# 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_1
_database_code_depnum_ccdc_archive 'CCDC 1062250'
_audit_update_record             
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-26
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H2 Co O8 P, C2 H7 N'
_chemical_formula_sum            'C4 H9 Co N O8 P'
_chemical_formula_weight         289.02
_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 0.0033 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'
Co Co 0.3494 0.9721 '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      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   16.3686(9)
_cell_length_b                   8.2405(5)
_cell_length_c                   13.1615(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1775.29(18)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    2296
_cell_measurement_temperature    293
_cell_measurement_theta_max      28.9370
_cell_measurement_theta_min      3.7830
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.141
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82290
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear reddish violet'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    2.163
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1168
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.36
_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  0.0243
_diffrn_reflns_av_unetI/netI     0.0287
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5460
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         3.171
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'New Gemini, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   ?
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1593
_reflns_number_total             1821
_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, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection       
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.870
_refine_diff_density_min         -0.450
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       0.0083(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         1821
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0384
_refine_ls_R_factor_gt           0.0320
_refine_ls_restrained_S_all      1.044
_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)+(0.0332P)²+3.1734P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0762
_refine_ls_wR_factor_ref         0.0803
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Restrained distances
 C4-C5
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5')
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=1-FVAR(1)
 Sof(H4AB)=Sof(H4AA)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4AB,H4AA), C4(H4BC,H4BD), C5(H5A,H5B), C5'(H5'A,H5'B)
5.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C)
5.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O3(H3)
;
_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
Co1 Co 0.41738(2) 0.20341(5) 0.63064(3) 0.01644(15) Uani 1 1 d . . . . .
P1 P 0.43389(4) 0.56995(9) 0.72291(6) 0.0167(2) Uani 1 1 d . . . . .
O1 O 0.43234(14) 0.4507(3) 0.63740(16) 0.0271(5) Uani 1 1 d . . . . .
O2 O 0.37262(14) 0.7108(3) 0.7025(2) 0.0376(6) Uani 1 1 d . . . . .
H2 H 0.3943 0.7792 0.6662 0.056 Uiso 1 1 calc R . . . .
O3 O 0.39795(13) 0.4911(3) 0.82289(16) 0.0254(5) Uani 1 1 d . . . . .
H3 H 0.3721 0.4092 0.8081 0.038 Uiso 1 1 calc R . . . .
O4 O 0.51685(13) 0.6376(3) 0.74449(17) 0.0329(6) Uani 1 1 d . . . . .
O5 O 0.42280(12) -0.0456(2) 0.58671(16) 0.0204(5) Uani 1 1 d . . . . .
O6 O 0.49371(13) -0.2094(2) 0.48428(16) 0.0221(5) Uani 1 1 d . . . . .
O7 O 0.31739(11) 0.2286(3) 0.53163(15) 0.0227(5) Uani 1 1 d . . . . .
O8 O 0.31673(11) 0.2226(3) 0.73561(15) 0.0215(5) Uani 1 1 d . . . . .
