# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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_h1-105-4
_database_code_depnum_ccdc_archive 'CCDC 1989710'
loop_
_audit_author_name
_audit_author_address
'Zhien Lin'
;Sichuan University
China
;
_audit_update_record             
;
2020-03-11 deposited with the CCDC.	2020-04-14 downloaded from the CCDC.
;
_audit_creation_date             2019-12-25
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C6 H12 N O6 P Zn'
_chemical_formula_sum            'C6 H12 N O6 P Zn'
_chemical_formula_weight         290.51
_chemical_melting_point          ?
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'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 '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      orthorhombic
_space_group_IT_number           73
_space_group_name_H-M_alt        'I b c a'
_space_group_name_Hall           '-I 2b 2c'
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+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-x+1/2, y+1, -z+1'
'x+1, -y+1, -z+1/2'
'-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+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'x+1/2, -y, z'
'-x, y, z+1/2'

_cell_length_a                   8.72446(14)
_cell_length_b                   22.3339(4)
_cell_length_c                   20.8612(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     4064.84(10)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    3453
_cell_measurement_temperature    294(3)
_cell_measurement_theta_max      72.7210
_cell_measurement_theta_min      4.2440
_shelx_estimated_absorpt_T_max   0.380
_shelx_estimated_absorpt_T_min   0.252
_exptl_absorpt_coefficient_mu    5.005
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.47338
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.899
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       prism
_exptl_crystal_F_000             2368
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.24
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            5625
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.005
_diffrn_reflns_theta_max         67.005
_diffrn_reflns_theta_min         3.959
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      294(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  31.00   1.00    4.41    --  -36.54  57.00   0.00   84
  2  ω    -63.00  31.00   1.00    4.41    --  -36.54  77.00 -90.00   94
  3  ω   -105.00 -52.00   1.00    4.41    --  -36.54-156.00 -74.00   53
  4  ω     23.00  90.00   1.00    4.41    --   36.54-125.00-180.00   67
  5  ω     41.00 125.00   1.00   17.63    --  108.71 -53.00 -47.00   84
  6  ω     91.00 176.00   1.00   17.63    --  108.71  61.00 120.00   85
  7  ω     39.00  95.00   1.00   17.63    --  108.71 -94.00-120.00   56
  8  ω     49.00 102.00   1.00   17.63    --  108.71 -94.00 120.00   53
  9  ω     59.00  99.00   1.00   17.63    --  108.71 -61.00-150.00   40
 10  ω     46.00 100.00   1.00   17.63    --  108.71-111.00  90.00   54
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1026805000
_diffrn_orient_matrix_UB_12      0.0374709000
_diffrn_orient_matrix_UB_13      -0.0447191000
_diffrn_orient_matrix_UB_21      0.0470483000
_diffrn_orient_matrix_UB_22      -0.0572925000
_diffrn_orient_matrix_UB_23      -0.0361613000
_diffrn_orient_matrix_UB_31      -0.1357103000
_diffrn_orient_matrix_UB_32      0.0085238000
_diffrn_orient_matrix_UB_33      -0.0463280000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1673
_reflns_number_total             1819
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (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         0.844
_refine_diff_density_min         -0.697
_refine_diff_density_rms         0.146
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.077
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1819
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0542
_refine_ls_R_factor_gt           0.0517
_refine_ls_restrained_S_all      1.077
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1034P)²+5.1484P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1391
_refine_ls_wR_factor_ref         0.1422
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C2(H2)
2.b Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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
Zn1 Zn 0.5000 0.7500 0.55369(3) 0.0214(3) Uani 1 2 d S T P . .
Zn2 Zn 0.5000 0.7500 0.76149(3) 0.0236(3) Uani 1 2 d S T P . .
P1 P 0.27789(9) 0.69513(3) 0.65501(3) 0.0197(3) Uani 1 1 d . . . . .
O1 O 0.3175(3) 0.74326(10) 0.60585(12) 0.0278(5) Uani 1 1 d . . . . .
O2 O 0.3867(3) 0.69446(11) 0.71050(12) 0.0366(6) Uani 1 1 d . . . . .
