# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2017

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

data_GaPO-34A(pyr)
_database_code_depnum_ccdc_archive 'CCDC 1577782'
_audit_update_record             
;
2017-11-17 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;
#=============================================================================
# POWDER SPECIMEN AND CRYSTAL DATA

_chemical_formula_moiety         'F3 (OH)2 (H2O)2 Ga7 O24 P6, 2(C5 H6 N)'
_chemical_formula_sum            'C10 H18 F3 Ga7 N2 O28 P6'
_chemical_formula_weight         1345.1
_exptl_crystal_colour            colourless

_cell_length_a                   10.226818(63)
_cell_length_b                   12.095846(71)
_cell_length_c                   13.867132(81)
_cell_angle_alpha                104.65314(40)
_cell_angle_beta                 100.81105(60)
_cell_angle_gamma                102.52279(62)
_cell_volume                     1565.838(18)
_cell_formula_units_Z            2
_diffrn_ambient_temperature      293
_cell_measurement_temperature    293
_pd_spec_mounting                'glass capillary'
_pd_spec_mount_mode              transmission
_pd_spec_shape                   cylinder


#=============================================================================

#  EXPERIMENTAL DATA

_diffrn_source                   Synchrotron
_diffrn_radiation_type           'X-ray synchrotron'
_diffrn_measurement_device_type  'I11 diffractometer Diamond Light Source'

_diffrn_radiation_monochromator  'Si(111) double monochromator'


#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

#_pd_meas_number_of_points       149000
_pd_meas_2theta_range_min        1.000
_pd_meas_2theta_range_max        149.999
_pd_meas_2theta_range_inc        0.001

#=============================================================================

#  REFINEMENT DATA


# Use the next field to give any special details about the fitting of the
# powder pattern.


# The next three items are given as text.

_pd_proc_ls_profile_function     'spherical harmonics series'
_pd_proc_ls_background_function  'Chebychev polynomial and one additional peak'



#  The following profile R-factors are NOT CORRECTED for background
#  The sum is extended to all non-excluded points.
#  These are the current CIF standard

_pd_proc_ls_prof_R_factor        0.088
_pd_proc_ls_prof_wR_factor       0.116

#  Items related to LS refinement

_refine_ls_R_I_factor            0.036
_refine_ls_goodness_of_fit_all   3.03
_refine_ls_number_reflns         5951
_refine_ls_number_structural_parameters 150
_refine_ls_number_profile_parameters 46
_refine_ls_number_restraints     60

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        3.000
_pd_proc_2theta_range_max        60.000
_pd_proc_2theta_range_inc        0.002
_diffrn_radiation_wavelength     0.825781

_computing_structure_solution    TOPAS
_computing_structure_refinement  TOPAS


#=============================================================================
_symmetry_cell_setting           triclinic

