# Electronic Supplementary Material (ESI) for RSC Advances.
# 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. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1041971'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H11 Ga N O8 P2'
_chemical_formula_weight         332.80

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'
Ga Ga 0.2307 1.6083 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.3010(7)
_cell_length_b                   8.3046(7)
_cell_length_c                   8.9569(8)
_cell_angle_alpha                66.510(3)
_cell_angle_beta                 65.630(5)
_cell_angle_gamma                76.000(2)
_cell_volume                     513.61(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Chunk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             334
_exptl_absorpt_coefficient_mu    3.019
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            5127
_diffrn_reflns_av_R_equivalents  0.0318
_diffrn_reflns_av_sigmaI/netI    0.0385
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.04
_diffrn_reflns_theta_max         26.49
_reflns_number_total             2129
_reflns_number_gt                1948
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0460P)²+1.2401P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2129
_refine_ls_number_parameters     172
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0983
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_restrained_S_all      1.120
_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
Ga1 Ga 0.50193(5) 0.48463(5) 0.25649(5) 0.01551(15) Uani 1 1 d . . .
P1 P 0.65272(13) 0.25447(12) 0.54267(12) 0.0155(2) Uani 1 1 d . . .
P2 P 0.73600(13) 0.62838(13) -0.13816(12) 0.0153(2) Uani 1 1 d . . .
O1 O 0.2955(4) 0.4589(4) 0.2457(4) 0.0254(7) Uani 1 1 d . . .
O2 O 0.5591(4) 0.2843(4) 0.4145(4) 0.0261(7) Uani 1 1 d . . .
O3 O 0.8000(4) 0.3834(4) 0.4509(4) 0.0323(8) Uani 1 1 d . . .
H3A H 0.8818 0.3514 0.3747 0.048 Uiso 1 1 calc R . .
O4 O 0.7191(5) 0.0664(4) 0.6047(4) 0.0337(8) Uani 1 1 d . . .
O5 O 0.5187(4) 0.3181(4) 0.6939(4) 0.0235(6) Uani 1 1 d . . .
O6 O 0.6839(4) 0.5016(4) 0.0511(4) 0.0255(7) Uani 1 1 d . . .
O7 O 0.9250(4) 0.6643(5) -0.2090(4) 0.0341(8) Uani 1 1 d . . .
O8 O 0.6033(4) 0.7970(4) -0.1347(4) 0.0332(8) Uani 1 1 d . . .
H8A H 0.6461 0.8807 -0.2212 0.050 Uiso 1 1 calc R . .
C1 C -0.0815(16) 0.8228(13) 0.0547(12) 0.034(2) Uani 0.50 1 d P . .
C2 C -0.0059(18) 0.9343(17) -0.1419(16) 0.050(3) Uani 0.50 1 d PU . .
C3 C 0.1553(12) 0.9104(15) 0.0945(13) 0.038(2) Uani 0.50 1 d P . .
C4 C 0.2230(14) 1.022(2) -0.0998(16) 0.065(4) Uani 0.50 1 d P . .
C5 C -0.1304(16) 1.0910(13) 0.1320(13) 0.044(3) Uani 0.50 1 d P . .
C6 C -0.059(2) 1.2009(15) -0.0630(15) 0.063(4) Uani 0.50 1 d P . .
C7 C -0.1238(10) 0.7966(8) 0.3528(7) 0.0540(17) Uani 1 1 d . . .
N1 N -0.0582(5) 0.9077(5) 0.1604(5) 0.0257(8) 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
Ga1 O6 1.814(3) . ?
Ga1 O2 1.814(3) . ?
Ga1 O5 1.814(3) 2_666 ?
Ga1 O1 1.822(3) . ?
P1 O4 1.482(3) . ?
P1 O5 1.547(3) . ?
P1 O2 1.549(3) . ?
P1 O3 1.555(3) . ?
P2 O7 1.486(3) . ?
P2 O6 1.537(3) . ?
P2 O1 1.542(3) 2_665 ?
P2 O8 1.560(3) . ?
O1 P2 1.542(3) 2_665 ?
O3 H3A 0.8200 . ?
O5 Ga1 1.814(3) 2_666 ?
O8 H8A 0.8200 . ?
C1 C6 1.164(18) 2_575 ?
C1 N1 1.477(9) . ?
C1 C2 1.556(15) . ?
C1 C4 1.580(19) 2_575 ?
C2 C5 1.134(17) 2_575 ?
C2 N1 1.457(12) 2_575 ?
C2 C3 1.616(18) 2_575 ?
C3 C6 1.52(2) 2_575 ?
C3 C4 1.536(14) . ?
C3 C2 1.616(18) 2_575 ?
C3 N1 1.623(10) . ?
C4 C5 1.52(2) 2_575 ?
C4 N1 1.575(11) 2_575 ?
C4 C1 1.580(19) 2_575 ?
C5 C2 1.134(17) 2_575 ?
C5 N1 1.456(10) . ?
C5 C4 1.52(2) 2_575 ?
C5 C6 1.540(15) . ?
C6 C1 1.164(18) 2_575 ?
C6 N1 1.422(12) 2_575 ?
C6 C3 1.52(2) 2_575 ?
C7 N1 1.523(6) . ?
N1 C6 1.422(12) 2_575 ?
N1 C2 1.457(12) 2_575 ?
N1 C4 1.575(11) 2_575 ?