N1 N 0.38202(18) 0.5168(4) 0.4168(2) 0.0418(8) Uani 1 1 d . . . . .
H1A H 0.3932 0.4323 0.3771 0.063 Uiso 1 1 calc R . . . .
H1B H 0.4170 0.5968 0.4036 0.063 Uiso 1 1 calc R . . . .
H1C H 0.3866 0.4875 0.4816 0.063 Uiso 1 1 calc R . . . .
C1 C 0.47618(16) -0.0735(3) 0.5206(2) 0.0180(6) Uani 1 1 d . . . . .
C2 C 0.2500 0.2500 0.5746(3) 0.0168(8) Uani 1 2 d S T P . .
C3 C 0.2500 0.2500 0.6922(3) 0.0168(8) Uani 1 2 d S T P . .
C4 C 0.2977(3) 0.5730(6) 0.3970(3) 0.0543(11) Uani 1 1 d D . . . .
H4AB H 0.2909 0.6083 0.3272 0.065 Uiso 0.395(7) 1 calc R . . A 1
H4AA H 0.2579 0.4892 0.4122 0.065 Uiso 0.395(7) 1 calc R . . A 1
H4BC H 0.2661 0.4790 0.3764 0.065 Uiso 0.605(7) 1 calc R . . A 2
H4BD H 0.2999 0.6454 0.3389 0.065 Uiso 0.605(7) 1 calc R . . A 2
C5 C 0.2915(7) 0.7101(11) 0.4686(8) 0.0415(14) Uani 0.395(7) 1 d D . . A 1
H5A H 0.3324 0.7906 0.4511 0.050 Uiso 0.395(7) 1 calc R . . A 1
H5B H 0.3035 0.6715 0.5366 0.050 Uiso 0.395(7) 1 calc R . . A 1
C5' C 0.2494(5) 0.6595(7) 0.4802(5) 0.0415(14) Uani 0.605(7) 1 d . . . A 2
H5'A H 0.1929 0.6248 0.4753 0.050 Uiso 0.605(7) 1 calc R . . A 2
H5'B H 0.2699 0.6226 0.5454 0.050 Uiso 0.605(7) 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
Co1 O1 2.054(2) . ?
Co1 O4 2.038(2) 3_646 ?
Co1 O5 2.134(2) . ?
Co1 O6 2.100(2) 5_656 ?
Co1 O7 2.102(2) . ?
Co1 O8 2.156(2) . ?
P1 O1 1.494(2) . ?
P1 O2 1.557(2) . ?
P1 O3 1.581(2) . ?
P1 O4 1.495(2) . ?
O2 H2 0.8200 . ?
O3 H3 0.8200 . ?
O4 Co1 2.038(2) 3_656 ?
O5 C1 1.255(3) . ?
O6 Co1 2.100(2) 5_656 ?
O6 C1 1.250(3) . ?
O7 C2 1.252(3) . ?
O8 C3 1.253(3) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C4 1.479(5) . ?
C1 C1 1.539(5) 5_656 ?
C2 O7 1.252(3) 2 ?
C2 C3 1.548(6) . ?
C3 O8 1.253(3) 2 ?
C4 H4AB 0.9700 . ?
C4 H4AA 0.9700 . ?
C4 H4BC 0.9700 . ?
C4 H4BD 0.9700 . ?
C4 C5 1.475(8) . ?
C4 C5' 1.527(7) . ?
C5 C5 1.51(2) 2_565 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5' C5' 1.492(12) 2_565 ?
C5' H5'A 0.9700 . ?
C5' H5'B 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 Co1 O5 163.88(8) . . ?
O1 Co1 O6 85.72(8) . 5_656 ?
O1 Co1 O7 91.25(9) . . ?
O1 Co1 O8 89.46(8) . . ?
O4 Co1 O1 99.56(10) 3_646 . ?
O4 Co1 O5 86.60(9) 3_646 . ?
O4 Co1 O6 102.77(9) 3_646 5_656 ?
O4 Co1 O7 159.60(9) 3_646 . ?
O4 Co1 O8 84.63(8) 3_646 . ?
O5 Co1 O8 106.03(8) . . ?
O6 Co1 O5 78.37(7) 5_656 . ?
O6 Co1 O7 95.20(8) 5_656 . ?
O6 Co1 O8 171.74(8) 5_656 . ?
O7 Co1 O5 87.66(8) . . ?
O7 Co1 O8 78.18(8) . . ?
O1 P1 O2 110.46(14) . . ?
O1 P1 O3 110.49(12) . . ?
O1 P1 O4 113.81(14) . . ?
O2 P1 O3 102.14(12) . . ?
O4 P1 O2 109.86(14) . . ?
O4 P1 O3 109.46(12) . . ?
P1 O1 Co1 133.39(13) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 H3 109.5 . . ?
P1 O4 Co1 137.06(14) . 3_656 ?
C1 O5 Co1 113.16(17) . . ?
C1 O6 Co1 114.42(18) . 5_656 ?
C2 O7 Co1 114.8(2) . . ?
C3 O8 Co1 112.8(2) . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C4 N1 H1A 109.5 . . ?
C4 N1 H1B 109.5 . . ?
C4 N1 H1C 109.5 . . ?
O5 C1 C1 116.9(3) . 5_656 ?
O6 C1 O5 126.1(3) . . ?
O6 C1 C1 117.0(3) . 5_656 ?
O7 C2 O7 126.3(4) 2 . ?
O7 C2 C3 116.87(19) . . ?
O7 C2 C3 116.86(19) 2 . ?
O8 C3 O8 125.8(4) 2 . ?
O8 C3 C2 117.10(19) . . ?
O8 C3 C2 117.10(19) 2 . ?
N1 C4 H4AB 111.6 . . ?
N1 C4 H4AA 111.6 . . ?
N1 C4 H4BC 107.3 . . ?
N1 C4 H4BD 107.3 . . ?
N1 C4 C5' 120.2(4) . . ?
H4AB C4 H4AA 109.4 . . ?
H4BC C4 H4BD 106.9 . . ?
C5 C4 N1 101.0(5) . . ?
C5 C4 H4AB 111.6 . . ?
C5 C4 H4AA 111.6 . . ?
C5' C4 H4BC 107.3 . . ?
C5' C4 H4BD 107.3 . . ?
C4 C5 C5 113.3(9) . 2_565 ?
C4 C5 H5A 108.9 . . ?
C4 C5 H5B 108.9 . . ?
C5 C5 H5A 108.9 2_565 . ?
C5 C5 H5B 108.9 2_565 . ?
H5A C5 H5B 107.7 . . ?
C4 C5' H5'A 108.0 . . ?
C4 C5' H5'B 108.0 . . ?
C5' C5' C4 117.3(5) 2_565 . ?
C5' C5' H5'A 108.0 2_565 . ?
C5' C5' H5'B 108.0 2_565 . ?
H5'A C5' H5'B 107.2 . . ?