_symmetry_space_group_name_H-M   P-1
loop_
_symmetry_equiv_pos_as_xyz
'-x, -y, -z'
'x, y, z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Ga1 Ga+3 2 0.93685(37) 0.51240(33) 0.12905(29) 1 1.644(26)
Ga2 Ga+3 2 0.73922(52) 0.84070(40) 0.27732(36) 1 1.644(26)
Ga3 Ga+3 2 0.74671(59) 0.50043(47) 0.50635(40) 1 1.644(26)
Ga4 Ga+3 2 1.06087(47) 0.22064(37) 0.52337(34) 1 1.644(26)
Ga5 Ga+3 2 0.24336(51) 0.84515(39) 0.27877(35) 1 1.644(26)
Ga6 Ga+3 2 0.43689(43) 0.53003(35) 0.14111(32) 1 1.644(26)
Ga7 Ga+3 2 0.44932(44) 0.78065(36) 0.47713(31) 1 1.644(26)
P1 P 2 -0.03298(46) 0.51342(39) 0.36601(35) 1 0.497(64)
P2 P 2 0.03571(47) -0.04108(42) 0.36496(34) 1 0.497(64)
P3 P 2 0.56415(50) 0.99422(40) 0.36974(36) 1 0.497(64)
P4 P 2 0.48232(47) 0.52968(41) 0.36030(36) 1 0.497(64)
P5 P 2 0.22436(50) 0.64511(40) 0.09070(35) 1 0.497(64)
P6 P 2 0.68708(54) 0.64130(38) 0.07512(31) 1 0.497(64)
O11 O 2 -0.14362(79) 0.4537(12) 0.41460(59) 1 1.280(71)
O12 O 2 0.10012(81) 0.46738(88) 0.37337(93) 1 1.280(71)
O13 O 2 -0.0972(11) 0.49121(98) 0.25001(49) 1 1.280(71)
O14 O 2 0.0111(13) 0.65470(59) 0.40699(99) 1 1.280(71)
O21 O 2 0.0627(12) -0.10464(67) 0.44613(52) 1 1.280(71)
O22 O 2 -0.09422(80) -0.0484(11) 0.28216(75) 1 1.280(71)
O23 O 2 0.15970(80) -0.04429(98) 0.31638(74) 1 1.280(71)
O24 O 2 0.1052(14) 0.08593(65) 0.43834(93) 1 1.280(71)
O31 O 2 0.6401(10) 1.12292(58) 0.43307(72) 1 1.280(71)
O32 O 2 0.61480(86) 0.93251(92) 0.27696(59) 1 1.280(71)
O33 O 2 0.40685(80) 0.9578(11) 0.3329(11) 1 1.280(71)
O34 O 2 0.5415(12) 0.89751(61) 0.42313(52) 1 1.280(71)
O41 O 2 0.37533(80) 0.4667(11) 0.40674(59) 1 1.280(71)
O42 O 2 0.61801(81) 0.49529(93) 0.38779(90) 1 1.280(71)
O43 O 2 0.4185(16) 0.4620(11) 0.24221(49) 1 1.280(71)
O44 O 2 0.5111(14) 0.66400(60) 0.3920(10) 1 1.280(71)
O51 O 2 0.1589(17) 0.6306(11) -0.02405(51) 1 1.280(71)
O52 O 2 0.12206(87) 0.54700(78) 0.11548(74) 1 1.280(71)
O53 O 2 0.2241(16) 0.77234(60) 0.14456(80) 1 1.280(71)
O54 O 2 0.38009(74) 0.64996(85) 0.11965(97) 1 1.280(71)
O61 O 2 0.7383(16) 0.77221(66) 0.14626(77) 1 1.280(71)
O62 O 2 0.61856(95) 0.56223(80) 0.13447(58) 1 1.280(71)
O63 O 2 0.6342(18) 0.61136(96) -0.04443(52) 1 1.280(71)
O64 O 2 0.80604(83) 0.59308(61) 0.1050(10) 1 1.280(71)
O1 O 2 0.7734(13) 0.7560(11) 0.36951(79) 1 1.280(71)
O2 O 2 0.6065(13) 0.7884(14) 0.58288(97) 1 1.280(71)
O3 O 2 0.9232(15) 0.2068(15) 0.39869(95) 1 1.280(71)
O4 O 2 0.2896(13) 0.7579(10) 0.36873(80) 1 1.280(71)
F1 F 2 1.0452(12) 0.69995(80) 0.21200(82) 1 1.280(71)
F2 F 2 0.6651(14) 0.32609(77) 0.46594(89) 1 1.280(71)
F3 F 2 0.1730(14) 0.34398(78) 0.49261(92) 1 1.280(71)
N11 N 2 0.1032682 0.2311832 0.2346616 1 4.00(30)
C12 C 2 0.04201716 0.2709711 0.1618115 1 4.00(30)
C13 C 2 0.0236216 0.2132561 0.06234261 1 4.00(30)
C14 C 2 0.06647713 0.1157532 0.03572378 1 4.00(30)
C15 C 2 0.1277282 0.07596522 0.1085739 1 4.00(30)
C16 C 2 0.1461238 0.1336802 0.2080428 1 4.00(30)
H12 H 2 0.009930451 0.3439734 0.1817415 1 4
H11 H 2 0.1170413 0.2743954 0.3091358 1 4
H13 H 2 -0.0222382 0.2430461 0.007798429 1 4
H14 H 2 0.05270403 0.07254091 -0.0387504 1 4
H15 H 2 0.1598149 0.002962975 0.08864385 1 4
H16 H 2 0.1919836 0.1038902 0.2625869 1 4
N21 N 2 0.5996664 0.2412326 0.08031281 1 4.00(30)
C22 C 2 0.4919559 0.15228 0.0173008 1 4.00(30)
C23 C 2 0.4024417 0.09043725 0.05631428 1 4.00(30)
C24 C 2 0.4206378 0.1175472 0.1583398 1 4.00(30)
C25 C 2 0.5283483 0.2064998 0.2213518 1 4.00(30)
C26 C 2 0.6178625 0.2683426 0.1823383 1 4.00(30)
H22 H 2 0.4783321 0.1319823 -0.05908755 1 2
H21 H 2 0.6666873 0.2875354 0.05110271 1 2
H23 H 2 0.3217969 0.02383677 0.009136035 1 2
H24 H 2 0.3536169 0.07124438 0.1875499 1 2
H25 H 2 0.5419721 0.2267975 0.2977401 1 2
H26 H 2 0.6985073 0.334943 0.2295166 1 2
####################################################################### 
# 
# 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_rw14newparts
_database_code_depnum_ccdc_archive 'CCDC 1577783'
_audit_update_record             
;
2017-10-03 deposited with the CCDC.
2017-11-17 downloaded from the CCDC.
;
_audit_creation_date             2017-08-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2017.08.10 svn.r3461 for OlexSys, GUI svn.r5381)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'F2.67 Ga7 O28 P6, 1.67(C4 H6 N2)'
_chemical_formula_sum            'C6.66 H9.99 F2.67 Ga7 N3.33 O28 P6'
_chemical_formula_weight         1309.30
_chemical_melting_point          ?
_chemical_oxdiff_formula         'O8 P2 Ga'
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'
F F 0.0171 0.0103 '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'

