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

#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_JU94

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H10 Al3 Mg N O18 P4'
_chemical_formula_weight         565.24

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'
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'
Mg Mg 0.0486 0.0363 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.3675(4)
_cell_length_b                   14.9405(5)
_cell_length_c                   9.1706(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.4930(10)
_cell_angle_gamma                90.00
_cell_volume                     1675.93(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      28.37

_exptl_crystal_description       rod
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.14
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.240
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.746
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8591
_exptl_absorpt_correction_T_max  0.9027
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            12289
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_sigmaI/netI    0.0360
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         28.37
_reflns_number_total             4187
_reflns_number_gt                3468
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex 2'
_computing_cell_refinement       'Bruker SMART Apex 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0530P)²+2.3001P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4187
_refine_ls_number_parameters     271
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0364
_refine_ls_wR_factor_ref         0.1093
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_restrained_S_all      1.069
_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
Mg1 Mg 0.17502(7) 0.00546(6) 0.68007(11) 0.0145(2) Uani 1 1 d . . .
Al1 Al 0.14077(7) 0.31035(5) 0.63166(9) 0.01268(17) Uani 1 1 d . . .
Al2 Al -0.23008(6) 0.16606(5) 0.71144(9) 0.01115(17) Uani 1 1 d . . .
Al3 Al -0.43839(6) -0.17175(5) 0.54948(9) 0.01097(17) Uani 1 1 d . . .
P1 P 0.02354(5) 0.17367(5) 0.79636(8) 0.01201(15) Uani 1 1 d . . .
P2 P -0.33679(5) -0.18106(4) 0.27252(8) 0.01117(15) Uani 1 1 d . . .
P3 P -0.31216(5) 0.17794(4) 0.38467(8) 0.01071(15) Uani 1 1 d . . .
P4 P -0.25292(5) -0.03656(4) 0.66425(8) 0.01117(15) Uani 1 1 d . . .
O1 O -0.42724(16) 0.16431(15) 0.4251(2) 0.0229(5) Uani 1 1 d . . .
O2 O -0.18864(19) -0.08701(14) 0.7958(2) 0.0232(5) Uani 1 1 d . . .
O3 O -0.23331(17) 0.19449(14) 0.5277(2) 0.0197(4) Uani 1 1 d . . .
O4 O 0.05650(17) 0.10136(14) 0.6990(2) 0.0213(4) Uani 1 1 d . . .
O5 O -0.24796(16) -0.23571(14) 0.3661(2) 0.0219(5) Uani 1 1 d . . .
O6 O 0.04794(19) 0.26734(14) 0.7389(3) 0.0280(5) Uani 1 1 d . . .
O7 O -0.36725(17) -0.08007(14) 0.6310(3) 0.0247(5) Uani 1 1 d . . .
O8 O -0.37977(18) -0.23164(14) 0.1310(2) 0.0228(5) Uani 1 1 d . . .
O9 O -0.19299(18) -0.03411(15) 0.5354(2) 0.0232(5) Uani 1 1 d . . .
O10 O -0.28062(17) 0.09961(14) 0.3000(2) 0.0221(5) Uani 1 1 d . . .
O11 O -0.43246(16) -0.17332(14) 0.3618(2) 0.0194(4) Uani 1 1 d . . .
O12 O -0.29865(16) -0.09005(13) 0.2328(2) 0.0175(4) Uani 1 1 d . . .
O13 O -0.27705(16) 0.05659(12) 0.7247(2) 0.0172(4) Uani 1 1 d . . .
O14 O 0.08305(18) 0.16399(16) 0.9543(2) 0.0258(5) Uani 1 1 d . . .
O15 O -0.31581(16) 0.26481(13) 0.2944(2) 0.0180(4) Uani 1 1 d . . .
O16 O -0.09857(16) 0.17140(14) 0.8071(2) 0.0210(4) Uani 1 1 d . . .
O17 O 0.1539(2) -0.03549(18) 0.9082(3) 0.0376(6) Uani 1 1 d . . .
O18 O 0.04671(18) -0.08092(15) 0.6035(3) 0.0281(5) Uani 1 1 d . . .
N1 N -0.5030(3) 0.0007(3) 0.1566(4) 0.0237(8) Uani 0.70 1 d P . .
C1 C -0.5100(3) 0.0823(3) 0.0787(4) 0.0355(8) Uani 1 1 d . . .
C2 C -0.5584(3) -0.0754(3) 0.0438(6) 0.0475(11) Uani 1 1 d . . .
N2 N -0.6109(6) 0.0112(6) 0.0271(9) 0.0206(18) Uani 0.30 1 d P . .


_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
Mg1 O10 2.033(2) 3_556 ?
Mg1 O12 2.052(2) 3_556 ?
Mg1 O9 2.065(2) 3_556 ?
Mg1 O4 2.075(2) . ?
Mg1 O18 2.085(2) . ?
Mg1 O17 2.232(3) . ?
Al1 O14 1.720(2) 4_565 ?
Al1 O5 1.730(2) 3_556 ?
Al1 O2 1.740(2) 2_556 ?
Al1 O6 1.741(2) . ?
Al2 O16 1.732(2) . ?
Al2 O3 1.732(2) . ?
Al2 O15 1.734(2) 4_566 ?
Al2 O13 1.746(2) . ?
Al3 O1 1.716(2) 3_456 ?
Al3 O11 1.733(2) . ?
Al3 O8 1.734(2) 4_556 ?
Al3 O7 1.736(2) . ?
P1 O4 1.496(2) . ?
P1 O16 1.528(2) . ?
P1 O14 1.532(2) . ?
P1 O6 1.541(2) . ?
P2 O12 1.501(2) . ?
P2 O5 1.527(2) . ?
P2 O8 1.528(2) . ?
P2 O11 1.540(2) . ?
P3 O10 1.488(2) . ?
P3 O3 1.535(2) . ?
P3 O1 1.536(2) . ?
P3 O15 1.537(2) . ?
P4 O9 1.486(2) . ?
P4 O2 1.540(2) . ?
P4 O13 1.543(2) . ?
P4 O7 1.545(2) . ?
O1 Al3 1.716(2) 3_456 ?
O2 Al1 1.740(2) 2_546 ?
O5 Al1 1.730(2) 3_556 ?
O8 Al3 1.734(2) 4 ?
O9 Mg1 2.065(2) 3_556 ?
O10 Mg1 2.033(2) 3_556 ?
O12 Mg1 2.052(2) 3_556 ?
O14 Al1 1.720(2) 4_566 ?
O15 Al2 1.734(2) 4_565 ?
N1 C1 1.408(5) . ?
N1 C2 1.620(6) . ?
N1 N2 1.658(9) . ?
C1 C2 1.506(6) 3_455 ?
C1 N2 1.654(9) . ?
C2 N2 1.446(9) . ?
C2 C1 1.506(6) 3_455 ?