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
O6 Ga1 O2 105.72(14) . . ?
O6 Ga1 O5 108.10(13) . 2_666 ?
O2 Ga1 O5 113.35(13) . 2_666 ?
O6 Ga1 O1 111.02(13) . . ?
O2 Ga1 O1 107.70(14) . . ?
O5 Ga1 O1 110.87(14) 2_666 . ?
O4 P1 O5 112.25(18) . . ?
O4 P1 O2 110.29(19) . . ?
O5 P1 O2 108.00(18) . . ?
O4 P1 O3 113.8(2) . . ?
O5 P1 O3 103.79(17) . . ?
O2 P1 O3 108.30(18) . . ?
O7 P2 O6 111.05(19) . . ?
O7 P2 O1 110.34(18) . 2_665 ?
O6 P2 O1 107.44(17) . 2_665 ?
O7 P2 O8 113.38(19) . . ?
O6 P2 O8 105.86(17) . . ?
O1 P2 O8 108.51(18) 2_665 . ?
P2 O1 Ga1 130.14(18) 2_665 . ?
P1 O2 Ga1 130.94(18) . . ?
P1 O3 H3A 109.5 . . ?
P1 O5 Ga1 131.87(18) . 2_666 ?
P2 O6 Ga1 137.86(19) . . ?
P2 O8 H8A 109.5 . . ?
C6 C1 N1 63.9(8) 2_575 . ?
C6 C1 C2 90.4(10) 2_575 . ?
N1 C1 C2 109.9(7) . . ?
C6 C1 C4 123.3(11) 2_575 2_575 ?
N1 C1 C4 61.9(6) . 2_575 ?
C2 C1 C4 92.8(9) . 2_575 ?
C5 C2 N1 67.0(8) 2_575 2_575 ?
C5 C2 C1 88.8(11) 2_575 . ?
N1 C2 C1 109.2(8) 2_575 . ?
C5 C2 C3 125.3(11) 2_575 2_575 ?
N1 C2 C3 63.5(6) 2_575 2_575 ?
C1 C2 C3 86.6(9) . 2_575 ?
C6 C3 C4 91.8(9) 2_575 . ?
C6 C3 C2 103.9(8) 2_575 2_575 ?
C4 C3 C2 92.1(9) . 2_575 ?
C6 C3 N1 53.6(6) 2_575 . ?
C4 C3 N1 108.7(7) . . ?
C2 C3 N1 53.5(5) 2_575 . ?
C5 C4 C3 88.3(9) 2_575 . ?
C5 C4 N1 56.1(6) 2_575 2_575 ?
C3 C4 N1 107.8(7) . 2_575 ?
C5 C4 C1 106.6(8) 2_575 2_575 ?
C3 C4 C1 88.5(9) . 2_575 ?
N1 C4 C1 55.8(5) 2_575 2_575 ?
C2 C5 N1 67.2(8) 2_575 . ?
C2 C5 C4 129.2(11) 2_575 2_575 ?
N1 C5 C4 64.0(6) . 2_575 ?
C2 C5 C6 92.4(12) 2_575 . ?
N1 C5 C6 110.4(7) . . ?
C4 C5 C6 91.9(10) 2_575 . ?
C1 C6 N1 68.8(8) 2_575 2_575 ?
C1 C6 C3 130.8(11) 2_575 2_575 ?
N1 C6 C3 66.7(8) 2_575 2_575 ?
C1 C6 C5 88.5(11) 2_575 . ?
N1 C6 C5 110.3(8) 2_575 . ?
C3 C6 C5 87.9(10) 2_575 . ?
C6 N1 C5 139.3(6) 2_575 . ?
C6 N1 C2 118.3(9) 2_575 2_575 ?
C5 N1 C2 45.8(7) . 2_575 ?
C6 N1 C1 47.3(8) 2_575 . ?
C5 N1 C1 115.8(7) . . ?
C2 N1 C1 140.7(6) 2_575 . ?
C6 N1 C7 109.2(6) 2_575 . ?
C5 N1 C7 111.5(5) . . ?
C2 N1 C7 108.4(6) 2_575 . ?
C1 N1 C7 110.9(5) . . ?
C6 N1 C4 107.7(9) 2_575 2_575 ?
C5 N1 C4 59.9(8) . 2_575 ?
C2 N1 C4 104.6(8) 2_575 2_575 ?
C1 N1 C4 62.3(8) . 2_575 ?
C7 N1 C4 108.2(5) . 2_575 ?
C6 N1 C3 59.6(9) 2_575 . ?
C5 N1 C3 105.4(7) . . ?
C2 N1 C3 63.0(7) 2_575 . ?
C1 N1 C3 104.3(7) . . ?
C7 N1 C3 108.3(5) . . ?
C4 N1 C3 143.4(6) 2_575 . ?

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
O3 H3A O7 0.82 1.70 2.496(4) 163.9 2_765
O8 H8A O4 0.82 1.71 2.530(5) 175.1 1_564

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.49
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.628
_refine_diff_density_min         -0.639
_refine_diff_density_rms         0.133
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1041972'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C4 H10.50 Ga3 N O13.25 P3'
_chemical_formula_weight         586.70

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'
Ga Ga 0.2307 1.6083 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   8.6814(7)
_cell_length_b                   9.2316(8)
_cell_length_c                   9.5849(3)
_cell_angle_alpha                100.270(3)
_cell_angle_beta                 94.600(4)
_cell_angle_gamma                92.960(6)
_cell_volume                     751.72(9)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Chunk
_exptl_crystal_colour            colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.592
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             571
_exptl_absorpt_coefficient_mu    5.729
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7034
_diffrn_reflns_av_R_equivalents  0.0710
_diffrn_reflns_av_sigmaI/netI    0.0857
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.06
_diffrn_reflns_theta_max         26.00
_reflns_number_total             2956
_reflns_number_gt                2734
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0557P)²+0.3437P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2956
_refine_ls_number_parameters     226
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0452
_refine_ls_wR_factor_ref         0.1266
_refine_ls_wR_factor_gt          0.1242
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_restrained_S_all      1.136
_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
Ga1 Ga 0.63029(6) 0.16547(5) 0.14502(5) 0.00810(18) Uani 1 1 d . . .
Ga2 Ga 0.59314(6) -0.38971(5) 0.30737(5) 0.00700(18) Uani 1 1 d . . .
Ga3 Ga 0.77409(6) -0.43549(6) -0.13305(5) 0.00742(18) Uani 1 1 d . . .
P1 P 0.86400(14) 0.43301(13) 0.15999(13) 0.0085(3) Uani 1 1 d . . .
P2 P 0.43990(14) 0.30388(13) 0.36515(12) 0.0076(3) Uani 1 1 d . . .
P3 P 0.64200(14) -0.18206(13) 0.08304(13) 0.0077(3) Uani 1 1 d . . .
O1 O 1.0359(4) 0.4575(4) 0.2072(3) 0.0118(7) Uani 1 1 d . . .
O1W O 1.148(3) 0.606(2) 0.474(2) 0.057(6) Uani 0.25 1 d P . .
O2 O 0.7864(4) 0.5547(4) 0.2530(4) 0.0140(8) Uani 1 1 d . . .
O3 O 0.8261(4) 0.4316(4) 0.0013(4) 0.0133(8) Uani 1 1 d . . .
O4 O 0.8100(4) 0.2786(4) 0.1895(4) 0.0124(7) Uani 1 1 d . . .
O5 O 0.5058(4) 0.1586(4) 0.2892(4) 0.0138(8) Uani 1 1 d . . .
O6 O 0.4085(4) 0.2721(4) 0.5132(3) 0.0109(7) Uani 1 1 d . . .
O7 O 0.2901(4) 0.3310(4) 0.2859(4) 0.0169(8) Uani 1 1 d . . .
O8 O 0.5654(4) 0.4270(4) 0.3734(4) 0.0131(8) Uani 1 1 d . . .
O9 O 0.6886(4) -0.0201(4) 0.0805(4) 0.0157(8) Uani 1 1 d . . .
O10 O 0.7654(4) -0.2715(4) 0.0105(4) 0.0158(8) Uani 1 1 d . . .
O11 O 0.4794(4) -0.2291(4) 0.0022(4) 0.0186(8) Uani 1 1 d . . .
O12 O 0.6306(4) -0.2045(4) 0.2353(4) 0.0124(7) Uani 1 1 d . . .
O13 O 0.4039(4) -0.4273(4) 0.1877(4) 0.0163(8) Uani 1 1 d . . .
C1 C -0.0245(9) 0.8502(9) 0.4272(11) 0.063(3) Uani 1 1 d . . .
H1A H -0.1224 0.8533 0.3718 0.075 Uiso 1 1 calc R . .
H1B H 0.0058 0.7493 0.4092 0.075 Uiso 1 1 calc R . .
C2 C 0.0464(9) 1.1058(10) 0.4176(10) 0.058(2) Uani 1 1 d . . .
H2A H 0.1238 1.1739 0.3925 0.069 Uiso 1 1 calc R . .
H2B H -0.0501 1.1142 0.3621 0.069 Uiso 1 1 calc R . .
C3 C 0.0910(12) 0.9223(16) 0.2174(9) 0.121(6) Uani 1 1 d . . .
H3A H 0.1209 0.8246 0.1832 0.182 Uiso 1 1 calc R . .
H3B H 0.1609 0.9932 0.1887 0.182 Uiso 1 1 calc R . .
H3C H -0.0124 0.9323 0.1784 0.182 Uiso 1 1 calc R . .
C4 C 0.2568(8) 0.9308(9) 0.4424(10) 0.053(2) Uani 1 1 d . . .
H4A H 0.2826 0.8305 0.4143 0.080 Uiso 1 1 calc R . .
H4B H 0.2599 0.9547 0.5443 0.080 Uiso 1 1 calc R . .
H4C H 0.3302 0.9956 0.4096 0.080 Uiso 1 1 calc R . .
N1 N 0.0968(6) 0.9490(8) 0.3780(6) 0.0436(16) 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
Ga1 O4 1.809(3) . ?
Ga1 O9 1.826(3) . ?
Ga1 O5 1.829(3) . ?
Ga1 O11 1.839(4) 2_655 ?
Ga2 O6 1.864(3) 2_656 ?
Ga2 O2 1.867(3) 1_545 ?
Ga2 O13 1.906(3) . ?
Ga2 O8 1.919(3) 1_545 ?
Ga2 O12 1.977(3) . ?
Ga3 O1 1.854(3) 2_755 ?
Ga3 O10 1.865(3) . ?
Ga3 O13 1.923(3) 2_645 ?
Ga3 O7 1.953(3) 2_655 ?
Ga3 O3 1.973(3) 1_545 ?
P1 O1 1.518(3) . ?
P1 O2 1.525(4) . ?
P1 O3 1.528(4) . ?
P1 O4 1.558(3) . ?
P2 O7 1.508(4) . ?
P2 O8 1.521(3) . ?
P2 O6 1.542(3) . ?
P2 O5 1.567(4) . ?
P3 O12 1.520(3) . ?
P3 O10 1.523(4) . ?
P3 O9 1.534(3) . ?
P3 O11 1.556(4) . ?
O1 Ga3 1.854(3) 2_755 ?
O2 Ga2 1.867(3) 1_565 ?
O3 Ga3 1.973(3) 1_565 ?
O6 Ga2 1.864(3) 2_656 ?
O7 Ga3 1.953(3) 2_655 ?
O8 Ga2 1.919(3) 1_565 ?
O11 Ga1 1.839(4) 2_655 ?
O13 Ga3 1.923(3) 2_645 ?
C1 C2 1.501(13) 2_576 ?
C1 N1 1.515(9) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 C1 1.501(13) 2_576 ?
C2 N1 1.526(11) . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 N1 1.511(10) . ?
C3 H3A 0.9600 . ?
C3 H3B 0.9600 . ?
C3 H3C 0.9600 . ?
C4 N1 1.505(9) . ?
C4 H4A 0.9600 . ?
C4 H4B 0.9600 . ?
C4 H4C 0.9600 . ?