_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.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.0991(2)
_cell_length_b                   12.0631(6)
_cell_length_c                   13.8405(9)
_cell_angle_alpha                104.626(5)
_cell_angle_beta                 100.346(5)
_cell_angle_gamma                101.936(4)
_cell_volume                     781.41(8)
_cell_formula_units_Z            1
_cell_measurement_reflns_used    4718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.8860
_cell_measurement_theta_min      2.0790
_shelx_estimated_absorpt_T_max   0.939
_shelx_estimated_absorpt_T_min   0.741
_exptl_absorpt_coefficient_mu    6.380
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80233
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
'CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm.'
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.782
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             628
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0703
_diffrn_reflns_av_unetI/netI     0.0737
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9702
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.483
_diffrn_reflns_theta_min         3.115
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
'List of Runs (angles in degrees, time in seconds): # Type Start End Width tₑₓₚ ω θ κ φ Frames -------------------------------------------------------------------------- 1 ω -107.00 22.00 1.00 80.00 -- -17.00 -72.00-180.00 129 2 ω -53.00 73.00 1.00 80.00 -- -17.00 0.00 150.00 126 3 ω -70.00 14.00 1.00 80.00 -- -17.00 -72.00 0.00 84 4 ω -35.00 69.00 1.00 80.00 -- -17.00 72.00 90.00 104 5 ω -30.00 -15.00 1.00 80.00 -- -17.00 -72.00 -90.00 15 6 ω -60.00 38.00 1.00 80.00 -- -17.00 0.00 -30.00 98'
_diffrn_measurement_device       'four-circle κ goniometer'
_diffrn_measurement_device_type  
;
Rigaku FRE+ equipped with VHF Varimax confocal mirrors and an AFC10 goniometer and HG Saturn 724+ detector
;
_diffrn_measurement_method       'ω scans'
_diffrn_measurement_specimen_support 'MiTeGen MicroLoop'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0676449000
_diffrn_orient_matrix_UB_12      0.0332331000
_diffrn_orient_matrix_UB_13      -0.0282579000
_diffrn_orient_matrix_UB_21      0.1275446000
_diffrn_orient_matrix_UB_22      -0.0090622000
_diffrn_orient_matrix_UB_23      0.0220648000
_diffrn_orient_matrix_UB_31      -0.0256961000
_diffrn_orient_matrix_UB_32      -0.0527728000
_diffrn_orient_matrix_UB_33      -0.0412171000
_diffrn_radiation_monochromator  'Confocal mirrors, VHF Varimax'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_source                   'Rotating Anode'
_diffrn_source_type              'Rigaku FRE+'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2785
_reflns_number_total             3585
_reflns_odcompleteness_completeness 99.64
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.42
_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.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       
;
CrystalClear-SM Expert 3.1 b27 (Rigaku, 2013)
;
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.537
_refine_diff_density_min         -1.439
_refine_diff_density_rms         0.244
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         3585
_refine_ls_number_restraints     76
_refine_ls_R_factor_all          0.0854
_refine_ls_R_factor_gt           0.0607
_refine_ls_restrained_S_all      1.111
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0502P)²+11.0678P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1385
_refine_ls_wR_factor_ref         0.1472
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 O10, P2, O9, O11, O8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.008
3. Uiso/Uaniso restraints and constraints
C6 \\sim N4 \\sim C5 \\sim C3 \\sim N2 \\sim C1: within 1.7A with sigma of
0.004 and sigma for terminal atoms of 0.008
C4A \\sim C1A \\sim N2A \\sim C3A \\sim C6A \\sim N5A: within 1.7A with sigma
of 0.004 and sigma for terminal atoms of 0.008
O10 \\sim O9 \\sim P2 \\sim O8 \\sim O11: within 2A with sigma of 0.004 and