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
O10 Mg1 O12 90.51(9) 3_556 3_556 ?
O10 Mg1 O9 95.02(10) 3_556 3_556 ?
O12 Mg1 O9 93.76(9) 3_556 3_556 ?
O10 Mg1 O4 167.94(10) 3_556 . ?
O12 Mg1 O4 92.12(9) 3_556 . ?
O9 Mg1 O4 96.55(9) 3_556 . ?
O10 Mg1 O18 89.95(10) 3_556 . ?
O12 Mg1 O18 176.73(10) 3_556 . ?
O9 Mg1 O18 89.43(10) 3_556 . ?
O4 Mg1 O18 86.78(9) . . ?
O10 Mg1 O17 82.35(10) 3_556 . ?
O12 Mg1 O17 89.29(10) 3_556 . ?
O9 Mg1 O17 176.00(10) 3_556 . ?
O4 Mg1 O17 85.92(10) . . ?
O18 Mg1 O17 87.57(10) . . ?
O14 Al1 O5 111.40(12) 4_565 3_556 ?
O14 Al1 O2 103.61(11) 4_565 2_556 ?
O5 Al1 O2 110.29(11) 3_556 2_556 ?
O14 Al1 O6 113.58(12) 4_565 . ?
O5 Al1 O6 108.88(11) 3_556 . ?
O2 Al1 O6 108.95(12) 2_556 . ?
O16 Al2 O3 111.50(11) . . ?
O16 Al2 O15 109.85(10) . 4_566 ?
O3 Al2 O15 110.65(11) . 4_566 ?
O16 Al2 O13 107.77(11) . . ?
O3 Al2 O13 109.71(10) . . ?
O15 Al2 O13 107.23(10) 4_566 . ?
O1 Al3 O11 108.65(11) 3_456 . ?
O1 Al3 O8 110.29(11) 3_456 4_556 ?
O11 Al3 O8 109.91(11) . 4_556 ?
O1 Al3 O7 109.25(11) 3_456 . ?
O11 Al3 O7 110.18(11) . . ?
O8 Al3 O7 108.54(12) 4_556 . ?
O4 P1 O16 112.43(12) . . ?
O4 P1 O14 111.16(13) . . ?
O16 P1 O14 106.16(13) . . ?
O4 P1 O6 111.55(13) . . ?
O16 P1 O6 106.71(12) . . ?
O14 P1 O6 108.56(14) . . ?
O12 P2 O5 113.25(12) . . ?
O12 P2 O8 108.93(12) . . ?
O5 P2 O8 110.14(13) . . ?
O12 P2 O11 110.77(12) . . ?
O5 P2 O11 106.66(12) . . ?
O8 P2 O11 106.90(12) . . ?
O10 P3 O3 112.97(12) . . ?
O10 P3 O1 110.19(13) . . ?
O3 P3 O1 108.04(12) . . ?
O10 P3 O15 111.86(13) . . ?
O3 P3 O15 106.79(12) . . ?
O1 P3 O15 106.70(12) . . ?
O9 P4 O2 112.01(13) . . ?
O9 P4 O13 114.15(12) . . ?
O2 P4 O13 105.36(12) . . ?
O9 P4 O7 113.75(13) . . ?
O2 P4 O7 107.47(13) . . ?
O13 P4 O7 103.32(12) . . ?
P3 O1 Al3 167.11(16) . 3_456 ?
P4 O2 Al1 146.91(15) . 2_546 ?
P3 O3 Al2 135.42(14) . . ?
P1 O4 Mg1 143.77(14) . . ?
P2 O5 Al1 146.87(16) . 3_556 ?
P1 O6 Al1 135.00(15) . . ?
P4 O7 Al3 143.86(15) . . ?
P2 O8 Al3 148.08(15) . 4 ?
P4 O9 Mg1 154.57(15) . 3_556 ?
P3 O10 Mg1 140.81(14) . 3_556 ?
P2 O11 Al3 132.66(13) . . ?
P2 O12 Mg1 134.90(12) . 3_556 ?
P4 O13 Al2 137.38(13) . . ?
P1 O14 Al1 161.36(17) . 4_566 ?
P3 O15 Al2 140.19(13) . 4_565 ?
P1 O16 Al2 146.22(15) . . ?
C1 N1 C2 107.2(3) . . ?
C1 N1 N2 64.7(4) . . ?
C2 N1 N2 52.3(4) . . ?
N1 C1 C2 108.7(3) . 3_455 ?
N1 C1 N2 65.0(4) . . ?
C2 C1 N2 103.1(4) 3_455 . ?
N2 C2 C1 105.9(4) . 3_455 ?
N2 C2 N1 65.2(4) . . ?
C1 C2 N1 107.0(3) 3_455 . ?
C2 N2 C1 103.7(5) . . ?
C2 N2 N1 62.5(4) . . ?
C1 N2 N1 50.3(3) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.37
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.880
_refine_diff_density_min         -0.483
_refine_diff_density_rms         0.106
_database_code_depnum_ccdc_archive 'CCDC 1007280'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_JU94-400

