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

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

data_shelx
_database_code_depnum_ccdc_archive 'CCDC 1054825'
_audit_update_record             
;
2015-03-18 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C12 H28 As2 F7 Ga4 N4 O14'
_chemical_formula_weight         1014.10

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           18
_space_group_name_H-M_alt        'P 21 21 2'
_space_group_name_Hall           'P 2 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   10.3300(3)
_cell_length_b                   10.3823(4)
_cell_length_c                   12.3413(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1323.59(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    1977
_cell_measurement_theta_min      5.5640
_cell_measurement_theta_max      70.8810

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.545
_exptl_crystal_F_000             986
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_exptl_absorpt_coefficient_mu    8.593
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.36590
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;


_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_reflns_number            4024
_diffrn_reflns_av_unetI/netI     0.0633
_diffrn_reflns_av_R_equivalents  0.0425
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_theta_min         5.568
_diffrn_reflns_theta_max         71.868
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measured_fraction_theta_full 0.967
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_Laue_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_point_group_measured_fraction_full 0.976
_reflns_number_total             2262
_reflns_number_gt                2130
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.738
_reflns_Friedel_fraction_max     0.973
_reflns_Friedel_fraction_full    0.988

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          Twin
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0964P)²+2.2170P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.72(10)
_chemical_absolute_configuration ?
_refine_ls_number_reflns         2262
_refine_ls_number_parameters     200
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0552
_refine_ls_R_factor_gt           0.0525
_refine_ls_wR_factor_ref         0.1379
_refine_ls_wR_factor_gt          0.1351
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_restrained_S_all      1.034
_refine_ls_shift/su_max          0.032
_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1195(13) 0.8515(19) 0.7809(14) 0.039(4) Uani 1 1 d . . . . .
H1A H 0.0968 0.9384 0.7590 0.047 Uiso 1 1 calc R U . . .
H1B H 0.0507 0.7939 0.7583 0.047 Uiso 1 1 calc R U . . .