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
Co1 O5 C1 O6 177.5(2) . . . . ?
Co1 O5 C1 C1 -3.2(4) . . . 5_656 ?
Co1 O6 C1 O5 176.9(2) 5_656 . . . ?
Co1 O6 C1 C1 -2.3(4) 5_656 . . 5_656 ?
Co1 O7 C2 O7 178.38(16) . . . 2 ?
Co1 O7 C2 C3 -1.62(16) . . . . ?
Co1 O8 C3 O8 -174.85(15) . . . 2 ?
Co1 O8 C3 C2 5.15(15) . . . . ?
O1 P1 O4 Co1 -142.7(2) . . . 3_656 ?
O2 P1 O1 Co1 -127.56(18) . . . . ?
O2 P1 O4 Co1 92.9(2) . . . 3_656 ?
O3 P1 O1 Co1 -15.3(2) . . . . ?
O3 P1 O4 Co1 -18.5(3) . . . 3_656 ?
O4 P1 O1 Co1 108.33(19) . . . . ?
O7 C2 C3 O8 177.43(15) 2 . . . ?
O7 C2 C3 O8 -2.58(15) 2 . . 2 ?
O7 C2 C3 O8 177.42(15) . . . 2 ?
O7 C2 C3 O8 -2.57(15) . . . . ?
N1 C4 C5 C5 -177.6(7) . . . 2_565 ?
N1 C4 C5' C5' 95.1(7) . . . 2_565 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1062251'
_audit_update_record             
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C2 H2 O8 P Zn, C2 H7 N'
_chemical_formula_sum            'C4 H9 N O8 P Zn'
_chemical_formula_weight         295.46
_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           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   8.21854(16)
_cell_length_b                   16.3878(3)
_cell_length_c                   13.2772(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     1788.22(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    3189
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.4960
_cell_measurement_theta_min      4.2670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    5.879
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58493
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.195
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1192
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0276
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5107
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.050
_diffrn_reflns_theta_max         67.050
_diffrn_reflns_theta_min         5.399
_diffrn_ambient_temperature      293
_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -99.0000  -90.0000 74