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H8 Al3 Mg N O17 P4'
_chemical_formula_weight         547.22

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'
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'
Mg Mg 0.0486 0.0363 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/c'

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

_cell_length_a                   12.389(5)
_cell_length_b                   14.923(6)
_cell_length_c                   9.386(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 98.699(7)
_cell_angle_gamma                90.00
_cell_volume                     1715.2(12)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      1.66
_cell_measurement_theta_max      29.39

_exptl_crystal_description       rod
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.119
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1096
_exptl_absorpt_coefficient_mu    0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8692
_exptl_absorpt_correction_T_max  0.9314
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13511
_diffrn_reflns_av_R_equivalents  0.0681
_diffrn_reflns_av_sigmaI/netI    0.0768
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         1.66
_diffrn_reflns_theta_max         29.39
_reflns_number_total             4653
_reflns_number_gt                3203
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex 2'
_computing_cell_refinement       'Bruker SMART Apex 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0864P)²+26.7289P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4653
_refine_ls_number_parameters     253
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.1289
_refine_ls_R_factor_gt           0.0950
_refine_ls_wR_factor_ref         0.2681
_refine_ls_wR_factor_gt          0.2521
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_restrained_S_all      1.120
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.001

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
P1 P 0.19303(16) 0.17320(13) -0.1233(2) 0.0182(4) Uani 1 1 d . . .
P2 P 0.15605(16) -0.18447(13) -0.2128(2) 0.0189(4) Uani 1 1 d . . .
P3 P 0.52999(16) 0.17600(13) 0.2965(2) 0.0197(4) Uani 1 1 d . . .
P4 P 0.24592(16) -0.03510(12) 0.1722(2) 0.0173(4) Uani 1 1 d . . .
Al1 Al 0.27376(19) 0.16899(15) 0.2035(2) 0.0179(5) Uani 1 1 d . . .
Al2 Al 0.05654(18) -0.33043(15) -0.4396(3) 0.0183(5) Uani 1 1 d . . .
Al3 Al 0.35496(19) -0.18840(15) 0.3738(3) 0.0194(5) Uani 1 1 d . . .
Mg1 Mg 0.3233(2) -0.01529(19) -0.1586(3) 0.0255(6) Uani 1 1 d . . .
O1 O 0.2239(5) 0.0608(4) 0.2241(6) 0.0233(12) Uani 1 1 d . . .
O2 O 0.0606(5) -0.1774(4) -0.1239(6) 0.0268(12) Uani 1 1 d . . .
O3 O 0.1126(6) -0.2340(4) -0.3527(7) 0.0339(15) Uani 1 1 d . . .
O4 O 0.2681(5) 0.1928(4) 0.0202(6) 0.0280(13) Uani 1 1 d . . .
O5 O 0.3113(5) -0.0371(4) 0.0503(7) 0.0285(13) Uani 1 1 d . . .
O6 O 0.1930(5) -0.0920(4) -0.2505(7) 0.0292(13) Uani 1 1 d . . .
O7 O 0.4074(5) 0.1766(5) 0.2914(7) 0.0337(15) Uani 1 1 d . . .
O8 O 0.2446(5) -0.2387(4) -0.1213(7) 0.0315(14) Uani 1 1 d . . .
O9 O 0.5609(6) 0.2693(5) 0.2432(8) 0.0413(17) Uani 1 1 d . . .
O10 O 0.1900(5) 0.2594(4) -0.2159(7) 0.0270(13) Uani 1 1 d . . .
O11 O 0.0761(5) 0.1563(5) -0.0909(7) 0.0321(14) Uani 1 1 d . . .
O12 O 0.3029(6) -0.0848(4) 0.3057(7) 0.0329(14) Uani 1 1 d . . .
O13 O 0.1295(5) -0.0768(4) 0.1338(7) 0.0301(14) Uani 1 1 d . . .
O14 O 0.2306(6) 0.0941(4) -0.2024(7) 0.0339(14) Uani 1 1 d . . .
O15 O 0.5806(6) 0.1684(5) 0.4541(7) 0.0421(17) Uani 1 1 d . . .
O16 O 0.5682(6) 0.1022(5) 0.2076(8) 0.0398(16) Uani 1 1 d . . .
O17 O 0.4556(6) 0.0739(5) -0.1225(12) 0.060(3) Uani 1 1 d . . .
N1 N 0.0040(9) 0.9144(7) 0.4310(11) 0.053(3) Uani 1 1 d . . .
C1 C 0.0051(9) 0.9979(7) 0.3471(11) 0.037(2) Uani 1 1 d . . .
C2 C -0.0620(10) 0.9299(8) 0.5491(15) 0.052(3) Uani 1 1 d . . .