sigma for terminal atoms of 0.008
4. Rigid body (RIGU) restrains
 O11, O10, P2, O9, O8
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(F3A)=Sof(Ga3A)=Sof(C1A)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=Sof(N2A)=Sof(C3A)=
 Sof(H3A)=Sof(C4A)=Sof(H4A)=Sof(N5A)=Sof(C6A)=Sof(H6A)=1-FVAR(1)
 Sof(Ga3)=FVAR(1)
 Fixed Sof: N4(0.5) C5(0.5) H5(0.5) C6(0.5) H6(0.5) N2(0.5) C3(0.5) H3(0.5)
 C1(0.5) H1A(0.5) H1B(0.5) H1C(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C3(H3), C3A(H3A), C4A(H4A), C6A(H6A)
6.b Fitted pentagon refined as free rotating group:
 N4(C5,C6,N2,C3), N2A(C3A,C4A,N5A,C6A)
6.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C1A(H1AA,H1AB,H1AC)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
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
Ga4 Ga -0.500000 0.500000 0.500000 0.0065(3) Uani 1 2 d S T P . .
Ga1 Ga 1.37527(17) 0.77945(7) 0.47630(7) 0.0084(2) Uani 1 1 d . . . . .
Ga2 Ga 0.64093(18) 0.84296(7) 0.27831(7) 0.0119(2) Uani 1 1 d . . . . .
Ga3 Ga -0.2265(4) 0.5026(4) 0.13056(17) 0.0104(6) Uani 0.667(11) 1 d . . . A 1
P3 P -0.0638(4) 0.51963(16) 0.36057(16) 0.0075(4) Uani 1 1 d . . . . .
P1 P 1.2426(4) 0.97592(16) 0.36891(17) 0.0113(4) Uani 1 1 d . . . . .
F1 F 1.5371(9) 0.6676(4) 0.5247(4) 0.0120(9) Uani 1 1 d . . . . .
O14 O 0.1268(11) 0.4567(5) 0.4102(4) 0.0110(11) Uani 1 1 d . . . . .
O15 O -0.3520(11) 0.4897(5) 0.3797(4) 0.0118(11) Uani 1 1 d . . . . .
O4 O 1.2947(12) 1.1074(5) 0.4266(5) 0.0158(12) Uani 1 1 d . . . . .
O6 O 0.5772(11) 0.7556(4) 0.3670(4) 0.0116(11) Uani 1 1 d . . . . .
O2 O 1.2229(12) 0.8983(5) 0.4388(5) 0.0189(13) Uani 1 1 d . . . . .
O5 O 0.9705(12) 0.9383(5) 0.2857(5) 0.0197(14) Uani 1 1 d . . . . .
O13 O 0.0513(12) 0.6539(5) 0.3931(5) 0.0219(15) Uani 1 1 d . . . . .
O1 O 1.1665(14) 0.7898(7) 0.5915(5) 0.0276(16) Uani 1 1 d . . . . .
O12 O -0.1012(12) 0.4699(6) 0.2429(5) 0.0204(14) Uani 1 1 d . . . . .
O3 O 1.4709(14) 0.9631(5) 0.3126(6) 0.0294(18) Uani 1 1 d . . . . .
O10 O 0.4306(14) 0.5475(6) 0.1263(5) 0.0279(11) Uani 1 1 d . U . . .
O8 O 0.4837(16) 0.7650(6) 0.1437(5) 0.0366(14) Uani 1 1 d . U . . .
O11 O 0.0135(15) 0.6245(6) 0.1033(6) 0.0339(12) Uani 1 1 d . U . . .
O9 O 0.2958(17) 0.6197(7) -0.0262(6) 0.0435(15) Uani 1 1 d . U . . .
F3A F 0.864(3) 0.7172(12) 0.2338(11) 0.014(3) Uiso 0.333(11) 1 d . . . . .
P2 P 0.3071(6) 0.6386(2) 0.0873(2) 0.0325(6) Uani 1 1 d . U . . .
N4 N 0.761(4) 0.6998(15) 0.7791(13) 0.052(4) Uiso 0.5 1 d . U . B 1
C5 C 0.636(4) 0.7928(18) 0.7704(13) 0.056(4) Uiso 0.5 1 d G U . B 1
H5 H 0.536256 0.799483 0.709878 0.067 Uiso 0.5 1 calc R . . B 1
C6 C 0.689(4) 0.8737(15) 0.8705(16) 0.066(4) Uiso 0.5 1 d G U . B 1
H6 H 0.630810 0.942724 0.886945 0.079 Uiso 0.5 1 calc R . . B 1
N2 N 0.847(4) 0.8308(17) 0.9409(12) 0.063(4) Uiso 0.5 1 d G U . B 1
C3 C 0.892(4) 0.7233(16) 0.8845(15) 0.058(4) Uiso 0.5 1 d G U . B 1
H3 H 0.989475 0.676485 0.911691 0.069 Uiso 0.5 1 calc R . . B 1
C1 C 0.977(7) 0.877(3) 1.047(3) 0.071(6) Uiso 0.5 1 d . U . B 1
H1A H 1.023731 0.962185 1.067036 0.106 Uiso 0.5 1 calc GR . . B 1
H1B H 1.141526 0.851109 1.061014 0.106 Uiso 0.5 1 calc GR . . B 1
H1C H 0.852553 0.849013 1.085654 0.106 Uiso 0.5 1 calc GR . . B 1
Ga3A Ga -0.2261(7) 0.5549(8) 0.1457(3) 0.0087(11) Uani 0.333(11) 1 d . . . A 2
C1A C 0.726(9) 0.716(4) 0.801(3) 0.045(8) Uiso 0.333(11) 1 d . U . A -2
H1AA H 0.592986 0.640293 0.776976 0.067 Uiso 0.333(11) 1 calc GR . . A -2
H1AB H 0.893507 0.710642 0.841839 0.067 Uiso 0.333(11) 1 calc GR . . A -2
H1AC H 0.764335 0.741571 0.743610 0.067 Uiso 0.333(11) 1 calc GR . . A -2
N2A N 0.609(8) 0.808(3) 0.868(3) 0.078(7) Uiso 0.333(11) 1 d . U . A -2
C3A C 0.469(7) 0.892(3) 0.847(2) 0.081(7) Uiso 0.333(11) 1 d G U . A -2
H3A H 0.367539 0.889585 0.783498 0.098 Uiso 0.333(11) 1 calc R . . A -2
C4A C 0.511(8) 0.982(3) 0.942(3) 0.084(7) Uiso 0.333(11) 1 d G U . A -2
H4A H 0.441954 1.048842 0.950466 0.100 Uiso 0.333(11) 1 calc R . . A -2
N5A N 0.677(8) 0.953(3) 1.020(2) 0.083(7) Uiso 0.333(11) 1 d G U . A -2
C6A C 0.738(7) 0.845(3) 0.975(3) 0.081(7) Uiso 0.333(11) 1 d G U . A -2
H6A H 0.843721 0.805750 1.008874 0.097 Uiso 0.333(11) 1 calc R . . A -2