#__ type_ start__ end____ width___ exp.time_
  2 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921 -125.0000   60.0000 67

#__ type_ start__ end____ width___ exp.time_
  3 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921  -99.0000  150.0000 74

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.2921   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -60.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   38.00   91.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -180.0000 53

#__ type_ start__ end____ width___ exp.time_
  8 omega   52.00  106.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 54

#__ type_ start__ end____ width___ exp.time_
  9 omega   39.00  103.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 64

#__ type_ start__ end____ width___ exp.time_
 10 omega   62.00   87.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -120.0000 25

#__ type_ start__ end____ width___ exp.time_
 11 omega   40.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  120.0000 58

#__ type_ start__ end____ width___ exp.time_
 12 omega   66.00   98.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 32
;
_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      -0.1798119000
_diffrn_orient_matrix_UB_12      -0.0183500000
_diffrn_orient_matrix_UB_13      -0.0237292000
_diffrn_orient_matrix_UB_21      -0.0124289000
_diffrn_orient_matrix_UB_22      0.0807773000
_diffrn_orient_matrix_UB_23      -0.0588609000
_diffrn_orient_matrix_UB_31      0.0515015000
_diffrn_orient_matrix_UB_32      -0.0444412000
_diffrn_orient_matrix_UB_33      -0.0971373000
_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'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1516
_reflns_number_total             1597
_reflns_odcompleteness_completeness 99.84
_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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.240
_refine_diff_density_min         -0.545
_refine_diff_density_rms         0.134
_refine_ls_extinction_coef       0.00152(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1597
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0473
_refine_ls_R_factor_gt           0.0458
_refine_ls_restrained_S_all      1.077
_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)+(0.0744P)²+4.2938P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1218
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All C(H,H,H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C4-C5'
 1.51 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
Uanis(C5) = Uanis(C5')
4. Others
 Sof(H4BC)=Sof(H4BD)=Sof(C5')=Sof(H5'A)=Sof(H5'B)=1-FVAR(1)
 Sof(H4AA)=Sof(H4AB)=Sof(C5)=Sof(H5A)=Sof(H5B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C4(H4AA,H4AB), C4(H4BC,H4BD), C5(H5A,H5B), C5'(H5'A,H5'B)
5.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
5.c Idealised tetrahedral OH refined as rotating group:
 O3(H3), 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 0.29785(6) 0.58194(3) 0.63227(4) 0.0175(3) Uani 1 1 d . . . . .
P1 P 0.43137(11) 0.43557(5) 0.77770(7) 0.0164(3) Uani 1 1 d . . . . .
O1 O 0.3632(4) 0.51794(18) 0.7558(2) 0.0336(7) Uani 1 1 d . . . . .
O2 O 0.5509(4) 0.4348(2) 0.8622(2) 0.0270(7) Uani 1 1 d . . . . .
O3 O 0.2907(4) 0.3738(2) 0.7987(3) 0.0393(9) Uani 1 1 d . . . . .
H3 H 0.2256 0.3942 0.8381 0.059 Uiso 1 1 calc GR . . . .
O4 O 0.5100(4) 0.39937(18) 0.67853(19) 0.0263(6) Uani 1 1 d . . . . .
H4 H 0.5941 0.3751 0.6928 0.039 Uiso 1 1 calc GR . . . .
O5 O 0.2895(3) 0.49520(17) 0.5150(2) 0.0219(6) Uani 1 1 d . . . . .
O6 O 0.4520(3) 0.42328(16) 0.4138(2) 0.0217(6) Uani 1 1 d . . . . .
O7 O 0.2699(4) 0.68265(16) 0.5346(2) 0.0241(6) Uani 1 1 d . . . . .
O8 O 0.2790(4) 0.68348(17) 0.7366(2) 0.0246(6) Uani 1 1 d . . . . .
C1 C 0.4252(4) 0.4767(2) 0.4793(3) 0.0174(7) Uani 1 1 d . . . . .
C2 C 0.2500 0.7500 0.5770(4) 0.0189(10) Uani 1 2 d S T P . .
C3 C 0.2500 0.7500 0.6945(4) 0.0176(10) Uani 1 2 d S T P . .
C4 C 0.5754(9) 0.6992(5) 0.8972(5) 0.0662(19) Uani 1 1 d D . . . .
H4AA H 0.4865 0.7327 0.8727 0.079 Uiso 0.558(12) 1 calc R . . A 1
H4AB H 0.6524 0.6936 0.8422 0.079 Uiso 0.558(12) 1 calc R . . A 1
H4BC H 0.4932 0.7408 0.9074 0.079 Uiso 0.442(12) 1 calc R . . A 2
H4BD H 0.6144 0.7024 0.8284 0.079 Uiso 0.442(12) 1 calc R . . A 2
C5 C 0.6597(12) 0.7463(8) 0.9809(9) 0.051(2) Uani 0.558(12) 1 d . . . A 1
H5A H 0.6153 0.8011 0.9808 0.061 Uiso 0.558(12) 1 calc R . . A 1
H5B H 0.6284 0.7213 1.0442 0.061 Uiso 0.558(12) 1 calc R . . A 1
C5' C 0.7115(14) 0.7094(11) 0.9696(10) 0.051(2) Uani 0.442(12) 1 d D . . A 2
H5'A H 0.6710 0.6983 1.0368 0.061 Uiso 0.442(12) 1 calc R . . A 2
H5'B H 0.7940 0.6689 0.9545 0.061 Uiso 0.442(12) 1 calc R . . A 2
N1 N 0.5093(6) 0.6175(2) 0.9188(3) 0.0393(9) Uani 1 1 d . . . . .
H1A H 0.4413 0.6030 0.8698 0.047 Uiso 1 1 calc GR . . . .
H1B H 0.4561 0.6186 0.9772 0.047 Uiso 1 1 calc GR . . . .
H1C H 0.5904 0.5817 0.9224 0.047 Uiso 1 1 calc GR . . . .