O3 O 0.1124(3) 0.70057(11) 0.67676(12) 0.0334(6) Uani 1 1 d . . . . .
O4 O 0.2845(3) 0.63206(11) 0.62225(13) 0.0400(7) Uani 1 1 d . . . . .
H4 H 0.3499 0.6323 0.5940 0.060 Uiso 1 1 calc GR . . . .
O5 O 0.5444(5) 0.68741(14) 0.49159(15) 0.0568(9) Uani 1 1 d . . . . .
O6 O 0.4828(5) 0.60092(16) 0.53400(19) 0.0818(15) Uani 1 1 d . . . . .
N1 N 0.6451(3) 0.64691(11) 0.38408(12) 0.0262(6) Uani 1 1 d . . . . .
H1A H 0.6949 0.6775 0.4017 0.031 Uiso 1 1 calc R . . . .
H1B H 0.5577 0.6609 0.3679 0.031 Uiso 1 1 calc R . . . .
C1 C 0.5347(4) 0.63225(16) 0.49179(16) 0.0306(7) Uani 1 1 d . . . . .
C2 C 0.6099(4) 0.60213(15) 0.43425(15) 0.0312(7) Uani 1 1 d . . . . .
H2 H 0.7086 0.5866 0.4493 0.037 Uiso 1 1 calc R . . . .
C3 C 0.5241(5) 0.54942(19) 0.40635(18) 0.0383(9) Uani 1 1 d . . . . .
H3A H 0.4244 0.5625 0.3913 0.046 Uiso 1 1 calc R . . . .
H3B H 0.5084 0.5195 0.4394 0.046 Uiso 1 1 calc R . . . .
C4 C 0.6138(6) 0.52179(17) 0.35051(19) 0.0481(11) Uani 1 1 d . . . . .
H4A H 0.7062 0.5030 0.3668 0.058 Uiso 1 1 calc R . . . .
H4B H 0.5519 0.4911 0.3301 0.058 Uiso 1 1 calc R . . . .
C5 C 0.6572(6) 0.56943(19) 0.30103(18) 0.0506(11) Uani 1 1 d . . . . .
H5A H 0.7222 0.5515 0.2685 0.061 Uiso 1 1 calc R . . . .
H5B H 0.5650 0.5839 0.2801 0.061 Uiso 1 1 calc R . . . .
C6 C 0.7399(5) 0.62142(17) 0.33121(17) 0.0360(8) Uani 1 1 d . . . . .
H6A H 0.8378 0.6081 0.3481 0.043 Uiso 1 1 calc R . . . .
H6B H 0.7592 0.6520 0.2992 0.043 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
Zn1 O1 1.934(3) 6_564 ?
Zn1 O1 1.934(3) . ?
Zn1 O5 1.945(3) . ?
Zn1 O5 1.945(3) 6_564 ?
Zn2 O2 1.910(2) 6_564 ?
Zn2 O2 1.910(2) . ?
Zn2 O3 1.960(2) 13_566 ?
Zn2 O3 1.960(2) 10_657 ?
P1 O1 1.525(3) . ?
P1 O2 1.497(3) . ?
P1 O3 1.518(2) . ?
P1 O4 1.567(2) . ?
O3 Zn2 1.959(2) 13_566 ?
O4 H4 0.8200 . ?
O5 C1 1.235(5) . ?
O6 C1 1.212(5) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 C2 1.480(4) . ?
N1 C6 1.492(4) . ?
C1 C2 1.524(4) . ?
C2 H2 0.9800 . ?
C2 C3 1.511(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.533(6) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.530(6) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.505(6) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?

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
O1 Zn1 O1 111.53(15) 6_564 . ?
O1 Zn1 O5 118.86(12) 6_564 6_564 ?
O1 Zn1 O5 118.86(12) . . ?
O1 Zn1 O5 105.47(14) . 6_564 ?
O1 Zn1 O5 105.47(14) 6_564 . ?
O5 Zn1 O5 96.5(2) 6_564 . ?