_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
Ga4 F1 1.926(4) 2_666 ?
Ga4 F1 1.926(4) 1_355 ?
Ga4 O14 1.962(5) 2_566 ?
Ga4 O14 1.962(5) 1_455 ?
Ga4 O15 1.935(5) 2_466 ?
Ga4 O15 1.935(5) . ?
Ga1 F1 1.915(5) . ?
Ga1 O4 1.952(6) 2_876 ?
Ga1 O6 1.973(5) 1_655 ?
Ga1 O2 1.903(6) . ?
Ga1 O13 1.936(6) 1_655 ?
Ga1 O1 2.063(6) . ?
Ga2 O6 1.838(6) . ?
Ga2 O5 1.799(5) . ?
Ga2 O3 1.843(6) 1_455 ?
Ga2 O8 1.807(7) . ?
Ga2 F3A 2.115(14) . ?
Ga3 O12 1.743(7) . ?
Ga3 O10 1.930(8) 1_455 ?
Ga3 O11 1.872(7) . ?
Ga3 O9 1.707(9) 2_565 ?
P3 O14 1.523(6) . ?
P3 O15 1.526(5) . ?
P3 O13 1.522(6) . ?
P3 O12 1.549(6) . ?
P1 O4 1.528(5) . ?
P1 O2 1.508(7) . ?
P1 O5 1.536(6) . ?
P1 O3 1.525(6) . ?
O12 Ga3A 1.981(9) . ?
O10 P2 1.536(8) . ?
O10 Ga3A 1.703(8) 1_655 ?
O8 P2 1.524(7) . ?
O11 P2 1.533(8) . ?
O11 Ga3A 1.620(8) . ?
O9 P2 1.518(8) . ?
O9 Ga3A 2.239(11) 2_565 ?
F3A Ga3A 1.938(16) 1_655 ?
P2 Ga3A 2.838(6) 1_655 ?
N4 C5 1.4200 . ?
N4 C3 1.4200 . ?
C5 H5 0.9300 . ?
C5 C6 1.4200 . ?
C6 H6 0.9300 . ?
C6 N2 1.4200 . ?
N2 C3 1.4200 . ?
N2 C1 1.41(4) . ?
C3 H3 0.9300 . ?
C1 H1A 0.9600 . ?
C1 H1B 0.9600 . ?
C1 H1C 0.9600 . ?
C1A H1AA 0.9600 . ?
C1A H1AB 0.9600 . ?
C1A H1AC 0.9600 . ?
C1A N2A 1.54(5) . ?
N2A C3A 1.4200 . ?
N2A C6A 1.4200 . ?
C3A H3A 0.9300 . ?
C3A C4A 1.4200 . ?
C4A H4A 0.9300 . ?
C4A N5A 1.4200 . ?
N5A C6A 1.4200 . ?
C6A H6A 0.9300 . ?