C2 C 0.1360(16) 0.845(3) 0.9008(15) 0.068(8) Uani 1 1 d . . . . .
H2A H 0.1313 0.9316 0.9310 0.081 Uiso 1 1 calc R U . . .
H2B H 0.0668 0.7946 0.9323 0.081 Uiso 1 1 calc R U . . .
C3 C 0.3477(13) 0.8997(13) 0.7703(13) 0.027(3) Uani 1 1 d . . . . .
H3A H 0.4283 0.8842 0.7322 0.033 Uiso 1 1 calc R U . . .
H3B H 0.3227 0.9887 0.7587 0.033 Uiso 1 1 calc R U . . .
C4 C 0.3651(18) 0.8751(18) 0.8874(15) 0.043(4) Uani 1 1 d . . . . .
H4A H 0.3617 0.9559 0.9268 0.052 Uiso 1 1 calc R U . . .
H4B H 0.4492 0.8363 0.8999 0.052 Uiso 1 1 calc R U . . .
C5 C 0.279(3) 0.6607(17) 0.8733(17) 0.059(6) Uani 1 1 d . . . . .
H5A H 0.3611 0.6234 0.8954 0.071 Uiso 1 1 calc R U . . .
H5B H 0.2105 0.6027 0.8954 0.071 Uiso 1 1 calc R U . . .
C6 C 0.277(2) 0.6753(16) 0.7560(15) 0.047(5) Uani 1 1 d . . . . .
H6A H 0.2127 0.6184 0.7249 0.056 Uiso 1 1 calc R U . . .
H6B H 0.3609 0.6527 0.7261 0.056 Uiso 1 1 calc R U . . .
N1 N 0.2455(12) 0.8122(14) 0.7289(9) 0.031(3) Uani 1 1 d . . . . .
N2 N 0.2616(12) 0.7873(14) 0.9276(10) 0.035(3) Uani 1 1 d . . . . .
H2 H 0.2693 0.7770 1.0063 0.041 Uiso 1 1 calc R U . . .
O1 O 0.2347(8) 0.7436(8) 0.5024(7) 0.0159(17) Uani 1 1 d . . . . .
O2 O 0.1956(7) 0.9961(8) 0.5407(6) 0.0154(16) Uani 1 1 d . . . . .
O3 O -0.0123(8) 0.8047(9) 0.5371(7) 0.0192(18) Uani 1 1 d . . . . .
OH4 O 0.1093(10) 0.9016(9) 0.1516(7) 0.025(2) Uani 1 1 d . . . . .
O5 O 0.3204(7) 0.6633(8) 0.2975(7) 0.0170(17) Uani 1 1 d . . . . .
O6 O 0.3578(7) 0.8385(9) 0.1335(6) 0.0157(17) Uani 1 1 d . . . . .
F1 F 0.2493(6) 0.9137(6) 0.3333(5) 0.0146(13) Uani 1 1 d . . . . .
F2 F 0.0735(6) 0.7531(7) 0.3258(6) 0.0163(14) Uani 1 1 d . . . . .
F3 F 0.0000 1.0000 0.3791(8) 0.0164(19) Uani 1 2 d S T P . .
F6 F 0.1703(8) 0.6601(8) 0.1183(6) 0.0275(16) Uani 1 1 d . . . . .
Ga1 Ga 0.11699(12) 0.87382(12) 0.44263(11) 0.0087(3) Uani 1 1 d . . . . .
Ga2 Ga 0.21583(12) 0.78505(14) 0.21793(11) 0.0123(3) Uani 1 1 d . . . . .
As1 As 0.33644(10) 0.65063(11) 0.43197(9) 0.0079(3) Uani 1 1 d . . . . .
OW1 O 0.5000 1.0000 0.2417(13) 0.048(5) Uani 1 2 d S T P . .
OW2 O 0.5000 1.0000 0.4602(15) 0.048(4) Uani 1 2 d S T P . .
H1 H 0.23(2) 0.82(2) 0.665(18) 0.057 Uiso 1 1 d . U . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
C1 C2 1.49(2) . ?
C1 N1 1.507(19) . ?
C2 N2 1.47(2) . ?
C3 C4 1.48(2) . ?
C3 N1 1.484(18) . ?
C4 N2 1.49(2) . ?
C5 C6 1.46(3) . ?
C5 N2 1.49(2) . ?
C6 N1 1.50(2) . ?
O1 As1 1.671(9) . ?
O1 Ga1 1.963(8) . ?
O2 As1 1.672(9) 3_556 ?
O2 Ga1 1.933(8) . ?
O3 As1 1.674(8) 4_466 ?
O3 Ga1 1.913(8) . ?
OH4 Ga2 1.830(9) . ?
O5 As1 1.673(9) . ?
O5 Ga2 1.931(8) . ?
O6 Ga2 1.883(8) . ?
F1 Ga1 1.965(7) . ?
F1 Ga2 1.983(7) . ?
F2 Ga1 1.962(7) . ?
F2 Ga2 2.012(7) . ?
F3 Ga1 1.947(4) 2_575 ?
F3 Ga1 1.947(4) . ?
F6 Ga2 1.848(8) . ?
As1 O2 1.672(9) 3_546 ?
As1 O3 1.674(8) 4_566 ?