O2 Zn2 O2 112.32(15) . 6_564 ?
O2 Zn2 O3 118.22(11) 6_564 10_657 ?
O2 Zn2 O3 105.03(11) 6_564 13_566 ?
O2 Zn2 O3 105.03(11) . 10_657 ?
O2 Zn2 O3 118.22(11) . 13_566 ?
O3 Zn2 O3 97.80(16) 13_566 10_657 ?
O1 P1 O4 109.39(13) . . ?
O2 P1 O1 112.54(15) . . ?
O2 P1 O3 111.86(15) . . ?
O2 P1 O4 107.76(16) . . ?
O3 P1 O1 111.11(15) . . ?
O3 P1 O4 103.73(14) . . ?
P1 O1 Zn1 128.29(14) . . ?
P1 O2 Zn2 138.80(16) . . ?
P1 O3 Zn2 135.85(15) . 13_566 ?
P1 O4 H4 109.5 . . ?
C1 O5 Zn1 134.5(3) . . ?
H1A N1 H1B 107.9 . . ?
C2 N1 H1A 109.1 . . ?
C2 N1 H1B 109.1 . . ?
C2 N1 C6 112.3(3) . . ?
C6 N1 H1A 109.1 . . ?
C6 N1 H1B 109.1 . . ?
O5 C1 C2 114.1(3) . . ?
O6 C1 O5 127.1(3) . . ?
O6 C1 C2 118.5(3) . . ?
N1 C2 C1 110.4(3) . . ?
N1 C2 H2 106.4 . . ?
N1 C2 C3 110.9(3) . . ?
C1 C2 H2 106.4 . . ?
C3 C2 C1 115.7(3) . . ?
C3 C2 H2 106.4 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C2 C3 C4 110.7(3) . . ?
H3A C3 H3B 108.1 . . ?
C4 C3 H3A 109.5 . . ?
C4 C3 H3B 109.5 . . ?
C3 C4 H4A 109.4 . . ?
C3 C4 H4B 109.4 . . ?
H4A C4 H4B 108.0 . . ?
C5 C4 C3 111.0(3) . . ?
C5 C4 H4A 109.4 . . ?
C5 C4 H4B 109.4 . . ?
C4 C5 H5A 109.2 . . ?
C4 C5 H5B 109.2 . . ?
H5A C5 H5B 107.9 . . ?
C6 C5 C4 111.9(3) . . ?
C6 C5 H5A 109.2 . . ?
C6 C5 H5B 109.2 . . ?
N1 C6 C5 109.7(3) . . ?
N1 C6 H6A 109.7 . . ?
N1 C6 H6B 109.7 . . ?
C5 C6 H6A 109.7 . . ?
C5 C6 H6B 109.7 . . ?
H6A C6 H6B 108.2 . . ?

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
O4 H4 O6 0.82 1.85 2.621(4) 157.3 .
N1 H1A O1 0.89 2.07 2.885(3) 151.2 4_566
N1 H1B O3 0.89 1.96 2.845(4) 170.2 7_545

_olex2_date_sample_data_collection 2019-03-19
_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 1.825
_oxdiff_exptl_absorpt_empirical_full_min 0.640
####################################################################### 
# 
# 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_h1-92-6
_database_code_depnum_ccdc_archive 'CCDC 1989711'
loop_
_audit_author_name
_audit_author_address
'Zhien Lin'
;Sichuan University
China
;
_audit_update_record             
;
2020-03-11 deposited with the CCDC.	2020-04-14 downloaded from the CCDC.
;
_audit_creation_date             2019-12-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.04(Ga96 O384 P96), F'
_chemical_formula_sum            'C5 H16 F Ga4 N O21 P4'
_chemical_formula_weight         847.95
_chemical_melting_point          ?