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
O4 Ga1 O9 104.86(16) . . ?
O4 Ga1 O5 116.73(16) . . ?
O9 Ga1 O5 108.88(15) . . ?
O4 Ga1 O11 108.27(15) . 2_655 ?
O9 Ga1 O11 108.61(17) . 2_655 ?
O5 Ga1 O11 109.20(17) . 2_655 ?
O6 Ga2 O2 116.37(16) 2_656 1_545 ?
O6 Ga2 O13 118.22(16) 2_656 . ?
O2 Ga2 O13 125.10(16) 1_545 . ?
O6 Ga2 O8 94.84(14) 2_656 1_545 ?
O2 Ga2 O8 88.71(15) 1_545 1_545 ?
O13 Ga2 O8 92.15(15) . 1_545 ?
O6 Ga2 O12 86.72(14) 2_656 . ?
O2 Ga2 O12 88.60(15) 1_545 . ?
O13 Ga2 O12 89.06(15) . . ?
O8 Ga2 O12 177.28(14) 1_545 . ?
O1 Ga3 O10 115.42(15) 2_755 . ?
O1 Ga3 O13 124.61(16) 2_755 2_645 ?
O10 Ga3 O13 119.90(16) . 2_645 ?
O1 Ga3 O7 88.92(15) 2_755 2_655 ?
O10 Ga3 O7 94.00(16) . 2_655 ?
O13 Ga3 O7 89.99(15) 2_645 2_655 ?
O1 Ga3 O3 91.02(15) 2_755 1_545 ?
O10 Ga3 O3 93.86(15) . 1_545 ?
O13 Ga3 O3 82.90(14) 2_645 1_545 ?
O7 Ga3 O3 171.32(15) 2_655 1_545 ?
O1 P1 O2 105.9(2) . . ?
O1 P1 O3 113.4(2) . . ?
O2 P1 O3 112.2(2) . . ?
O1 P1 O4 107.0(2) . . ?
O2 P1 O4 110.6(2) . . ?
O3 P1 O4 107.56(19) . . ?
O7 P2 O8 113.2(2) . . ?
O7 P2 O6 109.7(2) . . ?
O8 P2 O6 112.35(19) . . ?
O7 P2 O5 110.1(2) . . ?
O8 P2 O5 106.9(2) . . ?
O6 P2 O5 104.06(19) . . ?
O12 P3 O10 112.5(2) . . ?
O12 P3 O9 110.32(19) . . ?
O10 P3 O9 105.98(19) . . ?
O12 P3 O11 106.6(2) . . ?
O10 P3 O11 110.5(2) . . ?
O9 P3 O11 111.0(2) . . ?
P1 O1 Ga3 140.2(2) . 2_755 ?
P1 O2 Ga2 142.2(2) . 1_565 ?
P1 O3 Ga3 141.3(2) . 1_565 ?
P1 O4 Ga1 133.0(2) . . ?
P2 O5 Ga1 119.6(2) . . ?
P2 O6 Ga2 134.0(2) . 2_656 ?
P2 O7 Ga3 137.2(2) . 2_655 ?
P2 O8 Ga2 138.5(2) . 1_565 ?
P3 O9 Ga1 140.7(2) . . ?
P3 O10 Ga3 137.9(2) . . ?
P3 O11 Ga1 133.1(2) . 2_655 ?
P3 O12 Ga2 129.1(2) . . ?
Ga2 O13 Ga3 143.4(2) . 2_645 ?
C2 C1 N1 112.9(6) 2_576 . ?
C2 C1 H1A 109.0 2_576 . ?
N1 C1 H1A 109.0 . . ?
C2 C1 H1B 109.0 2_576 . ?
N1 C1 H1B 109.0 . . ?
H1A C1 H1B 107.8 . . ?
C1 C2 N1 113.3(7) 2_576 . ?
C1 C2 H2A 108.9 2_576 . ?
N1 C2 H2A 108.9 . . ?
C1 C2 H2B 108.9 2_576 . ?
N1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 H3A 109.5 . . ?
N1 C3 H3B 109.5 . . ?
H3A C3 H3B 109.5 . . ?
N1 C3 H3C 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
N1 C4 H4A 109.5 . . ?
N1 C4 H4B 109.5 . . ?
H4A C4 H4B 109.5 . . ?
N1 C4 H4C 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C4 N1 C3 110.8(7) . . ?
C4 N1 C1 111.8(6) . . ?
C3 N1 C1 111.0(7) . . ?
C4 N1 C2 112.9(6) . . ?
C3 N1 C2 104.0(8) . . ?
C1 N1 C2 105.9(6) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.916
_refine_diff_density_min         -0.967
_refine_diff_density_rms         0.233
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1041973'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H8.50 F Ga3 N O12.25 P3'
_chemical_formula_weight         611.71

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'
Ga Ga 0.2307 1.6083 '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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_H-M   P-1