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
C2 C1 N1 108.2(12) . . ?
N2 C2 C1 110.0(14) . . ?
C4 C3 N1 108.5(12) . . ?
C3 C4 N2 110.1(13) . . ?
C6 C5 N2 110.8(15) . . ?
C5 C6 N1 108.9(14) . . ?
C3 N1 C6 110.4(12) . . ?
C3 N1 C1 107.6(12) . . ?
C6 N1 C1 110.6(12) . . ?
C2 N2 C5 111.7(18) . . ?
C2 N2 C4 107.9(16) . . ?
C5 N2 C4 107.6(15) . . ?
As1 O1 Ga1 126.3(5) . . ?
As1 O2 Ga1 132.3(4) 3_556 . ?
As1 O3 Ga1 133.4(5) 4_466 . ?
As1 O5 Ga2 127.7(5) . . ?
Ga1 F1 Ga2 103.3(3) . . ?
Ga1 F2 Ga2 102.3(3) . . ?
Ga1 F3 Ga1 132.5(5) 2_575 . ?
O3 Ga1 O2 99.1(4) . . ?
O3 Ga1 F3 93.7(3) . . ?
O2 Ga1 F3 94.1(3) . . ?
O3 Ga1 O1 86.8(4) . . ?
O2 Ga1 O1 87.5(3) . . ?
F3 Ga1 O1 178.2(4) . . ?
O3 Ga1 F2 92.8(4) . . ?
O2 Ga1 F2 167.4(3) . . ?
F3 Ga1 F2 89.5(3) . . ?
O1 Ga1 F2 88.7(3) . . ?
O3 Ga1 F1 169.6(3) . . ?
O2 Ga1 F1 90.0(3) . . ?
F3 Ga1 F1 90.8(3) . . ?
O1 Ga1 F1 88.4(3) . . ?
F2 Ga1 F1 77.9(3) . . ?
OH4 Ga2 F6 90.8(4) . . ?
OH4 Ga2 O6 91.5(4) . . ?
F6 Ga2 O6 92.1(4) . . ?
OH4 Ga2 O5 175.7(4) . . ?
F6 Ga2 O5 91.2(4) . . ?
O6 Ga2 O5 92.2(4) . . ?
OH4 Ga2 F1 88.9(4) . . ?
F6 Ga2 F1 174.3(3) . . ?
O6 Ga2 F1 93.6(3) . . ?
O5 Ga2 F1 88.8(3) . . ?
OH4 Ga2 F2 88.0(4) . . ?
F6 Ga2 F2 98.0(3) . . ?
O6 Ga2 F2 169.9(3) . . ?
O5 Ga2 F2 88.0(3) . . ?
F1 Ga2 F2 76.3(3) . . ?
O1 As1 O2 108.9(4) . 3_546 ?
O1 As1 O3 108.0(4) . 4_566 ?
O2 As1 O3 113.9(4) 3_546 4_566 ?
O1 As1 O5 114.1(4) . . ?
O2 As1 O5 104.8(4) 3_546 . ?
O3 As1 O5 107.3(4) 4_566 . ?

_refine_diff_density_max         1.181
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.226

_shelxl_version_number           2013-4

####################################################################### 
# 
# 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_shelx
_database_code_depnum_ccdc_archive 'CCDC 1054826'
_audit_update_record             
;
2015-03-18 deposited with the CCDC.
2015-06-11 downloaded from the CCDC.
;


_audit_creation_method           SHELXL-2013
_chemical_name_systematic        
;
 ?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C8 H24 As1 F8 Ga2 N4 O5'
_chemical_formula_weight         622.67

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga -1.2846 0.7763 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
As As -0.9300 1.0051 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;

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

_cell_length_a                   12.9563(2)
_cell_length_b                   13.6686(2)
_cell_length_c                   41.1833(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     7293.34(18)
_cell_formula_units_Z            16
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    7681
_cell_measurement_theta_min      4.0310
_cell_measurement_theta_max      69.4840

_exptl_crystal_description       Block
_exptl_crystal_colour            Colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_F_000             4912
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_absorpt_coefficient_mu    6.713
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.54025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;

_exptl_special_details           
;
 ?
;

_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     1.54184
_diffrn_radiation_type           CuK\a
_diffrn_source                   'sealed X-ray tube'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'four-circle diffractometer'
_diffrn_detector_area_resol_mean 16.2300
_diffrn_reflns_number            17627
_diffrn_reflns_av_unetI/netI     0.0447
_diffrn_reflns_av_R_equivalents  0.0423
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -49
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         4.824
_diffrn_reflns_theta_max         69.853
_diffrn_reflns_theta_full        67.684
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measured_fraction_theta_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.996
_reflns_number_total             6761
_reflns_number_gt                5892
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;