_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 2.019(3) . ?
Zn1 O2 2.049(3) 4_466 ?
Zn1 O5 2.109(3) . ?
Zn1 O6 2.147(3) 5_666 ?
Zn1 O7 2.111(3) . ?
Zn1 O8 2.171(3) . ?
P1 O1 1.490(3) . ?
P1 O2 1.491(3) . ?
P1 O3 1.562(3) . ?
P1 O4 1.582(3) . ?
O2 Zn1 2.049(3) 4_566 ?
O3 H3 0.8200 . ?
O4 H4 0.8200 . ?
O5 C1 1.249(4) . ?
O6 Zn1 2.147(3) 5_666 ?
O6 C1 1.253(4) . ?
O7 C2 1.250(4) . ?
O8 C3 1.248(4) . ?
C1 C1 1.548(7) 5_666 ?
C2 O7 1.250(4) 2_565 ?
C2 C3 1.560(7) . ?
C3 O8 1.248(4) 2_565 ?
C4 H4AA 0.9700 . ?
C4 H4AB 0.9700 . ?
C4 H4BC 0.9700 . ?
C4 H4BD 0.9700 . ?
C4 C5 1.519(12) . ?
C4 C5' 1.483(9) . ?
C4 N1 1.473(8) . ?
C5 C5 1.490(19) 2_665 ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5' C5' 1.47(3) 2_665 ?
C5' H5'A 0.9700 . ?
C5' H5'B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

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 O2 99.47(14) . 4_466 ?
O1 Zn1 O5 104.95(12) . . ?
O1 Zn1 O6 87.48(12) . 5_666 ?
O1 Zn1 O7 159.00(12) . . ?
O1 Zn1 O8 84.19(11) . . ?
O2 Zn1 O5 84.49(11) 4_466 . ?
O2 Zn1 O6 162.43(11) 4_466 5_666 ?
O2 Zn1 O7 91.10(12) 4_466 . ?
O2 Zn1 O8 90.54(11) 4_466 . ?
O5 Zn1 O6 78.11(10) . 5_666 ?
O5 Zn1 O7 94.03(11) . . ?
O5 Zn1 O8 170.18(11) . . ?
O6 Zn1 O8 106.30(10) 5_666 . ?
O7 Zn1 O6 87.73(11) . 5_666 ?
O7 Zn1 O8 77.57(11) . . ?
O1 P1 O2 113.70(19) . . ?
O1 P1 O3 110.1(2) . . ?
O1 P1 O4 109.32(16) . . ?
O2 P1 O3 110.4(2) . . ?
O2 P1 O4 110.73(16) . . ?
O3 P1 O4 101.97(17) . . ?
P1 O1 Zn1 136.80(18) . . ?
P1 O2 Zn1 132.89(17) . 4_566 ?
P1 O3 H3 109.5 . . ?
P1 O4 H4 109.5 . . ?
C1 O5 Zn1 114.5(2) . . ?
C1 O6 Zn1 113.2(2) . 5_666 ?
C2 O7 Zn1 115.4(3) . . ?
C3 O8 Zn1 113.4(3) . . ?
O5 C1 O6 126.1(3) . . ?
O5 C1 C1 117.0(4) . 5_666 ?
O6 C1 C1 116.9(4) . 5_666 ?
O7 C2 O7 126.5(5) . 2_565 ?
O7 C2 C3 116.8(2) 2_565 . ?
O7 C2 C3 116.8(2) . . ?
O8 C3 O8 126.8(5) 2_565 . ?
O8 C3 C2 116.6(2) 2_565 . ?
O8 C3 C2 116.6(2) . . ?
H4AA C4 H4AB 107.0 . . ?
H4BC C4 H4BD 108.9 . . ?
C5 C4 H4AA 107.5 . . ?
C5 C4 H4AB 107.5 . . ?
C5' C4 H4BC 110.8 . . ?
C5' C4 H4BD 110.8 . . ?
N1 C4 H4AA 107.5 . . ?
N1 C4 H4AB 107.5 . . ?
N1 C4 H4BC 110.8 . . ?
N1 C4 H4BD 110.8 . . ?
N1 C4 C5 119.2(7) . . ?
N1 C4 C5' 104.8(8) . . ?
C4 C5 H5A 107.4 . . ?
C4 C5 H5B 107.4 . . ?
C5 C5 C4 119.7(8) 2_665 . ?
C5 C5 H5A 107.4 2_665 . ?
C5 C5 H5B 107.4 2_665 . ?
H5A C5 H5B 106.9 . . ?
C4 C5' H5'A 108.5 . . ?
C4 C5' H5'B 108.5 . . ?
C5' C5' C4 115.2(12) 2_665 . ?
C5' C5' H5'A 108.5 2_665 . ?
C5' C5' H5'B 108.5 2_665 . ?
H5'A C5' H5'B 107.5 . . ?
C4 N1 H1A 109.5 . . ?
C4 N1 H1B 109.5 . . ?
C4 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