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
F1 Ga4 F1 180.0 2_666 1_355 ?
F1 Ga4 O14 92.8(2) 2_666 2_566 ?
F1 Ga4 O14 87.2(2) 1_355 2_566 ?
F1 Ga4 O14 92.8(2) 1_355 1_455 ?
F1 Ga4 O14 87.2(2) 2_666 1_455 ?
F1 Ga4 O15 91.8(2) 2_666 2_466 ?
F1 Ga4 O15 88.2(2) 1_355 2_466 ?
F1 Ga4 O15 91.8(2) 1_355 . ?
F1 Ga4 O15 88.2(2) 2_666 . ?
O14 Ga4 O14 180.0 1_455 2_566 ?
O15 Ga4 O14 91.1(2) 2_466 1_455 ?
O15 Ga4 O14 91.1(2) . 2_566 ?
O15 Ga4 O14 88.9(2) 2_466 2_566 ?
O15 Ga4 O14 88.9(2) . 1_455 ?
O15 Ga4 O15 180.0 2_466 . ?
F1 Ga1 O4 82.2(2) . 2_876 ?
F1 Ga1 O6 87.0(2) . 1_655 ?
F1 Ga1 O13 90.9(2) . 1_655 ?
F1 Ga1 O1 88.3(2) . . ?
O4 Ga1 O6 90.8(3) 2_876 1_655 ?
O4 Ga1 O1 90.5(3) 2_876 . ?
O6 Ga1 O1 175.0(3) 1_655 . ?
O2 Ga1 F1 175.6(2) . . ?
O2 Ga1 O4 94.5(2) . 2_876 ?
O2 Ga1 O6 95.9(3) . 1_655 ?
O2 Ga1 O13 92.2(2) . 1_655 ?
O2 Ga1 O1 88.9(3) . . ?
O13 Ga1 O4 171.9(3) 1_655 2_876 ?
O13 Ga1 O6 93.0(3) 1_655 1_655 ?
O13 Ga1 O1 85.1(3) 1_655 . ?
O6 Ga2 O3 104.7(3) . 1_455 ?
O6 Ga2 F3A 80.6(4) . . ?
O5 Ga2 O6 124.7(3) . . ?
O5 Ga2 O3 95.9(3) . 1_455 ?
O5 Ga2 O8 107.1(3) . . ?
O5 Ga2 F3A 78.7(4) . . ?
O3 Ga2 F3A 174.1(4) 1_455 . ?
O8 Ga2 O6 115.1(3) . . ?
O8 Ga2 O3 105.8(4) . 1_455 ?
O8 Ga2 F3A 73.8(5) . . ?
O12 Ga3 O10 113.9(3) . 1_455 ?
O12 Ga3 O11 115.3(3) . . ?
O11 Ga3 O10 105.4(4) . 1_455 ?
O9 Ga3 O12 110.1(4) 2_565 . ?
O9 Ga3 O10 105.3(4) 2_565 1_455 ?
O9 Ga3 O11 106.1(3) 2_565 . ?
O14 P3 O15 112.3(3) . . ?
O14 P3 O12 106.2(3) . . ?
O15 P3 O12 106.2(3) . . ?
O13 P3 O14 113.6(3) . . ?
O13 P3 O15 109.3(3) . . ?
O13 P3 O12 108.8(4) . . ?
O4 P1 O5 107.9(4) . . ?
O2 P1 O4 112.6(3) . . ?
O2 P1 O5 109.4(3) . . ?
O2 P1 O3 112.1(4) . . ?
O3 P1 O4 107.9(3) . . ?
O3 P1 O5 106.6(4) . . ?
Ga1 F1 Ga4 142.7(3) . 1_755 ?
P3 O14 Ga4 137.3(3) . 1_655 ?
P3 O15 Ga4 135.5(4) . . ?
P1 O4 Ga1 130.5(4) . 2_876 ?
Ga2 O6 Ga1 129.6(3) . 1_455 ?
P1 O2 Ga1 141.1(4) . . ?
P1 O5 Ga2 129.6(4) . . ?
P3 O13 Ga1 141.5(4) . 1_455 ?
P3 O12 Ga3 139.1(5) . . ?
P3 O12 Ga3A 122.4(5) . . ?
P1 O3 Ga2 132.5(4) . 1_655 ?
P2 O10 Ga3 135.4(4) . 1_655 ?
P2 O10 Ga3A 122.3(4) . 1_655 ?
P2 O8 Ga2 132.6(4) . . ?
P2 O11 Ga3 131.9(5) . . ?
P2 O11 Ga3A 146.7(6) . . ?
Ga3 O9 Ga3A 8.79(13) 2_565 2_565 ?
P2 O9 Ga3 134.3(5) . 2_565 ?
P2 O9 Ga3A 126.2(5) . 2_565 ?
Ga3A F3A Ga2 135.8(7) 1_655 . ?
O10 P2 Ga3A 30.5(3) . 1_655 ?
O8 P2 O10 111.2(4) . . ?
O8 P2 O11 110.3(5) . . ?
O8 P2 Ga3A 88.7(4) . 1_655 ?
O11 P2 O10 108.6(4) . . ?