_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_cell_refinement       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_structure_solution    'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0898P)²+17.5749P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         6761
_refine_ls_number_parameters     505
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0532
_refine_ls_wR_factor_ref         0.1458
_refine_ls_wR_factor_gt          0.1387
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_restrained_S_all      1.047
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.1908(5) 0.3771(5) 0.14360(17) 0.0378(16) Uani 1 1 d . . . . .
H1A H 0.1205 0.3992 0.1471 0.045 Uiso 1 1 calc R U . . .
H1B H 0.1971 0.3116 0.1525 0.045 Uiso 1 1 calc R U . . .
C2 C 0.2632(5) 0.4434(5) 0.16060(14) 0.0370(17) Uani 1 1 d . . . . .
H2A H 0.2464 0.4456 0.1835 0.044 Uiso 1 1 calc R U . . .
H2B H 0.3332 0.4191 0.1584 0.044 Uiso 1 1 calc R U . . .
C3 C 0.2071(5) 0.4743(5) 0.09395(13) 0.0286(14) Uani 1 1 d . . . . .
H3A H 0.1370 0.4987 0.0959 0.034 Uiso 1 1 calc R U . . .
H3B H 0.2245 0.4717 0.0711 0.034 Uiso 1 1 calc R U . . .
C4 C 0.2790(5) 0.5419(5) 0.11099(18) 0.0354(15) Uani 1 1 d . . . . .
H4A H 0.2717 0.6075 0.1023 0.043 Uiso 1 1 calc R U . . .
H4B H 0.3497 0.5209 0.1075 0.043 Uiso 1 1 calc R U . . .
C5 C 0.8736(5) 0.9769(4) 0.13131(14) 0.0271(12) Uani 1 1 d . . . . .
H5A H 0.9422 0.9523 0.1265 0.033 Uiso 1 1 calc R U . . .
H5B H 0.8770 1.0129 0.1516 0.033 Uiso 1 1 calc R U . . .
C6 C 0.8389(5) 1.0446(4) 0.10433(13) 0.0298(14) Uani 1 1 d . . . . .
H6A H 0.8856 1.0999 0.1029 0.036 Uiso 1 1 calc R U . . .
H6B H 0.8406 1.0101 0.0838 0.036 Uiso 1 1 calc R U . . .
C7 C 0.4008(3) 0.9124(3) 0.25673(10) 0.0074(8) Uani 1 1 d . . . . .
H7A H 0.3519 0.8726 0.2687 0.009 Uiso 1 1 calc R U . . .
H7B H 0.3625 0.9639 0.2459 0.009 Uiso 1 1 calc R U . . .
C8 C 0.6590(5) 0.9964(4) 0.11486(14) 0.0304(14) Uani 1 1 d . . . . .
H8A H 0.6544 0.9604 0.0946 0.037 Uiso 1 1 calc R U . . .
H8B H 0.5909 1.0213 0.1200 0.037 Uiso 1 1 calc R U . . .
C9 C 0.6944(5) 0.9285(4) 0.14156(14) 0.0266(13) Uani 1 1 d . . . . .