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.3128(7)
_cell_length_b                   9.3227(5)
_cell_length_c                   9.3497(3)
_cell_angle_alpha                103.170(3)
_cell_angle_beta                 93.600(4)
_cell_angle_gamma                90.140(5)
_cell_volume                     788.72(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.576
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             593
_exptl_absorpt_coefficient_mu    5.471
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            7581
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0405
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.03
_diffrn_reflns_theta_max         26.00
_reflns_number_total             3106
_reflns_number_gt                2682
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0171P)²+2.8514P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3106
_refine_ls_number_parameters     244
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          0.0419
_refine_ls_R_factor_gt           0.0325
_refine_ls_wR_factor_ref         0.0664
_refine_ls_wR_factor_gt          0.0632
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_restrained_S_all      1.012
_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
Ga1 Ga 0.43464(5) 0.13698(5) 0.58999(5) 0.00981(11) Uani 1 1 d . . .
Ga2 Ga 0.84181(5) 0.37514(5) 0.57661(5) 0.01153(11) Uani 1 1 d . . .
Ga3 Ga 0.61302(5) 0.39625(5) 1.16493(5) 0.01366(12) Uani 1 1 d . . .
P1 P 0.35546(11) -0.16698(11) 0.64834(11) 0.0111(2) Uani 1 1 d . . .
P2 P 0.18078(11) 0.37569(11) 0.59385(11) 0.0101(2) Uani 1 1 d . . .
P3 P 0.62255(11) 0.37697(11) 0.82798(11) 0.0108(2) Uani 1 1 d . . .
O1 O 0.3877(3) -0.2154(3) 0.7947(3) 0.0185(7) Uani 1 1 d . . .
O1W O 0.478(3) 0.514(3) 0.594(2) 0.100(8) Uani 0.25 1 d P . .
O2 O 0.4633(3) -0.2353(3) 0.5369(3) 0.0163(6) Uani 1 1 d . . .
O3 O 0.2037(3) -0.2302(3) 0.5862(3) 0.0175(6) Uani 1 1 d . . .
O4 O 0.3496(3) -0.0004(3) 0.6884(3) 0.0138(6) Uani 1 1 d U . .
O5 O 0.2595(3) 0.2331(3) 0.5638(3) 0.0188(7) Uani 1 1 d . . .
O6 O 0.1752(4) 0.4409(3) 0.4564(3) 0.0231(7) Uani 1 1 d . . .
O7 O 0.0273(3) 0.3434(4) 0.6289(4) 0.0249(7) Uani 1 1 d . . .
O8 O 0.2459(4) 0.4882(3) 0.7270(3) 0.0278(8) Uani 1 1 d . . .
O9 O 0.5034(3) 0.2655(3) 0.7707(3) 0.0181(7) Uani 1 1 d . . .
O10 O 0.7545(3) 0.3536(3) 0.7374(3) 0.0169(6) Uani 1 1 d . . .
O11 O 0.5670(3) 0.5326(3) 0.8355(4) 0.0335(9) Uani 1 1 d . . .
O12 O 0.6787(3) 0.3641(4) 0.9814(3) 0.0286(8) Uani 1 1 d . . .
F1 F 0.3900(2) -0.0170(2) 0.4093(2) 0.0136(5) Uani 1 1 d . . .
C1 C 0.2351(6) 0.0503(8) 0.1257(7) 0.0511(17) Uani 1 1 d . . .
H1A H 0.2947 -0.0214 0.1506 0.061 Uiso 1 1 calc R . .
C2 C 0.2752(7) 0.1240(9) 0.0248(7) 0.0561(19) Uani 1 1 d . . .
H2A H 0.3619 0.1023 -0.0191 0.067 Uiso 1 1 calc R . .
C3 C 0.1900(8) 0.2288(8) -0.0126(7) 0.061(2) Uani 1 1 d . . .
H3A H 0.2166 0.2778 -0.0833 0.073 Uiso 1 1 calc R . .
C4 C 0.0637(8) 0.2620(8) 0.0554(8) 0.063(2) Uani 1 1 d . . .
H4B H 0.0051 0.3356 0.0329 0.076 Uiso 1 1 calc R . .
C5 C 0.0251(7) 0.1861(7) 0.1560(7) 0.0467(15) Uani 1 1 d . . .
H5A H -0.0607 0.2080 0.2016 0.056 Uiso 1 1 calc R . .
C6 C 0.0642(6) -0.0042(7) 0.2974(6) 0.0448(15) Uani 1 1 d . . .
H6A H -0.0270 0.0304 0.3325 0.067 Uiso 1 1 calc R . .
H6B H 0.1348 0.0093 0.3788 0.067 Uiso 1 1 calc R . .
H6C H 0.0557 -0.1070 0.2500 0.067 Uiso 1 1 calc R . .
N1 N 0.1090(5) 0.0800(5) 0.1906(5) 0.0347(10) 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
Ga1 O5 1.893(3) . ?
Ga1 O9 1.907(3) . ?
Ga1 O4 1.934(3) . ?
Ga1 O2 1.946(3) 2_656 ?
Ga1 F1 1.973(2) . ?
Ga1 F1 1.983(2) 2_656 ?
Ga2 O10 1.804(3) . ?
Ga2 O7 1.809(3) 1_655 ?
Ga2 O6 1.816(3) 2_666 ?
Ga2 O3 1.818(3) 2_656 ?
Ga3 O8 1.800(3) 2_667 ?
Ga3 O11 1.804(3) 2_667 ?
Ga3 O1 1.810(3) 2_657 ?
Ga3 O12 1.818(3) . ?
P1 O4 1.514(3) . ?
P1 O2 1.527(3) . ?
P1 O1 1.548(3) . ?
P1 O3 1.555(3) . ?
P2 O5 1.498(3) . ?
P2 O8 1.524(3) . ?
P2 O7 1.530(3) . ?
P2 O6 1.540(3) . ?
P3 O9 1.505(3) . ?
P3 O10 1.524(3) . ?
P3 O12 1.527(3) . ?
P3 O11 1.530(3) . ?
O1 Ga3 1.810(3) 2_657 ?
O1W O1W 1.79(4) 2_666 ?
O2 Ga1 1.946(3) 2_656 ?
O3 Ga2 1.818(3) 2_656 ?
O6 Ga2 1.816(3) 2_666 ?
O7 Ga2 1.809(3) 1_455 ?
O8 Ga3 1.800(3) 2_667 ?
O11 Ga3 1.804(3) 2_667 ?
F1 Ga1 1.983(2) 2_656 ?
C1 N1 1.356(7) . ?
C1 C2 1.357(9) . ?
C1 H1A 0.9300 . ?
C2 C3 1.353(10) . ?
C2 H2A 0.9300 . ?
C3 C4 1.375(10) . ?
C3 H3A 0.9300 . ?
C4 C5 1.364(8) . ?
C4 H4B 0.9300 . ?
C5 N1 1.345(7) . ?
C5 H5A 0.9300 . ?
C6 N1 1.482(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
O5 Ga1 O9 97.59(13) . . ?
O5 Ga1 O4 94.11(12) . . ?
O9 Ga1 O4 92.99(12) . . ?
O5 Ga1 O2 93.88(12) . 2_656 ?
O9 Ga1 O2 95.95(12) . 2_656 ?
O4 Ga1 O2 167.11(12) . 2_656 ?
O5 Ga1 F1 91.73(11) . . ?
O9 Ga1 F1 170.53(11) . . ?
O4 Ga1 F1 84.64(11) . . ?
O2 Ga1 F1 85.03(11) 2_656 . ?
O5 Ga1 F1 171.94(11) . 2_656 ?
O9 Ga1 F1 90.47(11) . 2_656 ?
O4 Ga1 F1 85.64(11) . 2_656 ?
O2 Ga1 F1 85.03(11) 2_656 2_656 ?
F1 Ga1 F1 80.22(10) . 2_656 ?
O10 Ga2 O7 101.03(13) . 1_655 ?
O10 Ga2 O6 112.99(14) . 2_666 ?
O7 Ga2 O6 109.81(15) 1_655 2_666 ?
O10 Ga2 O3 113.75(13) . 2_656 ?
O7 Ga2 O3 104.90(14) 1_655 2_656 ?
O6 Ga2 O3 113.25(13) 2_666 2_656 ?
O8 Ga3 O11 118.21(15) 2_667 2_667 ?
O8 Ga3 O1 111.11(14) 2_667 2_657 ?
O11 Ga3 O1 110.33(14) 2_667 2_657 ?
O8 Ga3 O12 101.65(15) 2_667 . ?
O11 Ga3 O12 110.35(16) 2_667 . ?
O1 Ga3 O12 103.94(15) 2_657 . ?
O4 P1 O2 116.82(16) . . ?
O4 P1 O1 106.18(16) . . ?
O2 P1 O1 110.05(17) . . ?
O4 P1 O3 108.91(16) . . ?
O2 P1 O3 107.64(16) . . ?
O1 P1 O3 106.84(17) . . ?
O5 P2 O8 113.28(17) . . ?
O5 P2 O7 107.87(18) . . ?
O8 P2 O7 106.53(19) . . ?
O5 P2 O6 109.71(17) . . ?
O8 P2 O6 110.10(18) . . ?
O7 P2 O6 109.22(18) . . ?
O9 P3 O10 113.83(17) . . ?
O9 P3 O12 109.84(18) . . ?
O10 P3 O12 104.45(17) . . ?
O9 P3 O11 110.01(18) . . ?
O10 P3 O11 109.18(18) . . ?
O12 P3 O11 109.4(2) . . ?
P1 O1 Ga3 130.90(18) . 2_657 ?
P1 O2 Ga1 126.99(17) . 2_656 ?
P1 O3 Ga2 128.02(18) . 2_656 ?
P1 O4 Ga1 127.75(17) . . ?
P2 O5 Ga1 146.33(19) . . ?
P2 O6 Ga2 135.05(19) . 2_666 ?
P2 O7 Ga2 141.1(2) . 1_455 ?
P2 O8 Ga3 155.2(2) . 2_667 ?
P3 O9 Ga1 139.09(19) . . ?
P3 O10 Ga2 148.83(19) . . ?
P3 O11 Ga3 131.6(2) . 2_667 ?
P3 O12 Ga3 137.7(2) . . ?
Ga1 F1 Ga1 99.78(10) . 2_656 ?
N1 C1 C2 120.7(6) . . ?
N1 C1 H1A 119.7 . . ?
C2 C1 H1A 119.7 . . ?
C3 C2 C1 120.5(6) . . ?
C3 C2 H2A 119.8 . . ?
C1 C2 H2A 119.8 . . ?
C2 C3 C4 119.2(6) . . ?
C2 C3 H3A 120.4 . . ?
C4 C3 H3A 120.4 . . ?
C5 C4 C3 119.4(7) . . ?
C5 C4 H4B 120.3 . . ?
C3 C4 H4B 120.3 . . ?
N1 C5 C4 121.1(6) . . ?
N1 C5 H5A 119.4 . . ?
C4 C5 H5A 119.4 . . ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C5 N1 C1 119.2(5) . . ?
C5 N1 C6 120.6(5) . . ?
C1 N1 C6 120.2(5) . . ?