_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
P1 O14 1.506(6) . ?
P1 O4 1.544(6) . ?
P1 O11 1.545(6) . ?
P1 O10 1.550(6) . ?
P2 O6 1.512(6) . ?
P2 O8 1.520(6) . ?
P2 O3 1.531(6) . ?
P2 O2 1.551(6) . ?
P3 O16 1.500(7) . ?
P3 O7 1.512(6) . ?
P3 O15 1.521(7) . ?
P3 O9 1.547(7) . ?
P4 O5 1.498(6) . ?
P4 O12 1.533(6) . ?
P4 O1 1.549(6) . ?
P4 O13 1.562(6) . ?
Al1 O7 1.738(6) . ?
Al1 O10 1.740(6) 4_566 ?
Al1 O4 1.747(6) . ?
Al1 O1 1.750(6) . ?
Al2 O11 1.721(6) 2_544 ?
Al2 O13 1.737(6) 4 ?
Al2 O2 1.742(6) 4 ?
Al2 O3 1.746(6) . ?
Al3 O15 1.716(7) 3_656 ?
Al3 O9 1.743(7) 2_645 ?
Al3 O8 1.753(7) 4_556 ?
Al3 O12 1.758(6) . ?
Mg1 O16 1.971(7) 3_655 ?
Mg1 O14 2.002(7) . ?
Mg1 O5 2.016(7) . ?
Mg1 O6 2.060(7) . ?
Mg1 O17 2.098(8) . ?
O2 Al2 1.742(6) 4_556 ?
O8 Al3 1.753(7) 4 ?
O9 Al3 1.743(7) 2_655 ?
O10 Al1 1.740(6) 4_565 ?
O11 Al2 1.721(6) 2_554 ?
O13 Al2 1.737(6) 4_556 ?
O15 Al3 1.716(7) 3_656 ?
O16 Mg1 1.971(7) 3_655 ?
N1 C1 1.476(14) . ?
N1 C2 1.491(16) . ?
C1 C2 1.549(16) 3_576 ?
C2 C1 1.549(16) 3_576 ?

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
O14 P1 O4 112.8(4) . . ?
O14 P1 O11 109.7(4) . . ?
O4 P1 O11 108.6(4) . . ?
O14 P1 O10 110.9(4) . . ?
O4 P1 O10 107.0(3) . . ?
O11 P1 O10 107.6(4) . . ?
O6 P2 O8 113.6(4) . . ?
O6 P2 O3 108.6(4) . . ?
O8 P2 O3 110.9(4) . . ?
O6 P2 O2 110.3(4) . . ?
O8 P2 O2 106.0(4) . . ?
O3 P2 O2 107.3(4) . . ?
O16 P3 O7 112.7(4) . . ?
O16 P3 O15 111.6(4) . . ?
O7 P3 O15 107.2(4) . . ?
O16 P3 O9 111.5(4) . . ?
O7 P3 O9 106.3(4) . . ?
O15 P3 O9 107.2(4) . . ?
O5 P4 O12 112.3(4) . . ?
O5 P4 O1 113.5(3) . . ?
O12 P4 O1 105.7(3) . . ?
O5 P4 O13 113.7(4) . . ?
O12 P4 O13 106.9(4) . . ?
O1 P4 O13 103.9(3) . . ?
O7 Al1 O10 109.9(3) . 4_566 ?
O7 Al1 O4 110.3(3) . . ?
O10 Al1 O4 111.4(3) 4_566 . ?
O7 Al1 O1 109.5(3) . . ?
O10 Al1 O1 106.0(3) 4_566 . ?
O4 Al1 O1 109.5(3) . . ?
O11 Al2 O13 107.2(3) 2_544 4 ?
O11 Al2 O2 110.2(3) 2_544 4 ?
O13 Al2 O2 110.8(3) 4 4 ?
O11 Al2 O3 109.8(3) 2_544 . ?
O13 Al2 O3 109.0(3) 4 . ?
O2 Al2 O3 109.8(3) 4 . ?
O15 Al3 O9 114.7(4) 3_656 2_645 ?
O15 Al3 O8 109.7(4) 3_656 4_556 ?
O9 Al3 O8 109.6(3) 2_645 4_556 ?
O15 Al3 O12 106.4(4) 3_656 . ?
O9 Al3 O12 108.1(4) 2_645 . ?
O8 Al3 O12 108.1(3) 4_556 . ?
O16 Mg1 O14 151.5(3) 3_655 . ?
O16 Mg1 O5 105.9(3) 3_655 . ?
O14 Mg1 O5 101.9(3) . . ?
O16 Mg1 O6 93.2(3) 3_655 . ?
O14 Mg1 O6 88.7(3) . . ?
O5 Mg1 O6 98.6(3) . . ?
O16 Mg1 O17 84.9(3) 3_655 . ?
O14 Mg1 O17 85.8(3) . . ?
O5 Mg1 O17 96.7(4) . . ?
O6 Mg1 O17 164.6(4) . . ?
P4 O1 Al1 137.4(4) . . ?
P2 O2 Al2 132.7(4) . 4_556 ?
P2 O3 Al2 149.5(5) . . ?
P1 O4 Al1 138.5(4) . . ?
P4 O5 Mg1 150.2(4) . . ?
P2 O6 Mg1 130.9(4) . . ?
P3 O7 Al1 153.5(5) . . ?
P2 O8 Al3 144.5(5) . 4 ?
P3 O9 Al3 137.0(5) . 2_655 ?
P1 O10 Al1 142.0(4) . 4_565 ?
P1 O11 Al2 163.9(5) . 2_554 ?
P4 O12 Al3 145.2(4) . . ?
P4 O13 Al2 144.7(4) . 4_556 ?
P1 O14 Mg1 138.5(4) . . ?
P3 O15 Al3 165.3(6) . 3_656 ?
P3 O16 Mg1 153.6(5) . 3_655 ?
C1 N1 C2 108.4(9) . . ?
N1 C1 C2 107.0(9) . 3_576 ?
N1 C2 C1 109.1(9) . 3_576 ?

