# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2014

####################################################################### 
# 
# 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_JU102
_audit_block_doi                 10.5517/cc13hk38
_database_code_depnum_ccdc_archive 'CCDC 1027839'
_audit_update_record             
;
2014-10-07 deposited with the CCDC.
2014-12-15 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2013
_chemical_name_systematic        JU102
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'Al H5 Mg O10 P2'
_chemical_formula_weight         278.27

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Al Al 0.0645 0.0514 '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'
Mg Mg 0.0486 0.0363 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_H-M_alt        'P 21'
_space_group_name_Hall           'P 2yb'

_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, y+1/2, -z'

_cell_length_a                   5.0119(11)
_cell_length_b                   7.7690(17)
_cell_length_c                   9.995(2)
_cell_angle_alpha                90
_cell_angle_beta                 102.595(3)
_cell_angle_gamma                90
_cell_volume                     379.81(14)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       flake
_exptl_crystal_colour            colorless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.433
_exptl_crystal_F_000             280
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.210
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.180
_exptl_absorpt_coefficient_mu    0.812
_shelx_estimated_absorpt_T_min   0.848
_shelx_estimated_absorpt_T_max   0.868
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_T_max  0.8677
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            2795
_diffrn_reflns_av_unetI/netI     0.0278
_diffrn_reflns_av_R_equivalents  0.0159
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         2.088
_diffrn_reflns_theta_max         28.328
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measured_fraction_theta_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             1689
_reflns_number_gt                1648
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.869
_reflns_Friedel_fraction_max     0.999
_reflns_Friedel_fraction_full    0.998