H9A H 0.6934 0.9629 0.1622 0.032 Uiso 1 1 calc R U . . .
H9B H 0.6475 0.8734 0.1431 0.032 Uiso 1 1 calc R U . . .
C10 C 0.6073(4) 0.9559(4) 0.23710(12) 0.0136(10) Uani 1 1 d . . . . .
H10A H 0.6453 0.9047 0.2482 0.016 Uiso 1 1 calc R U . . .
H10B H 0.6564 0.9954 0.2251 0.016 Uiso 1 1 calc R U . . .
C11 C 0.4524(4) 0.8517(4) 0.23227(13) 0.0194(11) Uani 1 1 d . . . . .
H11A H 0.4018 0.8267 0.2170 0.023 Uiso 1 1 calc R U . . .
H11B H 0.4854 0.7964 0.2428 0.023 Uiso 1 1 calc R U . . .
C12 C 0.5541(4) 1.0178(4) 0.26132(14) 0.0223(11) Uani 1 1 d . . . . .
H12A H 0.5195 1.0716 0.2504 0.027 Uiso 1 1 calc R U . . .
H12B H 0.6042 1.0451 0.2763 0.027 Uiso 1 1 calc R U . . .
C13 C 0.4625(4) 0.0264(4) 0.96822(13) 0.0181(10) Uani 1 1 d . . . . .
H13A H 0.4171 0.0651 0.9546 0.022 Uiso 1 1 calc R U . . .
H13B H 0.5031 -0.0159 0.9543 0.022 Uiso 1 1 calc R U . . .
C14 C 0.5331(4) 0.0929(4) 0.98692(14) 0.0200(11) Uani 1 1 d . . . . .
H14A H 0.5755 0.1301 0.9720 0.024 Uiso 1 1 calc R U . . .
H14B H 0.4925 0.1387 0.9996 0.024 Uiso 1 1 calc R U . . .
C15 C 0.4514(4) 0.5232(4) 1.03055(14) 0.0246(12) Uani 1 1 d . . . . .
H15A H 0.4772 0.4719 1.0447 0.030 Uiso 1 1 calc R U . . .
H15B H 0.4060 0.5648 1.0432 0.030 Uiso 1 1 calc R U . . .
C16 C 0.4599(5) 0.4174(4) 0.98207(14) 0.0252(12) Uani 1 1 d . . . . .
H16A H 0.4197 0.3924 0.9640 0.030 Uiso 1 1 calc R U . . .
H16B H 0.4859 0.3620 0.9943 0.030 Uiso 1 1 calc R U . . .
N1 N 0.2134(4) 0.3750(4) 0.10803(12) 0.0286(11) Uani 1 1 d . . . . .
H1C H 0.2820 0.3486 0.1045 0.034 Uiso 1 1 calc R U . . .
H1D H 0.1642 0.3325 0.0972 0.034 Uiso 1 1 calc R U . . .
N2 N 0.2559(5) 0.5427(4) 0.14661(14) 0.0379(14) Uani 1 1 d . . . . .
H2C H 0.3043 0.5856 0.1576 0.045 Uiso 1 1 calc R U . . .
H2D H 0.1869 0.5682 0.1501 0.045 Uiso 1 1 calc R U . . .
N3 N 0.4756(4) 0.9572(4) 0.27995(13) 0.0332(12) Uani 1 1 d . . . . .
H3C H 0.5107 0.9062 0.2921 0.040 Uiso 1 1 calc R U . . .
H3D H 0.4390 0.9985 0.2953 0.040 Uiso 1 1 calc R U . . .
N4 N 0.5326(4) 0.9111(4) 0.21419(13) 0.0366(13) Uani 1 1 d . . . . .
H4C H 0.5692 0.8691 0.1991 0.044 Uiso 1 1 calc R U . . .
H4D H 0.4987 0.9622 0.2018 0.044 Uiso 1 1 calc R U . . .