_diffrn_measured_fraction_theta_max 0.985
_diffrn_reflns_theta_full        29.39
_diffrn_measured_fraction_theta_full 0.985
_refine_diff_density_max         1.804
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.200
_database_code_depnum_ccdc_archive 'CCDC 1007281'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_JU95

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H10 Al3 Mg N O18 P4'
_chemical_formula_weight         565.24

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'
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'
Mg Mg 0.0486 0.0363 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 21/n'

loop_
_symmetry_equiv_pos_as_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                   8.1871(16)
_cell_length_b                   14.690(3)
_cell_length_c                   14.096(3)
_cell_angle_alpha                90.00
_cell_angle_beta                 92.24(3)
_cell_angle_gamma                90.00
_cell_volume                     1694.0(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      27.47

_exptl_crystal_description       rod
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.216
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1136
_exptl_absorpt_coefficient_mu    0.738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9298
_exptl_absorpt_correction_T_max  0.9298
_exptl_absorpt_process_details   sadabs

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15881
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.47
_reflns_number_total             3818
_reflns_number_gt                3488
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex 2'
_computing_cell_refinement       'Bruker SMART Apex 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0461P)²+3.5324P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3818
_refine_ls_number_parameters     262
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.0964
_refine_ls_wR_factor_gt          0.0951
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_restrained_S_all      1.080
_refine_ls_shift/su_max          0.001
_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
P1 P 0.12445(8) 0.55718(4) 0.29306(4) 0.01101(14) Uani 1 1 d . . .
P2 P -0.12832(8) 0.78329(4) 0.59383(4) 0.01184(14) Uani 1 1 d . . .
P3 P 0.12399(7) 0.17289(4) -0.23350(4) 0.01267(14) Uani 1 1 d . . .
P4 P 0.18767(8) 0.37041(4) 0.07400(4) 0.01219(14) Uani 1 1 d . . .
Al1 Al 0.00767(9) 0.36014(5) 0.26019(5) 0.01129(16) Uani 1 1 d . . .
Al2 Al 0.03560(9) 0.72538(5) 0.41092(5) 0.01171(16) Uani 1 1 d . . .
Al3 Al -0.00500(9) 0.33231(5) -0.11410(5) 0.01309(16) Uani 1 1 d . . .
Mg8 Mg 0.46358(10) 0.51370(6) 0.18063(6) 0.01294(18) Uani 1 1 d . . .
O1 O 0.0784(2) 0.61302(12) 0.38038(12) 0.0162(4) Uani 1 1 d . . .
O2 O 0.3037(2) 0.56439(14) 0.27761(14) 0.0228(4) Uani 1 1 d . . .
O5 O -0.0677(2) 0.72073(13) 0.51509(13) 0.0201(4) Uani 1 1 d . . .
O13 O 0.0469(2) 0.35922(14) 0.14129(13) 0.0228(4) Uani 1 1 d . . .
O14 O 0.1100(2) 0.38600(13) -0.02538(12) 0.0187(4) Uani 1 1 d . . .
O3 O 0.0748(3) 0.45936(13) 0.31516(14) 0.0243(4) Uani 1 1 d . . .
O4 O 0.0176(2) 0.59072(14) 0.20794(13) 0.0212(4) Uani 1 1 d . . .
O6 O -0.0471(3) 0.87355(14) 0.59483(17) 0.0351(6) Uani 1 1 d . . .
O9 O 0.1001(3) 0.23480(14) -0.14745(15) 0.0274(5) Uani 1 1 d . . .
O10 O 0.0925(3) 0.22869(14) -0.32328(15) 0.0282(5) Uani 1 1 d . . .
O15 O 0.2764(3) 0.27827(15) 0.07248(16) 0.0293(5) Uani 1 1 d . . .
O16 O 0.2971(3) 0.44747(16) 0.10031(15) 0.0318(5) Uani 1 1 d . . .
O11 O 0.0155(3) 0.09181(14) -0.22916(15) 0.0314(5) Uani 1 1 d . . .
O12 O 0.3016(3) 0.1444(2) -0.22820(18) 0.0522(8) Uani 1 1 d . . .
O7 O -0.1008(4) 0.73301(16) 0.68707(15) 0.0443(7) Uani 1 1 d . . .
O8 O -0.3116(3) 0.7935(2) 0.57492(19) 0.0440(7) Uani 1 1 d . . .
O17 O 0.6500(3) 0.46896(14) 0.09067(14) 0.0271(5) Uani 1 1 d . . .
O18 O 0.6516(3) 0.59250(18) 0.26032(17) 0.0387(6) Uani 1 1 d . . .
N1 N 0.0834(4) 0.0845(2) 0.0199(2) 0.0403(7) Uani 1 1 d . . .
C2 C 0.1700(4) 0.0050(3) -0.0203(3) 0.0395(8) Uani 1 1 d . . .
C1 C -0.0934(5) 0.0822(3) -0.0142(4) 0.0542(12) Uani 1 1 d . . .