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.00
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.654
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.112
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1041974'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C6 H9 Ga2 N O12 P3'
_chemical_formula_weight         519.49

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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)/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                   8.5770(5)
_cell_length_b                   20.4760(4)
_cell_length_c                   8.9999(8)
_cell_angle_alpha                90.00
_cell_angle_beta                 111.013(3)
_cell_angle_gamma                90.00
_cell_volume                     1475.48(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Prism
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.339
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1020
_exptl_absorpt_coefficient_mu    4.043
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  0.5298
_exptl_absorpt_correction_T_max  0.6879
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            15445
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_sigmaI/netI    0.0547
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         3.14
_diffrn_reflns_theta_max         27.48
_reflns_number_total             3366
_reflns_number_gt                2672
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0316P)²+0.9328P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3366
_refine_ls_number_parameters     217
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0437
_refine_ls_wR_factor_ref         0.0865
_refine_ls_wR_factor_gt          0.0806
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_restrained_S_all      1.095
_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
Ga1 Ga 1.20058(5) 0.79038(2) 1.16878(5) 0.01457(13) Uani 1 1 d . . .
Ga2 Ga 0.70710(5) 0.78344(2) 0.83147(5) 0.01262(12) Uani 1 1 d . . .
P1 P 0.93598(12) 0.90118(5) 1.00768(13) 0.0152(2) Uani 1 1 d . . .
P2 P 0.91696(13) 0.69190(5) 1.10317(13) 0.0136(2) Uani 1 1 d . . .
P3 P 0.43705(12) 0.75230(5) 0.49835(12) 0.0134(2) Uani 1 1 d . . .
O1 O 0.8867(4) 0.95485(14) 1.1033(4) 0.0253(7) Uani 1 1 d . . .
H1A H 0.9320 0.9893 1.0956 0.038 Uiso 1 1 calc R . .
O2 O 0.9997(4) 0.93116(15) 0.8891(4) 0.0356(9) Uani 1 1 d . . .
O3 O 0.7814(4) 0.86160(15) 0.9315(4) 0.0326(8) Uani 1 1 d . . .
O4 O 1.0699(4) 0.86132(16) 1.1292(4) 0.0364(9) Uani 1 1 d . . .
O5 O 1.0908(3) 0.71365(14) 1.1120(4) 0.0217(7) Uani 1 1 d . . .
O6 O 0.8823(3) 0.72099(14) 1.2411(3) 0.0201(7) Uani 1 1 d . . .
O7 O 0.7888(3) 0.70642(13) 0.9404(3) 0.0181(6) Uani 1 1 d . . .
O8 O 0.9234(4) 0.61603(14) 1.1127(3) 0.0231(7) Uani 1 1 d . . .
H8A H 0.9484 0.6046 1.2056 0.035 Uiso 1 1 calc R . .
O9 O 0.5454(3) 0.79541(14) 0.6309(3) 0.0194(7) Uani 1 1 d . . .
O10 O 0.5288(4) 0.71290(14) 0.4162(4) 0.0238(7) Uani 1 1 d . . .
O11 O 0.3447(4) 0.70238(14) 0.5641(4) 0.0225(7) Uani 1 1 d . . .
O12 O 0.3112(3) 0.79841(14) 0.3815(3) 0.0231(7) Uani 1 1 d . . .
C1 C 0.6515(8) -0.0330(3) 0.3517(7) 0.064(2) Uani 1 1 d . . .
H1B H 0.6756 -0.0675 0.4236 0.076 Uiso 1 1 calc R . .
C2 C 0.5712(7) -0.0450(3) 0.1941(6) 0.0507(16) Uani 1 1 d . . .
H2A H 0.5376 -0.0872 0.1590 0.061 Uiso 1 1 calc R . .
C3 C 0.6670(7) 0.0769(3) 0.3050(7) 0.0470(15) Uani 1 1 d . . .
H3A H 0.7004 0.1187 0.3434 0.056 Uiso 1 1 calc R . .
C4 C 0.5887(7) 0.0667(2) 0.1469(6) 0.0400(13) Uani 1 1 d . . .
H4A H 0.5676 0.1021 0.0779 0.048 Uiso 1 1 calc R . .
C5 C 0.5397(5) 0.0059(2) 0.0861(5) 0.0221(10) Uani 1 1 d . . .
C6 C 0.7892(9) 0.0394(3) 0.5767(7) 0.085(3) Uani 1 1 d . . .
H6A H 0.8110 0.0853 0.5934 0.128 Uiso 1 1 calc R . .
H6B H 0.8930 0.0160 0.6104 0.128 Uiso 1 1 calc R . .
H6C H 0.7236 0.0250 0.6374 0.128 Uiso 1 1 calc R . .
N1 N 0.6958(6) 0.0269(2) 0.4044(5) 0.0456(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
Ga1 O4 1.791(3) . ?
Ga1 O5 1.809(3) . ?
Ga1 O11 1.809(3) 4_676 ?
Ga1 O12 1.814(3) 1_656 ?
Ga2 O3 1.835(3) . ?
Ga2 O9 1.856(3) . ?
Ga2 O7 1.857(3) . ?
Ga2 O10 1.939(3) 4_576 ?
Ga2 O6 1.951(3) 4_575 ?
P1 O2 1.494(3) . ?
P1 O3 1.494(3) . ?
P1 O4 1.510(3) . ?
P1 O1 1.545(3) . ?
P2 O6 1.499(3) . ?
P2 O7 1.512(3) . ?
P2 O5 1.531(3) . ?
P2 O8 1.556(3) . ?
P3 O10 1.495(3) . ?
P3 O9 1.507(3) . ?
P3 O12 1.532(3) . ?
P3 O11 1.536(3) . ?
O1 H1A 0.8200 . ?
O6 Ga2 1.951(3) 4_576 ?
O8 H8A 0.8200 . ?
O10 Ga2 1.939(3) 4_575 ?
O11 Ga1 1.809(3) 4_475 ?
O12 Ga1 1.814(3) 1_454 ?
C1 N1 1.320(7) . ?
C1 C2 1.358(7) . ?
C1 H1B 0.9300 . ?
C2 C5 1.383(6) . ?
C2 H2A 0.9300 . ?
C3 N1 1.324(7) . ?
C3 C4 1.354(7) . ?
C3 H3A 0.9300 . ?
C4 C5 1.365(6) . ?
C4 H4A 0.9300 . ?
C5 C5 1.472(9) 3_655 ?
C6 N1 1.491(7) . ?
C6 H6A 0.9600 . ?
C6 H6B 0.9600 . ?
C6 H6C 0.9600 . ?