O11 P2 Ga3A 137.9(3) . 1_655 ?
O9 P2 O10 111.0(5) . . ?
O9 P2 O8 106.4(4) . . ?
O9 P2 O11 109.3(5) . . ?
O9 P2 Ga3A 100.0(4) . 1_655 ?
C3 N4 C5 108.0 . . ?
N4 C5 H5 126.0 . . ?
C6 C5 N4 108.0 . . ?
C6 C5 H5 126.0 . . ?
C5 C6 H6 126.0 . . ?
C5 C6 N2 108.0 . . ?
N2 C6 H6 126.0 . . ?
C6 N2 C3 108.0 . . ?
C1 N2 C6 134(2) . . ?
C1 N2 C3 118(2) . . ?
N4 C3 N2 108.0 . . ?
N4 C3 H3 126.0 . . ?
N2 C3 H3 126.0 . . ?
N2 C1 H1A 109.5 . . ?
N2 C1 H1B 109.5 . . ?
N2 C1 H1C 109.5 . . ?
H1A C1 H1B 109.5 . . ?
H1A C1 H1C 109.5 . . ?
H1B C1 H1C 109.5 . . ?
O12 Ga3A O9 83.9(4) . 2_565 ?
O12 Ga3A P2 137.7(2) . 1_455 ?
O10 Ga3A O12 113.2(4) 1_455 . ?
O10 Ga3A O9 93.5(4) 1_455 2_565 ?
O10 Ga3A F3A 90.4(6) 1_455 1_455 ?
O10 Ga3A P2 27.2(3) 1_455 1_455 ?
O11 Ga3A O12 115.7(4) . . ?
O11 Ga3A O10 131.0(5) . 1_455 ?
O11 Ga3A O9 94.4(4) . 2_565 ?
O11 Ga3A F3A 76.5(6) . 1_455 ?
O11 Ga3A P2 104.9(4) . 1_455 ?
O9 Ga3A P2 105.3(3) 2_565 1_455 ?
F3A Ga3A O12 102.5(5) 1_455 . ?
F3A Ga3A O9 170.4(5) 1_455 2_565 ?
F3A Ga3A P2 74.8(5) 1_455 1_455 ?
H1AA C1A H1AB 109.5 . . ?
H1AA C1A H1AC 109.5 . . ?
H1AB C1A H1AC 109.5 . . ?
N2A C1A H1AA 109.5 . . ?
N2A C1A H1AB 109.5 . . ?
N2A C1A H1AC 109.5 . . ?
C3A N2A C1A 134(3) . . ?
C3A N2A C6A 108.0 . . ?
C6A N2A C1A 115(3) . . ?
N2A C3A H3A 126.0 . . ?
N2A C3A C4A 108.0 . . ?
C4A C3A H3A 126.0 . . ?
C3A C4A H4A 126.0 . . ?
C3A C4A N5A 108.0 . . ?
N5A C4A H4A 126.0 . . ?
C6A N5A C4A 108.0 . . ?
N2A C6A N5A 108.0 . . ?
N2A C6A H6A 126.0 . . ?
N5A C6A H6A 126.0 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ga2 O8 P2 O10 -46.2(9) . . . . ?
Ga2 O8 P2 O11 74.3(8) . . . . ?
Ga2 O8 P2 O9 -167.2(7) . . . . ?
Ga2 O8 P2 Ga3A -67.2(7) . . . 1_655 ?
Ga3 O10 P2 O8 -61.1(7) 1_655 . . . ?
Ga3 O10 P2 O11 177.5(5) 1_655 . . . ?
Ga3 O10 P2 O9 57.3(7) 1_655 . . . ?
Ga3 O11 P2 O10 -15.6(7) . . . . ?
Ga3 O11 P2 O8 -137.7(6) . . . . ?
Ga3 O11 P2 O9 105.6(6) . . . . ?
Ga3 O9 P2 O10 37.6(9) 2_565 . . . ?
Ga3 O9 P2 O8 158.8(7) 2_565 . . . ?
Ga3 O9 P2 O11 -82.1(9) 2_565 . . . ?
O14 P3 O15 Ga4 56.0(6) . . . . ?
O14 P3 O13 Ga1 2.6(9) . . . 1_455 ?
O14 P3 O12 Ga3 -166.6(5) . . . . ?
O14 P3 O12 Ga3A -159.9(4) . . . . ?
O15 P3 O14 Ga4 -129.8(5) . . . 1_655 ?
O15 P3 O13 Ga1 129.0(7) . . . 1_455 ?
O15 P3 O12 Ga3 73.6(6) . . . . ?
O15 P3 O12 Ga3A 80.3(4) . . . . ?
O4 P1 O2 Ga1 -127.0(6) . . . . ?
O4 P1 O5 Ga2 -109.8(5) . . . . ?
O4 P1 O3 Ga2 148.5(6) . . . 1_655 ?
O6 Ga2 O5 P1 -7.4(7) . . . . ?