_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
P1 O2 1.496(2) . ?
P1 O3 1.5287(19) . ?
P1 O1 1.5383(18) . ?
P1 O4 1.5382(19) . ?
P2 O6 1.483(2) . ?
P2 O7 1.517(2) . ?
P2 O8 1.521(2) . ?
P2 O5 1.5380(18) . ?
P3 O11 1.489(2) . ?
P3 O12 1.512(2) . ?
P3 O10 1.521(2) . ?
P3 O9 1.535(2) . ?
P4 O16 1.482(2) . ?
P4 O13 1.530(2) . ?
P4 O14 1.5328(18) . ?
P4 O15 1.537(2) . ?
Al1 O12 1.703(2) 4_566 ?
Al1 O13 1.719(2) . ?
Al1 O7 1.721(2) 3_566 ?
Al1 O3 1.730(2) . ?
Al2 O5 1.725(2) . ?
Al2 O10 1.726(2) 3_565 ?
Al2 O15 1.732(2) 2 ?
Al2 O1 1.7448(19) . ?
Al3 O8 1.718(2) 2_445 ?
Al3 O14 1.726(2) . ?
Al3 O4 1.740(2) 3_565 ?
Al3 O9 1.745(2) . ?
Mg8 O16 1.992(2) . ?
Mg8 O11 2.039(2) 4_666 ?
Mg8 O6 2.051(2) 4_675 ?
Mg8 O2 2.068(2) . ?
Mg8 O17 2.126(2) . ?
Mg8 O18 2.199(3) . ?
O4 Al3 1.740(2) 3_565 ?
O6 Mg8 2.051(2) 4_576 ?
O10 Al2 1.726(2) 3_565 ?
O15 Al2 1.732(2) 2_545 ?
O11 Mg8 2.039(2) 4_565 ?
O12 Al1 1.703(2) 4_665 ?
O7 Al1 1.721(2) 3_566 ?
O8 Al3 1.718(2) 2_455 ?
N1 C2 1.489(5) . ?
N1 C1 1.508(4) . ?
C2 C1 1.514(6) 3 ?
C1 C2 1.514(6) 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 P1 O3 111.51(12) . . ?
O2 P1 O1 110.56(11) . . ?
O3 P1 O1 105.23(11) . . ?
O2 P1 O4 113.28(12) . . ?
O3 P1 O4 108.19(12) . . ?
O1 P1 O4 107.67(11) . . ?
O6 P2 O7 112.06(16) . . ?
O6 P2 O8 110.66(16) . . ?
O7 P2 O8 108.17(18) . . ?
O6 P2 O5 112.59(12) . . ?
O7 P2 O5 107.04(12) . . ?
O8 P2 O5 106.01(13) . . ?
O11 P3 O12 110.51(17) . . ?
O11 P3 O10 112.52(13) . . ?
O12 P3 O10 108.78(14) . . ?
O11 P3 O9 110.29(12) . . ?
O12 P3 O9 106.11(15) . . ?
O10 P3 O9 108.39(12) . . ?
O16 P4 O13 112.93(13) . . ?
O16 P4 O14 109.87(12) . . ?
O13 P4 O14 106.67(11) . . ?
O16 P4 O15 113.26(14) . . ?
O13 P4 O15 106.38(12) . . ?
O14 P4 O15 107.36(12) . . ?
O12 Al1 O13 108.47(12) 4_566 . ?
O12 Al1 O7 110.58(16) 4_566 3_566 ?
O13 Al1 O7 108.58(11) . 3_566 ?
O12 Al1 O3 106.74(14) 4_566 . ?
O13 Al1 O3 112.04(10) . . ?
O7 Al1 O3 110.42(13) 3_566 . ?
O5 Al2 O10 108.69(11) . 3_565 ?
O5 Al2 O15 111.46(11) . 2 ?
O10 Al2 O15 115.66(12) 3_565 2 ?
O5 Al2 O1 106.42(9) . . ?
O10 Al2 O1 108.38(10) 3_565 . ?
O15 Al2 O1 105.77(11) 2 . ?
O8 Al3 O14 112.19(12) 2_445 . ?
O8 Al3 O4 115.71(12) 2_445 3_565 ?
O14 Al3 O4 105.55(10) . 3_565 ?
O8 Al3 O9 105.09(14) 2_445 . ?
O14 Al3 O9 108.04(10) . . ?
O4 Al3 O9 110.10(10) 3_565 . ?
O16 Mg8 O11 96.00(11) . 4_666 ?
O16 Mg8 O6 92.68(11) . 4_675 ?
O11 Mg8 O6 170.00(11) 4_666 4_675 ?
O16 Mg8 O2 96.59(10) . . ?
O11 Mg8 O2 89.04(9) 4_666 . ?
O6 Mg8 O2 94.91(9) 4_675 . ?
O16 Mg8 O17 90.08(10) . . ?
O11 Mg8 O17 90.01(9) 4_666 . ?
O6 Mg8 O17 85.01(9) 4_675 . ?
O2 Mg8 O17 173.32(10) . . ?
O16 Mg8 O18 175.92(10) . . ?
O11 Mg8 O18 87.53(11) 4_666 . ?
O6 Mg8 O18 83.63(11) 4_675 . ?
O2 Mg8 O18 85.48(9) . . ?
O17 Mg8 O18 87.88(10) . . ?
P1 O1 Al2 139.45(12) . . ?
P1 O2 Mg8 136.11(13) . . ?
P2 O5 Al2 140.68(13) . . ?
P4 O13 Al1 141.03(14) . . ?
P4 O14 Al3 142.08(13) . . ?
P1 O3 Al1 141.53(13) . . ?
P1 O4 Al3 144.69(14) . 3_565 ?
P2 O6 Mg8 137.44(14) . 4_576 ?
P3 O9 Al3 141.17(15) . . ?
P3 O10 Al2 152.19(16) . 3_565 ?
P4 O15 Al2 144.24(16) . 2_545 ?
P4 O16 Mg8 155.40(16) . . ?
P3 O11 Mg8 133.84(13) . 4_565 ?
P3 O12 Al1 163.8(2) . 4_665 ?
P2 O7 Al1 144.08(16) . 3_566 ?
P2 O8 Al3 147.68(17) . 2_455 ?
C2 N1 C1 109.1(3) . . ?
N1 C2 C1 109.4(3) . 3 ?
N1 C1 C2 108.7(3) . 3 ?