N5 N 0.7321(5) 1.0800(3) 0.11086(12) 0.0286(12) Uani 1 1 d . . . . .
H5C H 0.7094 1.1209 0.0930 0.034 Uiso 1 1 calc R U . . .
H5D H 0.7319 1.1195 0.1304 0.034 Uiso 1 1 calc R U . . .
N6 N 0.8003(4) 0.8927(3) 0.13488(11) 0.0229(10) Uani 1 1 d . . . . .
H6C H 0.8002 0.8542 0.1151 0.027 Uiso 1 1 calc R U . . .
H6D H 0.8229 0.8509 0.1525 0.027 Uiso 1 1 calc R U . . .
N7 N 0.3997(3) -0.0344(3) 0.99105(10) 0.0183(9) Uani 1 1 d . . . . .
H7C H 0.3556 0.0079 1.0039 0.022 Uiso 1 1 calc R U . . .
H7D H 0.3558 -0.0782 0.9787 0.022 Uiso 1 1 calc R U . . .
N8 N 0.3924(4) 0.4789(3) 1.00342(12) 0.0233(10) Uani 1 1 d . . . . .
H8C H 0.3612 0.5304 0.9905 0.028 Uiso 1 1 calc R U . . .
H8D H 0.3373 0.4387 1.0122 0.028 Uiso 1 1 calc R U . . .
O1 O 0.4130(3) -0.3174(3) 0.92963(9) 0.0210(8) Uani 1 1 d . . . . .
O2 O 0.4149(3) 0.2501(3) 1.04007(9) 0.0223(8) Uani 1 1 d . . . . .
O3 O 0.1155(3) 0.1437(3) 0.32181(10) 0.0264(9) Uani 1 1 d . . . . .
O4 O 0.5904(3) -0.3234(3) 0.89622(9) 0.0223(8) Uani 1 1 d . . . . .
O5 O 0.5031(3) -0.1451(3) 0.90951(10) 0.0265(9) Uani 1 1 d . . . . .
O6 O -0.0586(3) 0.1995(3) 0.28910(9) 0.0243(9) Uani 1 1 d . . . . .
O7 O -0.0667(3) 0.1135(3) 0.35141(9) 0.0213(8) Uani 1 1 d . . . . .
O8 O 0.0042(4) 0.3012(3) 0.34214(10) 0.0281(10) Uani 1 1 d . . . . .
OW1 O 0.5300(5) 0.1554(6) 0.3426(2) 0.089(3) Uani 1 1 d . . . . .
OW2 O 0.5030(5) 0.2105(6) 0.9054(3) 0.106(3) Uani 1 1 d . . . . .
F1 F -0.2803(3) 0.1916(2) 0.31053(7) 0.0241(7) Uani 1 1 d . . . . .
F2 F -0.2115(2) 0.3285(2) 0.27196(7) 0.0188(6) Uani 1 1 d . . . . .
F3 F -0.1947(2) 0.0559(2) 0.27478(7) 0.0199(7) Uani 1 1 d . . . . .
F4 F 0.1809(2) 0.1831(2) 0.25582(7) 0.0147(6) Uani 1 1 d . . . . .
F5 F 0.3618(2) 0.1983(2) 0.27114(7) 0.0149(6) Uani 1 1 d . . . . .
F6 F 0.2154(3) 0.3149(2) 0.30185(7) 0.0190(6) Uani 1 1 d . . . . .
F7 F 0.2631(2) 0.0447(2) 0.29523(7) 0.0179(6) Uani 1 1 d . . . . .
F8 F 0.3193(2) 0.1856(2) 0.33716(7) 0.0195(6) Uani 1 1 d . . . . .
F9 F 0.2526(2) 0.3613(2) 1.02456(7) 0.0195(6) Uani 1 1 d . . . . .
F10 F 0.1975(3) 0.2220(2) 1.06417(8) 0.0263(7) Uani 1 1 d . . . . .
F11 F 0.2888(2) 0.0900(2) 1.02766(7) 0.0207(7) Uani 1 1 d . . . . .
