaO6 octahedron and may be shorter
than expected as the structure is at high pressure. 
;
_vrf_PLAT913_GaPO_c5_p6          
;
PROBLEM: Missing # of Very Strong Reflections in FCF ....         14 Note  
RESPONSE: Overexposed reflections were omitted from the refinement.
;
# end Validation Reply Form