_diffrn_measured_fraction_theta_max 0.982
_diffrn_reflns_theta_full        27.47
_diffrn_measured_fraction_theta_full 0.982
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.573
_refine_diff_density_rms         0.094
_database_code_depnum_ccdc_archive 'CCDC 1007282'
#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication
#  deposited with the CCDC, and may include chemical, crystal,
#  experimental, refinement, atomic coordinates,
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted.
#
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material
#  of the CCDC or of third parties, and may not be copied or further
#  disseminated in any form, whether machine-readable or not,
#  except for the purpose of generating routine backup copies
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and
#  data retrieval see:
#                         www.ccdc.cam.ac.uk
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively.
#
data_JU95-300

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C2 H6 Al3 Mg N O16 P4'
_chemical_formula_weight         529.21

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'
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'
Mg Mg 0.0486 0.0363 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n

loop_
_symmetry_equiv_pos_as_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                   8.3877(14)
_cell_length_b                   14.399(2)
_cell_length_c                   14.017(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 91.552(3)
_cell_angle_gamma                90.00
_cell_volume                     1692.4(5)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      2.03
_cell_measurement_theta_max      28.27

_exptl_crystal_description       rod
_exptl_crystal_colour            white
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1056
_exptl_absorpt_coefficient_mu    0.723
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.8123
_exptl_absorpt_correction_T_max  0.9648
_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  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13543
_diffrn_reflns_av_R_equivalents  0.0391
_diffrn_reflns_av_sigmaI/netI    0.0393
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_theta_min         2.03
_diffrn_reflns_theta_max         28.27
_reflns_number_total             4196
_reflns_number_gt                3446
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       'Bruker SMART Apex 2'
_computing_cell_refinement       'Bruker SMART Apex 2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    SHELXP-97
_computing_publication_material  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)+(0.0451P)²+6.6924P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   .
_refine_ls_hydrogen_treatment    .
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         4196
_refine_ls_number_parameters     244
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0497
_refine_ls_wR_factor_ref         0.1310
_refine_ls_wR_factor_gt          0.1248
_refine_ls_goodness_of_fit_ref   1.123
_refine_ls_restrained_S_all      1.123
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002

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
P1 P 0.11845(11) 0.17078(7) 0.75604(7) 0.0138(2) Uani 1 1 d . . .
P2 P -0.10381(12) 0.45010(7) 0.69984(6) 0.0138(2) Uani 1 1 d . . .
Al2 Al -0.04930(13) 0.27704(8) 0.58014(8) 0.0130(2) Uani 1 1 d . . .
P3 P -0.32652(12) 0.14200(7) 0.56676(7) 0.0148(2) Uani 1 1 d . . .
P4 P -0.38002(11) 0.29003(7) 0.89613(6) 0.0131(2) Uani 1 1 d . . .
Al3 Al -0.02059(14) 0.32527(8) 0.88068(8) 0.0145(2) Uani 1 1 d . . .
Mg1 Mg -0.41617(16) 0.49485(9) 0.81931(9) 0.0175(3) Uani 1 1 d . . .
Al1 Al 0.49229(13) 0.14925(8) 0.75349(8) 0.0127(2) Uani 1 1 d . . .
O1 O 0.0496(4) 0.2169(2) 0.8451(2) 0.0259(7) Uani 1 1 d . . .
O2 O 0.2975(3) 0.1809(2) 0.7668(2) 0.0299(7) Uani 1 1 d . . .
O3 O -0.0699(3) 0.39521(19) 0.60887(18) 0.0172(6) Uani 1 1 d . . .
O4 O -0.4659(4) 0.3794(2) 0.8796(2) 0.0284(7) Uani 1 1 d . . .
O5 O -0.0297(4) 0.4003(2) 0.7857(2) 0.0270(7) Uani 1 1 d . . .
O6 O -0.2471(3) 0.2393(2) 0.5685(2) 0.0243(6) Uani 1 1 d . . .
O7 O -0.2819(4) 0.4608(2) 0.7094(2) 0.0273(7) Uani 1 1 d . . .
O8 O -0.3803(3) 0.2306(2) 0.80552(19) 0.0219(6) Uani 1 1 d . . .
O9 O -0.3944(3) 0.1265(2) 0.46632(19) 0.0218(6) Uani 1 1 d . . .
O10 O 0.0432(4) 0.2694(2) 0.4735(2) 0.0259(7) Uani 1 1 d . . .
O11 O -0.2060(3) 0.3058(2) 0.9272(2) 0.0239(6) Uani 1 1 d . . .
O12 O 0.0630(4) 0.2243(2) 0.6683(2) 0.0287(7) Uani 1 1 d . . .
O13 O 0.0693(4) 0.0708(2) 0.7498(2) 0.0281(7) Uani 1 1 d . . .
O14 O -0.4666(4) 0.1464(2) 0.6337(2) 0.0270(7) Uani 1 1 d . . .
O15 O -0.2096(4) 0.0688(2) 0.5951(2) 0.0303(7) Uani 1 1 d . . .
O16 O -0.0226(4) 0.5437(2) 0.6894(2) 0.0279(7) Uani 1 1 d . . .
N1 N -0.4115(5) 0.4187(3) 0.5268(3) 0.0365(10) Uani 1 1 d . . .
C1 C -0.3368(6) 0.4924(4) 0.4676(4) 0.0372(12) Uani 1 1 d . . .
C2 C -0.5891(7) 0.4139(4) 0.5107(4) 0.0436(13) Uani 1 1 d . . .