_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    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 Refined as a 2-component inversion twin.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0262P)²+0.2733P] 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_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   -0.02(16)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         1689
_refine_ls_number_parameters     143
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0252
_refine_ls_R_factor_gt           0.0243
_refine_ls_wR_factor_ref         0.0623
_refine_ls_wR_factor_gt          0.0616
_refine_ls_goodness_of_fit_ref   1.114
_refine_ls_restrained_S_all      1.114
_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_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 0.7267(2) 0.61885(13) 0.62590(10) 0.0107(2) Uani 1 1 d . . . . .
Mg1 Mg 0.4823(2) 0.67039(16) 1.15089(11) 0.0110(2) Uani 1 1 d . . . . .
P1 P 0.19540(17) 0.40281(12) 0.57946(8) 0.00951(18) Uani 1 1 d . . . . .
P2 P 0.85672(17) 0.55499(11) 0.93496(9) 0.00980(18) Uani 1 1 d . . . . .
O1 O 0.8851(5) 0.6387(4) 0.7982(2) 0.0167(6) Uani 1 1 d . . . . .
O2 O 0.3890(5) 0.5574(4) 0.6112(3) 0.0153(5) Uani 1 1 d . . . . .
O3 O 0.9006(5) 0.4730(3) 0.5416(3) 0.0130(5) Uani 1 1 d . . . . .
O4 O 0.7533(5) 0.8205(3) 0.5533(3) 0.0142(5) Uani 1 1 d . . . . .
O5 O 0.7358(5) 0.6861(4) 1.0165(3) 0.0136(5) Uani 1 1 d . . . . .
O6 O 0.7096(5) 0.3875(4) 0.9169(3) 0.0183(6) Uani 1 1 d . . . . .
O7 O 0.2270(5) 0.2783(4) 0.6965(3) 0.0152(5) Uani 1 1 d . . . . .
O8 O 1.1654(5) 0.5185(3) 1.0137(3) 0.0137(5) Uani 1 1 d D . . . .
H8 H 1.207(9) 0.403(3) 0.990(5) 0.021 Uiso 1 1 d D U . . .
O9 O 0.6518(6) 0.4242(4) 1.2242(3) 0.0244(7) Uani 1 1 d D . . . .
H9A H 0.704(11) 0.345(6) 1.162(4) 0.037 Uiso 1 1 d D U . . .
H9B H 0.743(9) 0.423(8) 1.3192(19) 0.037 Uiso 1 1 d D U . . .
O10 O 0.2520(6) 0.6323(4) 1.2928(3) 0.0191(6) Uani 1 1 d D . . . .
H10A H 0.075(6) 0.684(7) 1.288(5) 0.029 Uiso 1 1 d D U . . .
H10B H 0.248(10) 0.521(3) 1.334(5) 0.029 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
Al1 O2 1.734(3) . ?
Al1 O1 1.739(3) . ?
Al1 O4 1.744(3) . ?
Al1 O3 1.753(3) . ?
Mg1 O6 1.986(3) 2_657 ?
Mg1 O10 2.036(3) . ?
Mg1 O5 2.044(3) . ?
Mg1 O7 2.045(3) 2_657 ?
Mg1 O9 2.155(3) . ?
Mg1 O8 2.201(3) 1_455 ?
P1 O7 1.499(3) . ?
P1 O2 1.533(3) . ?
P1 O3 1.542(3) 1_455 ?
P1 O4 1.544(3) 2_646 ?
P2 O6 1.487(3) . ?
P2 O5 1.512(3) . ?
P2 O1 1.548(3) . ?
P2 O8 1.601(3) . ?
O3 P1 1.542(3) 1_655 ?
O4 P1 1.544(3) 2_656 ?
O6 Mg1 1.986(3) 2_647 ?
O7 Mg1 2.045(3) 2_647 ?
O8 Mg1 2.201(3) 1_655 ?
O8 H8 0.962(14) . ?
O9 H9A 0.955(14) . ?
O9 H9B 0.960(14) . ?
O10 H10A 0.967(14) . ?
O10 H10B 0.956(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
O2 Al1 O1 109.53(13) . . ?
O2 Al1 O4 111.95(14) . . ?
O1 Al1 O4 105.84(14) . . ?
O2 Al1 O3 111.09(13) . . ?
O1 Al1 O3 111.47(14) . . ?
O4 Al1 O3 106.85(13) . . ?
O6 Mg1 O10 93.15(12) 2_657 . ?
O6 Mg1 O5 92.83(12) 2_657 . ?
O10 Mg1 O5 174.01(13) . . ?
O6 Mg1 O7 96.85(12) 2_657 2_657 ?
O10 Mg1 O7 87.71(12) . 2_657 ?
O5 Mg1 O7 91.25(11) . 2_657 ?
O6 Mg1 O9 174.39(14) 2_657 . ?
O10 Mg1 O9 82.83(13) . . ?
O5 Mg1 O9 91.23(12) . . ?
O7 Mg1 O9 86.93(12) 2_657 . ?
O6 Mg1 O8 90.74(12) 2_657 1_455 ?
O10 Mg1 O8 85.08(12) . 1_455 ?
O5 Mg1 O8 95.18(11) . 1_455 ?
O7 Mg1 O8 169.80(12) 2_657 1_455 ?
O9 Mg1 O8 85.03(12) . 1_455 ?
O7 P1 O2 112.91(15) . . ?
O7 P1 O3 110.60(15) . 1_455 ?
O2 P1 O3 107.64(16) . 1_455 ?
O7 P1 O4 113.23(16) . 2_646 ?
O2 P1 O4 106.60(14) . 2_646 ?
O3 P1 O4 105.41(15) 1_455 2_646 ?
O6 P2 O5 114.13(16) . . ?
O6 P2 O1 113.49(16) . . ?
O5 P2 O1 108.54(15) . . ?
O6 P2 O8 107.77(15) . . ?
O5 P2 O8 108.21(14) . . ?
O1 P2 O8 104.10(15) . . ?
P2 O1 Al1 136.69(18) . . ?
P1 O2 Al1 142.69(19) . . ?
P1 O3 Al1 131.33(17) 1_655 . ?
P1 O4 Al1 140.50(18) 2_656 . ?
P2 O5 Mg1 133.93(17) . . ?
P2 O6 Mg1 167.17(19) . 2_647 ?
P1 O7 Mg1 141.55(17) . 2_647 ?
P2 O8 Mg1 134.43(16) . 1_655 ?
P2 O8 H8 106(3) . . ?
Mg1 O8 H8 119(3) 1_655 . ?
Mg1 O9 H9A 119(3) . . ?
Mg1 O9 H9B 114(4) . . ?
H9A O9 H9B 120(5) . . ?
Mg1 O10 H10A 124(3) . . ?
Mg1 O10 H10B 120(3) . . ?
H10A O10 H10B 107(4) . . ?

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 H8 O5 0.962(14) 1.713(18) 2.659(4) 167(4) 2_747
O9 H9A O1 0.955(14) 2.57(4) 3.254(4) 129(4) 2_747
O9 H9A O6 0.955(14) 2.47(4) 3.161(4) 129(4) .
O9 H9B O3 0.960(14) 2.225(19) 3.168(4) 167(5) 1_556
O10 H10A O7 0.967(14) 1.717(16) 2.678(4) 172(4) 2_557
O10 H10B O4 0.956(14) 1.927(16) 2.873(4) 170(5) 2_647

_refine_diff_density_max         0.369
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.070

_shelxl_version_number           2013-4