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'
P P 0.2955 0.4335 '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      cubic
_space_group_IT_number           226
_space_group_name_H-M_alt        'F m -3 c'
_space_group_name_Hall           '-F 4c 2 3'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'z, x, y'
'z, -x, -y'
'-z, -x, y'
'-z, x, -y'
'y, z, x'
'-y, z, -x'
'y, -z, -x'
'-y, -z, x'
'y+1/2, x+1/2, -z+1/2'
'-y+1/2, -x+1/2, -z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'x+1/2, z+1/2, -y+1/2'
'-x+1/2, z+1/2, y+1/2'
'-x+1/2, -z+1/2, -y+1/2'
'x+1/2, -z+1/2, y+1/2'
'z+1/2, y+1/2, -x+1/2'
'z+1/2, -y+1/2, x+1/2'
'-z+1/2, y+1/2, x+1/2'
'-z+1/2, -y+1/2, -x+1/2'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'-x, y+1/2, -z+1/2'
'x, -y+1/2, -z+1/2'
'z, x+1/2, y+1/2'
'z, -x+1/2, -y+1/2'
'-z, -x+1/2, y+1/2'
'-z, x+1/2, -y+1/2'
'y, z+1/2, x+1/2'
'-y, z+1/2, -x+1/2'
'y, -z+1/2, -x+1/2'
'-y, -z+1/2, x+1/2'
'y+1/2, x+1, -z+1'
'-y+1/2, -x+1, -z+1'
'y+1/2, -x+1, z+1'
'-y+1/2, x+1, z+1'
'x+1/2, z+1, -y+1'
'-x+1/2, z+1, y+1'
'-x+1/2, -z+1, -y+1'
'x+1/2, -z+1, y+1'
'z+1/2, y+1, -x+1'
'z+1/2, -y+1, x+1'
'-z+1/2, y+1, x+1'
'-z+1/2, -y+1, -x+1'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'-x+1/2, y, -z+1/2'
'x+1/2, -y, -z+1/2'
'z+1/2, x, y+1/2'
'z+1/2, -x, -y+1/2'
'-z+1/2, -x, y+1/2'
'-z+1/2, x, -y+1/2'
'y+1/2, z, x+1/2'
'-y+1/2, z, -x+1/2'
'y+1/2, -z, -x+1/2'
'-y+1/2, -z, x+1/2'
'y+1, x+1/2, -z+1'
'-y+1, -x+1/2, -z+1'
'y+1, -x+1/2, z+1'
'-y+1, x+1/2, z+1'
'x+1, z+1/2, -y+1'
'-x+1, z+1/2, y+1'
'-x+1, -z+1/2, -y+1'
'x+1, -z+1/2, y+1'
'z+1, y+1/2, -x+1'
'z+1, -y+1/2, x+1'
'-z+1, y+1/2, x+1'
'-z+1, -y+1/2, -x+1'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, -z'
'z+1/2, x+1/2, y'
'z+1/2, -x+1/2, -y'
'-z+1/2, -x+1/2, y'
'-z+1/2, x+1/2, -y'
'y+1/2, z+1/2, x'
'-y+1/2, z+1/2, -x'
'y+1/2, -z+1/2, -x'
'-y+1/2, -z+1/2, x'
'y+1, x+1, -z+1/2'
'-y+1, -x+1, -z+1/2'
'y+1, -x+1, z+1/2'
'-y+1, x+1, z+1/2'
'x+1, z+1, -y+1/2'
'-x+1, z+1, y+1/2'
'-x+1, -z+1, -y+1/2'
'x+1, -z+1, y+1/2'
'z+1, y+1, -x+1/2'
'z+1, -y+1, x+1/2'
'-z+1, y+1, x+1/2'
'-z+1, -y+1, -x+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-z, -x, -y'
'-z, x, y'
'z, x, -y'
'z, -x, y'
'-y, -z, -x'
'y, -z, x'
'-y, z, x'
'y, z, -x'
'-y-1/2, -x-1/2, z-1/2'
'y-1/2, x-1/2, z-1/2'
'-y-1/2, x-1/2, -z-1/2'
'y-1/2, -x-1/2, -z-1/2'
'-x-1/2, -z-1/2, y-1/2'
'x-1/2, -z-1/2, -y-1/2'
'x-1/2, z-1/2, y-1/2'
'-x-1/2, z-1/2, -y-1/2'
'-z-1/2, -y-1/2, x-1/2'
'-z-1/2, y-1/2, -x-1/2'
'z-1/2, -y-1/2, -x-1/2'
'z-1/2, y-1/2, x-1/2'
'-x, -y+1/2, -z+1/2'
'x, y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'
'-x, y+1/2, z+1/2'
'-z, -x+1/2, -y+1/2'
'-z, x+1/2, y+1/2'
'z, x+1/2, -y+1/2'
'z, -x+1/2, y+1/2'
'-y, -z+1/2, -x+1/2'
'y, -z+1/2, x+1/2'
'-y, z+1/2, x+1/2'
'y, z+1/2, -x+1/2'
'-y-1/2, -x, z'
'y-1/2, x, z'
'-y-1/2, x, -z'
'y-1/2, -x, -z'
'-x-1/2, -z, y'
'x-1/2, -z, -y'
'x-1/2, z, y'
'-x-1/2, z, -y'
'-z-1/2, -y, x'
'-z-1/2, y, -x'
'z-1/2, -y, -x'
'z-1/2, y, x'
'-x+1/2, -y, -z+1/2'
'x+1/2, y, -z+1/2'
'x+1/2, -y, z+1/2'
'-x+1/2, y, z+1/2'
'-z+1/2, -x, -y+1/2'
'-z+1/2, x, y+1/2'
'z+1/2, x, -y+1/2'
'z+1/2, -x, y+1/2'
'-y+1/2, -z, -x+1/2'
'y+1/2, -z, x+1/2'
'-y+1/2, z, x+1/2'
'y+1/2, z, -x+1/2'
'-y, -x-1/2, z'
'y, x-1/2, z'
'-y, x-1/2, -z'
'y, -x-1/2, -z'
'-x, -z-1/2, y'
'x, -z-1/2, -y'
'x, z-1/2, y'
'-x, z-1/2, -y'
'-z, -y-1/2, x'
'-z, y-1/2, -x'
'z, -y-1/2, -x'
'z, y-1/2, x'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z'