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
O4 Ga1 O5 115.02(15) . . ?
O4 Ga1 O11 109.02(15) . 4_676 ?
O5 Ga1 O11 107.92(13) . 4_676 ?
O4 Ga1 O12 100.93(14) . 1_656 ?
O5 Ga1 O12 113.54(14) . 1_656 ?
O11 Ga1 O12 110.23(14) 4_676 1_656 ?
O3 Ga2 O9 111.64(14) . . ?
O3 Ga2 O7 118.87(14) . . ?
O9 Ga2 O7 129.40(12) . . ?
O3 Ga2 O10 87.55(13) . 4_576 ?
O9 Ga2 O10 87.56(13) . 4_576 ?
O7 Ga2 O10 91.54(12) . 4_576 ?
O3 Ga2 O6 93.52(13) . 4_575 ?
O9 Ga2 O6 91.12(12) . 4_575 ?
O7 Ga2 O6 88.81(12) . 4_575 ?
O10 Ga2 O6 178.54(13) 4_576 4_575 ?
O2 P1 O3 112.77(19) . . ?
O2 P1 O4 111.2(2) . . ?
O3 P1 O4 111.0(2) . . ?
O2 P1 O1 110.40(18) . . ?
O3 P1 O1 105.44(17) . . ?
O4 P1 O1 105.66(18) . . ?
O6 P2 O7 115.64(16) . . ?
O6 P2 O5 108.66(17) . . ?
O7 P2 O5 110.42(17) . . ?
O6 P2 O8 111.41(17) . . ?
O7 P2 O8 104.40(16) . . ?
O5 P2 O8 105.84(17) . . ?
O10 P3 O9 115.04(17) . . ?
O10 P3 O12 111.06(17) . . ?
O9 P3 O12 105.36(17) . . ?
O10 P3 O11 105.51(17) . . ?
O9 P3 O11 109.96(17) . . ?
O12 P3 O11 109.92(17) . . ?
P1 O1 H1A 109.5 . . ?
P1 O3 Ga2 142.5(2) . . ?
P1 O4 Ga1 147.3(2) . . ?
P2 O5 Ga1 131.78(18) . . ?
P2 O6 Ga2 137.53(18) . 4_576 ?
P2 O7 Ga2 133.17(18) . . ?
P2 O8 H8A 109.5 . . ?
P3 O9 Ga2 136.55(18) . . ?
P3 O10 Ga2 143.41(19) . 4_575 ?
P3 O11 Ga1 133.58(18) . 4_475 ?
P3 O12 Ga1 129.91(19) . 1_454 ?
N1 C1 C2 121.1(6) . . ?
N1 C1 H1B 119.5 . . ?
C2 C1 H1B 119.5 . . ?
C1 C2 C5 119.7(5) . . ?
C1 C2 H2A 120.1 . . ?
C5 C2 H2A 120.1 . . ?
N1 C3 C4 119.5(5) . . ?
N1 C3 H3A 120.2 . . ?
C4 C3 H3A 120.2 . . ?
C3 C4 C5 121.9(5) . . ?
C3 C4 H4A 119.1 . . ?
C5 C4 H4A 119.1 . . ?
C4 C5 C2 116.8(5) . . ?
C4 C5 C5 122.1(5) . 3_655 ?
C2 C5 C5 121.1(5) . 3_655 ?
N1 C6 H6A 109.5 . . ?
N1 C6 H6B 109.5 . . ?
H6A C6 H6B 109.5 . . ?
N1 C6 H6C 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C1 N1 C3 121.0(5) . . ?
C1 N1 C6 120.8(5) . . ?
C3 N1 C6 118.1(5) . . ?

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
O1 H1A O2 0.82 1.72 2.521(4) 165.1 3_777
O8 H8A O2 0.82 1.71 2.527(4) 171.4 4_576

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.555
_refine_diff_density_rms         0.124
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 1041975'
_audit_update_record             
;
2015-01-04 deposited with the CCDC.
2015-08-26 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
; 
 ? 
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H30 Ga7 N4 O34 P8'
_chemical_formula_weight         1486.18

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'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   C2/c

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

_cell_length_a                   13.9877(8)
_cell_length_b                   11.9198(4)
_cell_length_c                   23.0454(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 104.269(3)
_cell_angle_gamma                90.00
_cell_volume                     3723.8(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    ?
_cell_measurement_theta_min      ?
_cell_measurement_theta_max      ?