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
Zn1 O5 C1 O6 175.4(3) . . . . ?
Zn1 O5 C1 C1 -3.8(5) . . . 5_666 ?
Zn1 O6 C1 O5 176.1(3) 5_666 . . . ?
Zn1 O6 C1 C1 -4.8(5) 5_666 . . 5_666 ?
Zn1 O7 C2 O7 -179.6(2) . . . 2_565 ?
Zn1 O7 C2 C3 0.4(2) . . . . ?
Zn1 O8 C3 O8 174.1(2) . . . 2_565 ?
Zn1 O8 C3 C2 -5.9(2) . . . . ?
O1 P1 O2 Zn1 -109.8(3) . . . 4_566 ?
O2 P1 O1 Zn1 142.5(3) . . . . ?
O3 P1 O1 Zn1 -93.0(3) . . . . ?
O3 P1 O2 Zn1 125.9(3) . . . 4_566 ?
O4 P1 O1 Zn1 18.2(4) . . . . ?
O4 P1 O2 Zn1 13.7(3) . . . 4_566 ?
O7 C2 C3 O8 3.9(2) . . . . ?
O7 C2 C3 O8 -176.1(2) . . . 2_565 ?
O7 C2 C3 O8 3.9(2) 2_565 . . 2_565 ?
O7 C2 C3 O8 -176.1(2) 2_565 . . . ?
N1 C4 C5 C5 105.4(12) . . . 2_665 ?
N1 C4 C5' C5' -174.4(10) . . . 2_665 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1062252'
_audit_update_record             
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H3 Mn O7 P, C2 H7 N'
_chemical_formula_sum            'C3 H10 Mn N O7 P'
_chemical_formula_weight         258.03
_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'
Mn Mn -0.5299 2.8052 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.56671(11)
_cell_length_b                   15.6297(3)
_cell_length_c                   9.54079(18)
_cell_angle_alpha                90
_cell_angle_beta                 91.8039(17)
_cell_angle_gamma                90
_cell_volume                     829.69(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2516
_cell_measurement_temperature    293
_cell_measurement_theta_max      71.8550
_cell_measurement_theta_min      5.4340
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    14.973
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.44617
_exptl_absorpt_correction_type   numerical
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear light pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_preparation       ?
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.2
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0460
_diffrn_reflns_av_unetI/netI     0.0365
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            4944
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.059
_diffrn_reflns_theta_max         67.059
_diffrn_reflns_theta_min         5.434
_diffrn_ambient_temperature      293
_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  150.0000 94

#__ type_ start__ end____ width___ exp.time_
  2 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000 -120.0000 67

#__ type_ start__ end____ width___ exp.time_
  3 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -60.0000 94

#__ type_ start__ end____ width___ exp.time_
  5 omega  -31.00   53.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  -30.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega   38.00   91.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   40.00   98.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -60.0000 58

#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   98.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000    0.0000 58

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  109.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  120.0000 70

#__ type_ start__ end____ width___ exp.time_
 11 omega   90.00  175.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -90.0000 85

#__ type_ start__ end____ width___ exp.time_
 12 omega   38.00   91.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
 13 omega   39.00  109.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000    0.0000 70

#__ type_ start__ end____ width___ exp.time_
 14 omega   40.00  135.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -77.0000  150.0000 95

#__ type_ start__ end____ width___ exp.time_
 15 omega   40.00   98.00   1.0000    2.3000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
 16 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000   30.0000 88

#__ type_ start__ end____ width___ exp.time_
 17 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -120.0000 88

#__ type_ start__ end____ width___ exp.time_
 18 omega  -33.00   29.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000  150.0000 62