'x+1/2, -y+1/2, z'
'-x+1/2, y+1/2, z'
'-z+1/2, -x+1/2, -y'
'-z+1/2, x+1/2, y'
'z+1/2, x+1/2, -y'
'z+1/2, -x+1/2, y'
'-y+1/2, -z+1/2, -x'
'y+1/2, -z+1/2, x'
'-y+1/2, z+1/2, x'
'y+1/2, z+1/2, -x'
'-y, -x, z-1/2'
'y, x, z-1/2'
'-y, x, -z-1/2'
'y, -x, -z-1/2'
'-x, -z, y-1/2'
'x, -z, -y-1/2'
'x, z, y-1/2'
'-x, z, -y-1/2'
'-z, -y, x-1/2'
'-z, y, -x-1/2'
'z, -y, -x-1/2'
'z, y, x-1/2'

_cell_length_a                   24.02326(18)
_cell_length_b                   24.02326(18)
_cell_length_c                   24.02326(18)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     13864.2(3)
_cell_formula_units_Z            24
_cell_measurement_reflns_used    1754
_cell_measurement_temperature    291.00(10)
_cell_measurement_theta_max      72.3330
_cell_measurement_theta_min      5.2000
_shelx_estimated_absorpt_T_max   0.188
_shelx_estimated_absorpt_T_min   0.124
_exptl_absorpt_coefficient_mu    8.966
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41260
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    2.437
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             9936
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.28
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0501
_diffrn_reflns_av_unetI/netI     0.0260
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            3145
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        66.771
_diffrn_reflns_theta_max         66.771
_diffrn_reflns_theta_min         5.208
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      291.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   23.00   90.00   1.0000    2.2100
omega____ theta____ kappa____ phi______ frames
    -       36.4171 -125.0000  -60.0000 67

#__ type_ start__ end____ width___ exp.time_
  2 omega  -31.00   53.00   1.0000    2.2100
omega____ theta____ kappa____ phi______ frames
    -       36.4171  -57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega   41.00   78.00   1.0000    8.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 37

#__ type_ start__ end____ width___ exp.time_
  4 omega   92.00  150.00   1.0000    8.8400
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  -90.0000 58
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      -0.0212228000
_diffrn_orient_matrix_UB_12      0.0476398000
_diffrn_orient_matrix_UB_13      0.0373158000
_diffrn_orient_matrix_UB_21      0.0000857000
_diffrn_orient_matrix_UB_22      -0.0394890000
_diffrn_orient_matrix_UB_23      0.0505154000
_diffrn_orient_matrix_UB_31      0.0605189000
_diffrn_orient_matrix_UB_32      0.0167609000
_diffrn_orient_matrix_UB_33      0.0130395000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Enhance (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                532
_reflns_number_total             565
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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         1.551
_refine_diff_density_min         -1.152
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    undef
_refine_ls_matrix_type           full
_refine_ls_number_parameters     36
_refine_ls_number_reflns         565
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0652
_refine_ls_restrained_S_all      1.069
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1313P)²+276.9458P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1827
_refine_ls_wR_factor_ref         0.1855
_refine_special_details          ?