_exptl_crystal_description       Block
_exptl_crystal_colour            Colorless
_exptl_crystal_size_max          ?
_exptl_crystal_size_mid          ?
_exptl_crystal_size_min          ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.651
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2908
_exptl_absorpt_coefficient_mu    5.456
_exptl_absorpt_correction_type   ?
_exptl_absorpt_correction_T_min  ?
_exptl_absorpt_correction_T_max  ?
_exptl_absorpt_process_details   ?

_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  ?
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            18109
_diffrn_reflns_av_R_equivalents  0.0721
_diffrn_reflns_av_sigmaI/netI    0.0548
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         26.50
_reflns_number_total             3869
_reflns_number_gt                3173
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_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)+(0.0143P)²+34.3151P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         3869
_refine_ls_number_parameters     303
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0627
_refine_ls_R_factor_gt           0.0444
_refine_ls_wR_factor_ref         0.0799
_refine_ls_wR_factor_gt          0.0752
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_restrained_S_all      1.134
_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
Ga1 Ga -0.12785(4) -0.45824(5) 0.55326(3) 0.00926(14) Uani 1 1 d . . .
Ga2 Ga -0.15940(4) -0.32480(5) 0.41129(3) 0.00904(14) Uani 1 1 d . . .
Ga3 Ga -0.00245(4) 0.13163(5) 0.43825(3) 0.00958(14) Uani 1 1 d . . .
Ga4 Ga 0.0000 0.36604(7) 0.2500 0.01016(19) Uani 1 2 d S . .
P1 P 0.04793(10) -0.34307(11) 0.50613(6) 0.0098(3) Uani 1 1 d . . .
P2 P -0.03911(11) -0.44216(12) 0.33069(7) 0.0136(3) Uani 1 1 d D . .
P3 P -0.14912(10) -0.07031(11) 0.43814(6) 0.0087(3) Uani 1 1 d . . .
P4 P 0.11594(10) 0.22948(11) 0.35888(6) 0.0092(3) Uani 1 1 d . . .
O1 O -0.2590(3) -0.5006(3) 0.56720(16) 0.0108(8) Uani 1 1 d . . .
O2 O -0.0624(3) -0.5412(3) 0.62771(17) 0.0154(9) Uani 1 1 d . . .
O3 O -0.1377(3) -0.6015(3) 0.50851(16) 0.0118(8) Uani 1 1 d . . .
O4 O -0.1336(3) -0.3194(3) 0.59499(19) 0.0229(10) Uani 1 1 d . . .
O5 O 0.0014(3) -0.4171(3) 0.54509(17) 0.0139(9) Uani 1 1 d . . .
O6 O -0.1935(3) -0.3821(3) 0.47829(16) 0.0140(8) Uani 1 1 d . . .
O7 O -0.0236(3) -0.3022(3) 0.44918(17) 0.0134(8) Uani 1 1 d . . .
O8 O -0.2962(3) -0.3487(3) 0.36525(16) 0.0126(8) Uani 1 1 d . . .
O9 O -0.1271(3) -0.4315(3) 0.35954(17) 0.0171(9) Uani 1 1 d . . .
O10 O -0.0685(3) -0.5462(3) 0.28953(18) 0.0231(10) Uani 1 1 d D . .
O11 O -0.0356(3) -0.3365(3) 0.29274(18) 0.0246(10) Uani 1 1 d . . .
O12 O -0.1688(3) -0.1699(3) 0.39573(16) 0.0118(8) Uani 1 1 d . . .
O13 O -0.0670(3) -0.0015(3) 0.42189(17) 0.0149(9) Uani 1 1 d . . .
O14 O 0.1137(3) 0.1089(3) 0.49545(16) 0.0128(8) Uani 1 1 d . . .
O15 O -0.0881(3) 0.2338(3) 0.45681(17) 0.0143(9) Uani 1 1 d . . .
O16 O 0.0255(3) 0.1584(3) 0.36547(16) 0.0143(9) Uani 1 1 d . . .
O17 O 0.0926(3) 0.2747(3) 0.29491(18) 0.0205(10) Uani 1 1 d . . .
C1 C -0.1639(9) -0.9524(12) 0.7518(4) 0.118(5) Uani 1 1 d . . .
H1A H -0.2074 -0.9332 0.7766 0.177 Uiso 1 1 calc R . .
H1B H -0.1013 -0.9164 0.7669 0.177 Uiso 1 1 calc R . .
H1C H -0.1549 -1.0322 0.7520 0.177 Uiso 1 1 calc R . .
C2 C -0.2828(8) -0.8094(10) 0.6764(6) 0.043(3) Uani 0.70 1 d P . .
C2' C -0.2271(18) -0.801(2) 0.7147(12) 0.032(6) Uani 0.30 1 d P . .
C3 C -0.2383(8) -0.7120(7) 0.6635(4) 0.066(3) Uani 1 1 d . . .
C4 C -0.1209(6) -0.8979(7) 0.6608(4) 0.031(2) Uani 0.80 1 d P . .
C4' C -0.186(3) -0.911(3) 0.6201(16) 0.030(8) Uani 0.20 1 d PU . .
C5 C -0.1563(6) -0.8374(7) 0.6021(4) 0.048(2) Uani 1 1 d . . .
N1 N -0.2071(5) -0.9142(5) 0.6899(3) 0.0444(17) Uani 1 1 d . . .
N2 N -0.1981(4) -0.7243(5) 0.6108(3) 0.0420(17) Uani 1 1 d . . .
H2A H -0.1503 -0.6728 0.6132 0.050 Uiso 1 1 calc R . .
H2B H -0.2463 -0.7084 0.5781 0.050 Uiso 1 1 calc R . .


_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 O4 1.925(4) . ?
Ga1 O5 1.927(4) . ?
Ga1 O6 1.967(4) . ?
Ga1 O3 1.982(4) . ?
Ga1 O2 1.997(4) . ?
Ga1 O1 2.003(3) . ?
Ga2 O6 1.855(4) . ?
Ga2 O9 1.874(4) . ?
Ga2 O12 1.880(4) . ?
Ga2 O7 1.903(4) . ?
Ga2 O8 1.967(4) . ?
Ga3 O13 1.819(4) . ?
Ga3 O15 1.832(4) . ?
Ga3 O16 1.841(4) . ?
Ga3 O14 1.842(4) . ?
Ga4 O10 1.809(4) 2_565 ?
Ga4 O10 1.809(4) 1_565 ?
Ga4 O17 1.810(4) 2 ?
Ga4 O17 1.810(4) . ?
P1 O5 1.516(4) . ?
P1 O7 1.521(4) . ?
P1 O3 1.528(4) 5_546 ?
P1 O15 1.582(4) 5_556 ?
P2 O2 1.517(4) 5_546 ?
P2 O11 1.541(4) . ?
P2 O9 1.542(4) . ?
P2 O10 1.553(4) . ?
P3 O1 1.518(4) 7_446 ?
P3 O12 1.519(4) . ?
P3 O13 1.531(4) . ?
P3 O14 1.557(4) 5_556 ?
P4 O4 1.487(4) 5_556 ?
P4 O8 1.521(4) 3 ?
P4 O17 1.527(4) . ?
P4 O16 1.561(4) . ?
O1 P3 1.518(4) 7_446 ?
O2 P2 1.517(4) 5_546 ?
O3 P1 1.528(4) 5_546 ?
O4 P4 1.487(4) 5_556 ?
O8 P4 1.521(4) 3_445 ?
O10 Ga4 1.809(4) 1_545 ?
O14 P3 1.557(4) 5_556 ?
O15 P1 1.582(4) 5_556 ?
C1 N1 1.476(11) . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C2 C2' 1.03(3) . ?
C2 C3 1.383(14) . ?
C2 N1 1.618(14) . ?
C2' N1 1.52(3) . ?
C2' C3 1.56(2) . ?
C3 N2 1.466(10) . ?
C4 C4' 1.15(4) . ?
C4 C5 1.505(11) . ?
C4 N1 1.531(10) . ?
C4' C5 1.10(4) . ?
C4' N1 1.71(4) . ?
C5 N2 1.502(9) . ?
N2 H2A 0.9000 . ?
N2 H2B 0.9000 . ?