#__ type_ start__ end____ width___ exp.time_
 19 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000   60.0000 84
;
_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      0.0622825000
_diffrn_orient_matrix_UB_12      0.0874636000
_diffrn_orient_matrix_UB_13      0.0661587000
_diffrn_orient_matrix_UB_21      0.0176686000
_diffrn_orient_matrix_UB_22      0.0393028000
_diffrn_orient_matrix_UB_23      -0.1473943000
_diffrn_orient_matrix_UB_31      -0.2691946000
_diffrn_orient_matrix_UB_32      0.0228122000
_diffrn_orient_matrix_UB_33      0.0003933000
_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'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1407
_reflns_number_total             1481
_reflns_odcompleteness_completeness 99.87
_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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.607
_refine_diff_density_min         -0.701
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1481
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0436
_refine_ls_restrained_S_all      1.035
_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)+(0.0884P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1129
_refine_ls_wR_factor_ref         0.1150
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 OW1(HW1A,HW1B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_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
Mn1 Mn 0.69614(8) 0.66845(3) 0.56126(4) 0.0150(2) Uani 1 1 d . . . . .
P1 P 0.18503(13) 0.69831(5) 0.35375(7) 0.0148(2) Uani 1 1 d . . . . .
O1 O 0.4362(4) 0.72178(15) 0.4062(2) 0.0201(5) Uani 1 1 d . . . . .
O2 O -0.0102(4) 0.72222(14) 0.4528(2) 0.0210(5) Uani 1 1 d . . . . .
O3 O 0.1356(4) 0.73450(15) 0.2078(2) 0.0239(5) Uani 1 1 d . . . . .
O4 O 0.1828(4) 0.59687(14) 0.3359(2) 0.0225(5) Uani 1 1 d . . . . .
H4 H 0.0545 0.5778 0.3620 0.034 Uiso 1 1 calc GR . . . .
O5 O 0.7439(4) 0.55217(14) 0.4287(2) 0.0215(5) Uani 1 1 d . . . . .
O6 O 0.5761(4) 0.42681(14) 0.3702(2) 0.0207(5) Uani 1 1 d . . . . .
OW1 O 0.9774(4) 0.62553(16) 0.7303(2) 0.0294(6) Uani 1 1 d . . . . .
HW1A H 1.0176 0.6680 0.7879 0.044 Uiso 1 1 d GR . . . .
HW1B H 1.1105 0.6075 0.6914 0.044 Uiso 1 1 d GR . . . .
N1 N 0.3033(6) 0.33541(18) 0.8565(3) 0.0232(6) Uani 1 1 d . . . . .
H1A H 0.3791 0.3428 0.7766 0.028 Uiso 1 1 calc GR . . . .
H1B H 0.1595 0.3124 0.8382 0.028 Uiso 1 1 calc GR . . . .
H1C H 0.3891 0.3007 0.9125 0.028 Uiso 1 1 calc GR . . . .
C1 C 0.5926(5) 0.49375(18) 0.4416(3) 0.0162(6) Uani 1 1 d . . . . .
C2 C 0.2738(7) 0.4189(2) 0.9263(4) 0.0292(8) Uani 1 1 d . . . . .
H2A H 0.1821 0.4113 1.0102 0.035 Uiso 1 1 calc R . . . .
H2B H 0.1853 0.4574 0.8640 0.035 Uiso 1 1 calc R . . . .
C3 C 0.5150(7) 0.4574(2) 0.9651(4) 0.0341(9) Uani 1 1 d . . . . .
H3A H 0.6030 0.4191 1.0280 0.041 Uiso 1 1 calc R . . . .
H3B H 0.6073 0.4644 0.8813 0.041 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
Mn1 O1 2.201(2) . ?
Mn1 O2 2.134(2) 1_655 ?
Mn1 O3 2.097(2) 4_676 ?
Mn1 O5 2.235(2) . ?
Mn1 O6 2.237(2) 3_666 ?
Mn1 OW1 2.311(2) . ?
P1 O1 1.515(2) . ?
P1 O2 1.510(2) . ?
P1 O3 1.520(2) . ?
P1 O4 1.595(2) . ?
O2 Mn1 2.134(2) 1_455 ?
O3 Mn1 2.097(2) 4_575 ?
O4 H4 0.8200 . ?
O5 C1 1.251(4) . ?
O6 Mn1 2.237(2) 3_666 ?
O6 C1 1.250(4) . ?
OW1 HW1A 0.8862 . ?
OW1 HW1B 0.8853 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N1 C2 1.476(5) . ?
C1 C1 1.555(6) 3_666 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.507(5) . ?
C3 C3 1.501(7) 3_667 ?
C3 H3A 0.9700 . ?
C3 H3B 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 Mn1 O5 90.85(9) . . ?
O1 Mn1 O6 90.66(8) . 3_666 ?
O1 Mn1 OW1 174.62(9) . . ?
O2 Mn1 O1 91.28(8) 1_655 . ?
O2 Mn1 O5 86.51(8) 1_655 . ?
O2 Mn1 O6 160.07(8) 1_655 3_666 ?
O2 Mn1 OW1 86.57(9) 1_655 . ?
O3 Mn1 O1 93.33(8) 4_676 . ?
O3 Mn1 O2 100.37(9) 4_676 1_655 ?
O3 Mn1 O5 171.85(9) 4_676 . ?
O3 Mn1 O6 99.31(9) 4_676 3_666 ?
O3 Mn1 OW1 82.21(9) 4_676 . ?
O5 Mn1 O6 73.63(8) . 3_666 ?
O5 Mn1 OW1 93.95(9) . . ?
O6 Mn1 OW1 93.04(9) 3_666 . ?
O1 P1 O3 110.54(13) . . ?
O1 P1 O4 106.27(13) . . ?
O2 P1 O1 114.12(12) . . ?
O2 P1 O3 111.61(13) . . ?
O2 P1 O4 108.04(12) . . ?
O3 P1 O4 105.74(12) . . ?
P1 O1 Mn1 135.29(13) . . ?
P1 O2 Mn1 141.59(14) . 1_455 ?
P1 O3 Mn1 148.36(14) . 4_575 ?
P1 O4 H4 109.5 . . ?
C1 O5 Mn1 116.43(19) . . ?
C1 O6 Mn1 115.88(18) . 3_666 ?
Mn1 OW1 HW1A 111.6 . . ?
Mn1 OW1 HW1B 111.0 . . ?
HW1A OW1 HW1B 107.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
O5 C1 C1 116.3(3) . 3_666 ?
O6 C1 O5 126.5(3) . . ?
O6 C1 C1 117.2(3) . 3_666 ?
N1 C2 H2A 109.5 . . ?
N1 C2 H2B 109.5 . . ?
N1 C2 C3 110.7(3) . . ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.5 . . ?
C3 C2 H2B 109.5 . . ?
C2 C3 H3A 109.5 . . ?
C2 C3 H3B 109.5 . . ?
C3 C3 C2 110.7(4) 3_667 . ?
C3 C3 H3A 109.5 3_667 . ?
C3 C3 H3B 109.5 3_667 . ?
H3A C3 H3B 108.1 . . ?