F12 F 0.3485(2) -0.2895(2) 0.99753(7) 0.0160(6) Uani 1 1 d . . . . .
F13 F 0.1681(2) -0.2723(2) 0.98171(7) 0.0151(6) Uani 1 1 d . . . . .
F14 F 0.3021(2) -0.1552(2) 0.94988(7) 0.0186(6) Uani 1 1 d . . . . .
F15 F 0.2063(2) -0.2898(2) 0.91606(7) 0.0197(6) Uani 1 1 d . . . . .
F16 F 0.2725(2) -0.4272(2) 0.95831(7) 0.0177(6) Uani 1 1 d . . . . .
Ga1 Ga 0.24061(5) 0.17970(4) 0.29914(2) 0.01236(16) Uani 1 1 d . . . . .
Ga2 Ga -0.19788(5) 0.19248(4) 0.27325(2) 0.01255(16) Uani 1 1 d . . . . .
Ga3 Ga 0.28800(5) -0.29200(4) 0.95388(2) 0.01266(16) Uani 1 1 d . . . . .
Ga4 Ga 0.27515(5) 0.22558(4) 1.02629(2) 0.01356(16) Uani 1 1 d . . . . .
As1 As -0.00403(4) 0.18664(4) 0.32528(2) 0.01383(16) Uani 1 1 d . . . . .
As2 As 0.52514(4) -0.26073(4) 0.92446(2) 0.01355(15) 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
C1 C2 1.480(10) . ?
C1 N1 1.494(9) . ?
C2 N2 1.477(9) . ?
C3 N1 1.479(8) . ?
C3 C4 1.489(9) . ?
C4 N2 1.497(9) . ?
C5 N6 1.500(8) . ?
C5 C6 1.515(8) . ?
C6 N5 1.490(9) . ?
C7 C11 1.467(7) . ?
C7 N3 1.493(7) . ?
C8 N5 1.493(8) . ?
C8 C9 1.510(8) . ?
C9 N6 1.483(8) . ?
C10 C12 1.479(7) . ?
C10 N4 1.484(8) . ?
C11 N4 1.514(7) . ?
C12 N3 1.520(7) . ?
C13 N7 1.496(7) . ?
C13 C14 1.502(7) . ?
C14 N7 1.490(7) 5_657 ?
C15 N8 1.483(7) . ?
C15 C16 1.501(8) 5_667 ?
C16 N8 1.498(7) . ?
C16 C15 1.501(8) 5_667 ?
N7 C14 1.490(7) 5_657 ?
O1 As2 1.661(4) . ?
O1 Ga3 1.934(4) . ?
O2 As2 1.661(4) 5_657 ?
O2 Ga4 1.927(4) . ?
O3 As1 1.663(4) . ?
O3 Ga1 1.934(4) . ?
O4 As2 1.674(4) . ?
O5 As2 1.720(4) . ?
O6 As1 1.659(4) . ?
O6 Ga2 1.921(4) . ?
O7 As1 1.679(4) . ?
O8 As1 1.716(4) . ?
F1 Ga2 1.870(3) . ?
F2 Ga2 1.869(3) . ?
F3 Ga2 1.869(3) . ?
F4 Ga1 1.945(3) . ?
F4 Ga2 1.980(3) 6_656 ?
F5 Ga1 1.964(3) . ?
F5 Ga2 1.987(3) 6_656 ?
F6 Ga1 1.880(3) . ?
F7 Ga1 1.875(3) . ?
F8 Ga1 1.870(3) . ?
F9 Ga4 1.879(3) . ?
F10 Ga4 1.857(3) . ?
F11 Ga4 1.862(3) . ?
F12 Ga3 1.961(3) . ?
F12 Ga4 2.003(3) 8_655 ?
F13 Ga3 1.950(3) . ?
F13 Ga4 1.978(3) 8_655 ?
F14 Ga3 1.886(3) . ?
F15 Ga3 1.883(3) . ?
F16 Ga3 1.868(3) . ?
Ga2 F4 1.980(3) 6_556 ?
Ga2 F5 1.987(3) 6_556 ?
Ga4 F13 1.978(3) 8_665 ?
Ga4 F12 2.003(3) 8_665 ?
As2 O2 1.661(4) 5_657 ?