_olex2_refinement_description    
;
;
_atom_sites_solution_hydrogens   .
_atom_sites_solution_primary     direct
_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
Ga1 Ga 0.5000 0.58291(5) 0.31027(4) 0.0268(6) Uani 1 2 d S T P . .
P1 P 0.40308(9) 0.5000 0.31862(8) 0.0209(6) Uani 1 2 d S T P . .
O3 O 0.3505(2) 0.5000 0.3514(2) 0.0255(13) Uani 1 2 d S T P . .
O1 O 0.4356(2) 0.5521(2) 0.3328(2) 0.0471(15) Uani 1 1 d . . . . .
O2 O 0.3861(3) 0.5000 0.2575(3) 0.0482(18) Uani 1 2 d S T P . .
F1 F 0.5000 0.5000 0.2500 0.064(4) Uani 1 8 d S T P . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 O3 1.850(6) 106_565 ?
Ga1 O1 1.798(4) . ?
Ga1 O1 1.798(4) 100_655 ?
Ga1 O2 1.791(7) 86 ?
P1 O3 1.489(6) . ?
P1 O1 1.514(5) . ?
P1 O1 1.514(5) 99_565 ?
P1 O2 1.523(6) . ?
O3 Ga1 1.850(6) 6_566 ?
O2 Ga1 1.791(7) 86 ?

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
O1 Ga1 O3 101.19(17) 100_655 106_565 ?
O1 Ga1 O3 101.19(17) . 106_565 ?
O1 Ga1 O1 118.7(4) . 100_655 ?
O2 Ga1 O3 96.9(3) 86 106_565 ?
O2 Ga1 O1 116.4(2) 86 100_655 ?
O2 Ga1 O1 116.4(2) 86 . ?
O3 P1 O1 108.6(2) . . ?
O3 P1 O1 108.6(2) . 99_565 ?
O3 P1 O2 106.4(4) . . ?
O1 P1 O1 111.5(5) . 99_565 ?
O1 P1 O2 110.8(3) . . ?
O1 P1 O2 110.8(3) 99_565 . ?
P1 O3 Ga1 153.4(4) . 6_566 ?
P1 O1 Ga1 135.8(3) . . ?
P1 O2 Ga1 139.9(4) . 86 ?

_smtbx_masks_special_details     ?
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 0.000 0.000 126.5 123.7 ?
2 0.000 0.000 0.500 126.5 123.7 ?
3 -0.193 -0.269 -0.475 5922.7 662.9 ?
4 0.000 0.500 0.000 126.5 123.7 ?
5 0.000 0.500 0.500 126.5 123.7 ?
6 0.500 0.000 0.000 126.5 123.7 ?
7 0.500 0.000 0.500 126.5 123.7 ?
8 0.500 0.500 0.000 126.5 123.7 ?
9 0.500 0.500 0.500 126.5 123.7 ?

_olex2_date_sample_data_collection 2019-03-06
_olex2_submission_special_instructions 'No special instructions were received'