_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
P1 O13 1.499(3) . ?
P1 O2 1.512(3) . ?
P1 O12 1.514(3) . ?
P1 O1 1.540(3) . ?
P2 O7 1.511(3) . ?
P2 O16 1.519(3) . ?
P2 O5 1.519(3) . ?
P2 O3 1.533(3) . ?
Al2 O10 1.707(3) . ?
Al2 O12 1.711(3) . ?
Al2 O6 1.749(3) . ?
Al2 O3 1.758(3) . ?
P3 O15 1.487(3) . ?
P3 O9 1.521(3) . ?
P3 O14 1.525(3) . ?
P3 O6 1.551(3) . ?
P4 O4 1.490(3) . ?
P4 O11 1.529(3) . ?
P4 O8 1.531(3) . ?
P4 O10 1.536(3) 4_566 ?
P4 Mg1 3.1516(17) . ?
Al3 O5 1.715(3) . ?
Al3 O9 1.725(3) 4_666 ?
Al3 O11 1.725(3) . ?
Al3 O1 1.746(3) . ?
Mg1 O15 1.902(3) 2_456 ?
Mg1 O4 1.917(3) . ?
Mg1 O13 1.928(3) 2_456 ?
Mg1 O7 1.994(3) . ?
Al1 O2 1.711(3) . ?
Al1 O14 1.723(3) 1_655 ?
Al1 O8 1.734(3) 1_655 ?
Al1 O16 1.734(3) 2_546 ?
O8 Al1 1.734(3) 1_455 ?
O9 Al3 1.725(3) 4_565 ?
O10 P4 1.536(3) 4_665 ?
O13 Mg1 1.928(3) 2_446 ?
O14 Al1 1.723(3) 1_455 ?
O15 Mg1 1.902(3) 2_446 ?
O16 Al1 1.734(3) 2_556 ?
N1 C1 1.496(7) . ?
N1 C2 1.502(7) . ?
C1 C2 1.520(7) 3_466 ?
C2 C1 1.520(7) 3_466 ?

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
O13 P1 O2 111.67(19) . . ?
O13 P1 O12 111.33(18) . . ?
O2 P1 O12 108.3(2) . . ?
O13 P1 O1 110.61(19) . . ?
O2 P1 O1 105.71(18) . . ?
O12 P1 O1 109.01(18) . . ?
O7 P2 O16 111.37(19) . . ?
O7 P2 O5 111.25(18) . . ?
O16 P2 O5 108.68(19) . . ?
O7 P2 O3 109.42(17) . . ?
O16 P2 O3 106.46(16) . . ?
O5 P2 O3 109.53(16) . . ?
O10 Al2 O12 110.46(17) . . ?
O10 Al2 O6 110.53(16) . . ?
O12 Al2 O6 115.58(17) . . ?
O10 Al2 O3 108.24(15) . . ?
O12 Al2 O3 108.64(15) . . ?
O6 Al2 O3 102.90(15) . . ?
O15 P3 O9 111.81(18) . . ?
O15 P3 O14 112.2(2) . . ?
O9 P3 O14 107.49(17) . . ?
O15 P3 O6 110.86(18) . . ?
O9 P3 O6 107.28(17) . . ?
O14 P3 O6 106.88(18) . . ?
O4 P4 O11 111.74(19) . . ?
O4 P4 O8 111.32(18) . . ?
O11 P4 O8 107.40(16) . . ?
O4 P4 O10 112.35(19) . 4_566 ?
O11 P4 O10 107.28(18) . 4_566 ?
O8 P4 O10 106.45(17) . 4_566 ?
O4 P4 Mg1 25.45(13) . . ?
O11 P4 Mg1 92.35(13) . . ?
O8 P4 Mg1 103.96(12) . . ?
O10 P4 Mg1 136.38(13) 4_566 . ?
O5 Al3 O9 107.47(16) . 4_666 ?
O5 Al3 O11 111.99(17) . . ?
O9 Al3 O11 110.18(14) 4_666 . ?
O5 Al3 O1 110.48(15) . . ?
O9 Al3 O1 110.69(16) 4_666 . ?
O11 Al3 O1 106.07(16) . . ?
O15 Mg1 O4 109.36(16) 2_456 . ?
O15 Mg1 O13 110.47(15) 2_456 2_456 ?
O4 Mg1 O13 124.33(16) . 2_456 ?
O15 Mg1 O7 108.03(16) 2_456 . ?
O4 Mg1 O7 105.19(15) . . ?
O13 Mg1 O7 97.66(15) 2_456 . ?
O15 Mg1 P4 105.19(11) 2_456 . ?
O4 Mg1 P4 19.51(10) . . ?
O13 Mg1 P4 139.40(11) 2_456 . ?
O7 Mg1 P4 89.03(11) . . ?
O2 Al1 O14 109.22(17) . 1_655 ?
O2 Al1 O8 110.71(16) . 1_655 ?
O14 Al1 O8 106.78(15) 1_655 1_655 ?
O2 Al1 O16 108.17(17) . 2_546 ?
O14 Al1 O16 113.48(16) 1_655 2_546 ?
O8 Al1 O16 108.49(16) 1_655 2_546 ?
P1 O1 Al3 138.9(2) . . ?
P1 O2 Al1 155.8(2) . . ?
P2 O3 Al2 135.31(18) . . ?
P4 O4 Mg1 135.0(2) . . ?
P2 O5 Al3 157.1(2) . . ?
P3 O6 Al2 133.5(2) . . ?
P2 O7 Mg1 132.37(19) . . ?
P4 O8 Al1 135.53(19) . 1_455 ?
P3 O9 Al3 142.4(2) . 4_565 ?
P4 O10 Al2 149.7(2) 4_665 . ?
P4 O11 Al3 141.24(19) . . ?
P1 O12 Al2 164.5(3) . . ?
P1 O13 Mg1 138.8(2) . 2_446 ?
P3 O14 Al1 141.1(2) . 1_455 ?
P3 O15 Mg1 156.4(2) . 2_446 ?
P2 O16 Al1 142.6(2) . 2_556 ?
C1 N1 C2 112.2(4) . . ?
N1 C1 C2 109.8(4) . 3_466 ?
N1 C2 C1 109.8(4) . 3_466 ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        28.27
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         1.335
_refine_diff_density_min         -0.506
_refine_diff_density_rms         0.121
_database_code_depnum_ccdc_archive 'CCDC 1007283'