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
C2 C1 N1 110.6(5) . . ?
N2 C2 C1 109.7(5) . . ?
N1 C3 C4 110.5(5) . . ?
C3 C4 N2 109.9(5) . . ?
N6 C5 C6 110.7(5) . . ?
N5 C6 C5 110.0(5) . . ?
C11 C7 N3 112.1(4) . . ?
N5 C8 C9 111.0(5) . . ?
N6 C9 C8 110.4(5) . . ?
C12 C10 N4 111.2(4) . . ?
C7 C11 N4 110.3(4) . . ?
C10 C12 N3 109.9(5) . . ?
N7 C13 C14 110.2(4) . . ?
N7 C14 C13 110.1(4) 5_657 . ?
N8 C15 C16 110.8(5) . 5_667 ?
N8 C16 C15 110.3(5) . 5_667 ?
C3 N1 C1 110.9(5) . . ?
C2 N2 C4 111.3(5) . . ?
C7 N3 C12 109.5(4) . . ?
C10 N4 C11 110.9(4) . . ?
C6 N5 C8 111.1(5) . . ?
C9 N6 C5 110.5(4) . . ?
C14 N7 C13 111.2(4) 5_657 . ?
C15 N8 C16 111.8(4) . . ?
As2 O1 Ga3 135.7(2) . . ?
As2 O2 Ga4 135.5(2) 5_657 . ?
As1 O3 Ga1 137.1(2) . . ?
As1 O6 Ga2 134.5(2) . . ?
Ga1 F4 Ga2 103.91(13) . 6_656 ?
Ga1 F5 Ga2 102.97(13) . 6_656 ?
Ga3 F12 Ga4 102.97(14) . 8_655 ?
Ga3 F13 Ga4 104.30(13) . 8_655 ?
F8 Ga1 F7 91.68(13) . . ?
F8 Ga1 F6 90.15(13) . . ?
F7 Ga1 F6 178.17(13) . . ?
F8 Ga1 O3 93.63(16) . . ?
F7 Ga1 O3 85.49(16) . . ?
F6 Ga1 O3 94.37(16) . . ?
F8 Ga1 F4 169.66(13) . . ?
F7 Ga1 F4 90.39(12) . . ?
F6 Ga1 F4 87.82(12) . . ?
O3 Ga1 F4 96.63(15) . . ?
F8 Ga1 F5 92.88(13) . . ?
F7 Ga1 F5 87.27(13) . . ?
F6 Ga1 F5 92.66(13) . . ?
O3 Ga1 F5 170.40(16) . . ?
F4 Ga1 F5 77.09(12) . . ?
F3 Ga2 F2 175.84(14) . . ?
F3 Ga2 F1 88.80(13) . . ?
F2 Ga2 F1 88.60(14) . . ?
F3 Ga2 O6 91.01(16) . . ?
F2 Ga2 O6 92.79(16) . . ?
F1 Ga2 O6 104.93(16) . . ?
F3 Ga2 F4 88.48(13) . 6_556 ?
F2 Ga2 F4 88.40(13) . 6_556 ?
F1 Ga2 F4 92.47(14) . 6_556 ?
O6 Ga2 F4 162.59(14) . 6_556 ?
F3 Ga2 F5 93.56(12) . 6_556 ?
F2 Ga2 F5 88.33(13) . 6_556 ?
F1 Ga2 F5 167.94(14) . 6_556 ?
O6 Ga2 F5 86.87(15) . 6_556 ?
F4 Ga2 F5 75.79(12) 6_556 6_556 ?
F16 Ga3 F15 92.07(13) . . ?
F16 Ga3 F14 179.13(14) . . ?
F15 Ga3 F14 88.06(13) . . ?
F16 Ga3 O1 87.86(15) . . ?
F15 Ga3 O1 92.63(15) . . ?
F14 Ga3 O1 92.99(15) . . ?
F16 Ga3 F13 89.64(13) . . ?
F15 Ga3 F13 92.07(13) . . ?
F14 Ga3 F13 89.49(13) . . ?
O1 Ga3 F13 174.75(15) . . ?
F16 Ga3 F12 88.33(13) . . ?
F15 Ga3 F12 169.20(13) . . ?
F14 Ga3 F12 91.39(12) . . ?
O1 Ga3 F12 98.17(15) . . ?
F13 Ga3 F12 77.13(12) . . ?
F10 Ga4 F11 89.98(14) . . ?
F10 Ga4 F9 88.49(14) . . ?
F11 Ga4 F9 176.46(15) . . ?
F10 Ga4 O2 105.45(16) . . ?
F11 Ga4 O2 94.29(16) . . ?
F9 Ga4 O2 89.19(16) . . ?
F10 Ga4 F13 169.00(15) . 8_665 ?
F11 Ga4 F13 90.43(13) . 8_665 ?
F9 Ga4 F13 90.46(13) . 8_665 ?
O2 Ga4 F13 85.48(14) . 8_665 ?
F10 Ga4 F12 93.48(15) . 8_665 ?
F11 Ga4 F12 89.51(13) . 8_665 ?
F9 Ga4 F12 87.40(13) . 8_665 ?
O2 Ga4 F12 160.67(14) . 8_665 ?
F13 Ga4 F12 75.53(12) 8_665 8_665 ?
O6 As1 O3 111.0(2) . . ?
O6 As1 O7 115.64(19) . . ?
O3 As1 O7 107.19(19) . . ?
O6 As1 O8 107.0(2) . . ?
O3 As1 O8 107.4(2) . . ?
O7 As1 O8 108.30(18) . . ?
O2 As2 O1 109.69(19) 5_657 . ?
O2 As2 O4 114.84(19) 5_657 . ?
O1 As2 O4 106.98(19) . . ?
O2 As2 O5 108.2(2) 5_657 . ?
O1 As2 O5 109.2(2) . . ?
O4 As2 O5 107.81(19) . . ?

_refine_diff_density_max         1.364
_refine_diff_density_min         -1.069
_refine_diff_density_rms         0.182

_shelxl_version_number           2013-4