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
O4 Ga1 O5 89.20(16) . . ?
O4 Ga1 O6 88.52(17) . . ?
O5 Ga1 O6 92.46(16) . . ?
O4 Ga1 O3 173.81(16) . . ?
O5 Ga1 O3 96.58(15) . . ?
O6 Ga1 O3 89.03(16) . . ?
O4 Ga1 O2 93.63(17) . . ?
O5 Ga1 O2 88.11(15) . . ?
O6 Ga1 O2 177.78(16) . . ?
O3 Ga1 O2 88.77(15) . . ?
O4 Ga1 O1 89.07(16) . . ?
O5 Ga1 O1 176.49(16) . . ?
O6 Ga1 O1 90.55(15) . . ?
O3 Ga1 O1 85.27(15) . . ?
O2 Ga1 O1 88.95(15) . . ?
O6 Ga2 O9 115.58(17) . . ?
O6 Ga2 O12 120.02(16) . . ?
O9 Ga2 O12 124.20(17) . . ?
O6 Ga2 O7 95.87(16) . . ?
O9 Ga2 O7 91.05(16) . . ?
O12 Ga2 O7 87.91(15) . . ?
O6 Ga2 O8 88.87(16) . . ?
O9 Ga2 O8 85.01(16) . . ?
O12 Ga2 O8 91.52(15) . . ?
O7 Ga2 O8 174.82(16) . . ?
O13 Ga3 O15 107.97(16) . . ?
O13 Ga3 O16 99.70(16) . . ?
O15 Ga3 O16 113.28(17) . . ?
O13 Ga3 O14 109.00(17) . . ?
O15 Ga3 O14 116.28(16) . . ?
O16 Ga3 O14 109.24(16) . . ?
O10 Ga4 O10 109.3(3) 2_565 1_565 ?
O10 Ga4 O17 116.96(18) 2_565 2 ?
O10 Ga4 O17 104.06(17) 1_565 2 ?
O10 Ga4 O17 104.06(17) 2_565 . ?
O10 Ga4 O17 116.96(18) 1_565 . ?
O17 Ga4 O17 106.0(3) 2 . ?
O5 P1 O7 114.2(2) . . ?
O5 P1 O3 112.0(2) . 5_546 ?
O7 P1 O3 110.5(2) . 5_546 ?
O5 P1 O15 107.9(2) . 5_556 ?
O7 P1 O15 105.8(2) . 5_556 ?
O3 P1 O15 105.9(2) 5_546 5_556 ?
O2 P2 O11 108.0(2) 5_546 . ?
O2 P2 O9 117.4(2) 5_546 . ?
O11 P2 O9 108.6(2) . . ?
O2 P2 O10 110.3(2) 5_546 . ?
O11 P2 O10 110.3(2) . . ?
O9 P2 O10 102.1(2) . . ?
O1 P3 O12 111.5(2) 7_446 . ?
O1 P3 O13 110.7(2) 7_446 . ?
O12 P3 O13 106.8(2) . . ?
O1 P3 O14 107.6(2) 7_446 5_556 ?
O12 P3 O14 111.4(2) . 5_556 ?
O13 P3 O14 108.8(2) . 5_556 ?
O4 P4 O8 112.6(2) 5_556 3 ?
O4 P4 O17 113.2(2) 5_556 . ?
O8 P4 O17 106.5(2) 3 . ?
O4 P4 O16 108.5(2) 5_556 . ?
O8 P4 O16 108.3(2) 3 . ?
O17 P4 O16 107.5(2) . . ?
P3 O1 Ga1 129.6(2) 7_446 . ?
P2 O2 Ga1 140.1(2) 5_546 . ?
P1 O3 Ga1 122.1(2) 5_546 . ?
P4 O4 Ga1 163.1(3) 5_556 . ?
P1 O5 Ga1 139.1(2) . . ?
Ga2 O6 Ga1 137.8(2) . . ?
P1 O7 Ga2 136.1(2) . . ?
P4 O8 Ga2 128.2(2) 3_445 . ?
P2 O9 Ga2 132.3(2) . . ?
P2 O10 Ga4 132.5(3) . 1_545 ?
P3 O12 Ga2 130.7(2) . . ?
P3 O13 Ga3 141.4(2) . . ?
P3 O14 Ga3 139.2(2) 5_556 . ?
P1 O15 Ga3 120.5(2) 5_556 . ?
P4 O16 Ga3 122.8(2) . . ?
P4 O17 Ga4 135.8(2) . . ?
N1 C1 H1A 109.5 . . ?
N1 C1 H1B 109.5 . . ?
H1A C1 H1B 109.5 . . ?
N1 C1 H1C 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
C2' C2 C3 79.3(15) . . ?
C2' C2 N1 65.8(16) . . ?
C3 C2 N1 112.4(9) . . ?
C2 C2' N1 76.1(19) . . ?
C2 C2' C3 60.4(14) . . ?
N1 C2' C3 108.1(16) . . ?
C2 C3 N2 112.3(8) . . ?
C2 C3 C2' 40.3(10) . . ?
N2 C3 C2' 124.8(11) . . ?
C4' C4 C5 46.6(18) . . ?
C4' C4 N1 77.8(19) . . ?
C5 C4 N1 109.6(7) . . ?
C5 C4' C4 84(3) . . ?
C5 C4' N1 123(3) . . ?
C4 C4' N1 61.2(17) . . ?
C4' C5 N2 118.3(19) . . ?
C4' C5 C4 49.2(19) . . ?
N2 C5 C4 111.2(7) . . ?
C1 N1 C2' 88.9(11) . . ?
C1 N1 C4 106.5(7) . . ?
C2' N1 C4 106.8(10) . . ?
C1 N1 C2 121.1(8) . . ?
C2' N1 C2 38.1(9) . . ?
C4 N1 C2 111.5(6) . . ?
C1 N1 C4' 142.3(14) . . ?
C2' N1 C4' 115.3(15) . . ?
C4 N1 C4' 41.0(12) . . ?
C2 N1 C4' 93.5(13) . . ?
C3 N2 C5 116.3(6) . . ?
C3 N2 H2A 108.2 . . ?
C5 N2 H2A 108.2 . . ?
C3 N2 H2B 108.2 . . ?
C5 N2 H2B 108.2 . . ?
H2A N2 H2B 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
N2 H2A O3 0.90 2.60 3.066(7) 112.7 .
N2 H2A O2 0.90 1.97 2.856(7) 167.8 .

_diffrn_measured_fraction_theta_max 0.999
_diffrn_reflns_theta_full        26.50
_diffrn_measured_fraction_theta_full 0.999
_refine_diff_density_max         0.757
_refine_diff_density_min         -0.644
_refine_diff_density_rms         0.153