O6 Ga2 O8 P2 -0.6(9) . . . . ?
O2 P1 O4 Ga1 71.3(6) . . . 2_876 ?
O2 P1 O5 Ga2 13.1(6) . . . . ?
O2 P1 O3 Ga2 23.9(8) . . . 1_655 ?
O5 Ga2 O6 Ga1 108.0(4) . . . 1_455 ?
O5 Ga2 O8 P2 142.9(7) . . . . ?
O5 P1 O4 Ga1 -167.8(4) . . . 2_876 ?
O5 P1 O2 Ga1 113.0(6) . . . . ?
O5 P1 O3 Ga2 -95.8(7) . . . 1_655 ?
O13 P3 O14 Ga4 -5.1(7) . . . 1_655 ?
O13 P3 O15 Ga4 -71.1(6) . . . . ?
O13 P3 O12 Ga3 -44.0(7) . . . . ?
O13 P3 O12 Ga3A -37.2(5) . . . . ?
O12 Ga3 O11 P2 59.0(8) . . . . ?
O12 P3 O14 Ga4 114.5(5) . . . 1_655 ?
O12 P3 O15 Ga4 171.7(5) . . . . ?
O12 P3 O13 Ga1 -115.4(7) . . . 1_455 ?
O3 Ga2 O6 Ga1 -0.1(5) 1_455 . . 1_455 ?
O3 Ga2 O5 P1 105.0(6) 1_455 . . . ?
O3 Ga2 O8 P2 -115.6(7) 1_455 . . . ?
O3 P1 O4 Ga1 -53.0(6) . . . 2_876 ?
O3 P1 O2 Ga1 -5.0(7) . . . . ?
O3 P1 O5 Ga2 134.5(5) . . . . ?
O10 Ga3 O12 P3 -43.2(7) 1_455 . . . ?
O10 Ga3 O11 P2 -174.5(6) 1_455 . . . ?
O8 Ga2 O6 Ga1 -115.8(5) . . . 1_455 ?
O8 Ga2 O5 P1 -146.4(5) . . . . ?
O11 Ga3 O12 P3 78.8(7) . . . . ?
O9 Ga3 O12 P3 -161.2(6) 2_565 . . . ?
O9 Ga3 O11 P2 -63.1(7) 2_565 . . . ?
F3A Ga2 O6 Ga1 177.1(5) . . . 1_455 ?
F3A Ga2 O5 P1 -77.4(6) . . . . ?
F3A Ga2 O8 P2 70.5(8) . . . . ?
P2 O11 Ga3A O12 18.5(13) . . . . ?
P2 O11 Ga3A O10 -165.3(8) . . . 1_455 ?
P2 O11 Ga3A O9 -66.8(10) . . . 2_565 ?
P2 O11 Ga3A F3A 116.1(11) . . . 1_455 ?
P2 O11 Ga3A P2 -173.9(9) . . . 1_455 ?
N4 C5 C6 N2 0.0 . . . . ?
C5 N4 C3 N2 0.0 . . . . ?
C5 C6 N2 C3 0.0 . . . . ?
C5 C6 N2 C1 174(3) . . . . ?
C6 N2 C3 N4 0.0 . . . . ?
C3 N4 C5 C6 0.0 . . . . ?
C1 N2 C3 N4 -175(2) . . . . ?
Ga3A O10 P2 O8 -45.0(7) 1_655 . . . ?
Ga3A O10 P2 O11 -166.5(5) 1_655 . . . ?
Ga3A O10 P2 O9 73.3(6) 1_655 . . . ?
Ga3A O11 P2 O10 1.3(11) . . . . ?
Ga3A O11 P2 O8 -120.8(10) . . . . ?
Ga3A O11 P2 O9 122.6(10) . . . . ?
Ga3A O11 P2 Ga3A -8.9(13) . . . 1_655 ?
Ga3A O9 P2 O10 33.0(7) 2_565 . . . ?
Ga3A O9 P2 O8 154.2(6) 2_565 . . . ?
Ga3A O9 P2 O11 -86.7(7) 2_565 . . . ?
Ga3A O9 P2 Ga3A 62.6(6) 2_565 . . 1_655 ?
C1A N2A C3A C4A -156(4) . . . . ?
C1A N2A C6A N5A 161(3) . . . . ?
N2A C3A C4A N5A 0.0 . . . . ?
C3A N2A C6A N5A 0.0 . . . . ?
C3A C4A N5A C6A 0.0 . . . . ?
C4A N5A C6A N2A 0.0 . . . . ?
C6A N2A C3A C4A 0.0 . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
'Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling - Detector area scaling'
_oxdiff_exptl_absorpt_empirical_full_max 2.824
_oxdiff_exptl_absorpt_empirical_full_min 0.186