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
Mn1 O5 C1 O6 174.2(2) . . . . ?
Mn1 O5 C1 C1 -5.8(4) . . . 3_666 ?
Mn1 O6 C1 O5 174.2(2) 3_666 . . . ?
Mn1 O6 C1 C1 -5.8(4) 3_666 . . 3_666 ?
O1 P1 O2 Mn1 -125.3(2) . . . 1_455 ?
O1 P1 O3 Mn1 -31.2(3) . . . 4_575 ?
O2 P1 O1 Mn1 76.8(2) . . . . ?
O2 P1 O3 Mn1 96.9(3) . . . 4_575 ?
O3 P1 O1 Mn1 -156.41(17) . . . . ?
O3 P1 O2 Mn1 108.4(2) . . . 1_455 ?
O4 P1 O1 Mn1 -42.1(2) . . . . ?
O4 P1 O2 Mn1 -7.4(3) . . . 1_455 ?
O4 P1 O3 Mn1 -145.8(3) . . . 4_575 ?
N1 C2 C3 C3 179.5(4) . . . 3_667 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1062253'
_audit_update_record             
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H3 Cd O7 P, C2 H7 N'
_chemical_formula_sum            'C3 H10 Cd N O7 P'
_chemical_formula_weight         315.49
_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'
Cd Cd 0.1185 4.6533 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   5.63389(10)
_cell_length_b                   15.9428(2)
_cell_length_c                   9.61828(15)
_cell_angle_alpha                90
_cell_angle_beta                 91.1156(15)
_cell_angle_gamma                90
_cell_volume                     863.75(2)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4791
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.4750
_cell_measurement_theta_min      5.3640
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    22.209
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.31729
_exptl_absorpt_correction_type   numerical
_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)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.426
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             616
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0298
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6211
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.061
_diffrn_reflns_theta_max         67.061
_diffrn_reflns_theta_min         5.372
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9797
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   23.00   90.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000   90.0000 67

#__ type_ start__ end____ width___ exp.time_
  2 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00   63.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -77.0000  150.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega    1.00   75.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -99.0000  -90.0000 74

#__ type_ start__ end____ width___ exp.time_
  6 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000 -150.0000 88

#__ type_ start__ end____ width___ exp.time_
  7 omega   39.00  109.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000   30.0000 70

#__ type_ start__ end____ width___ exp.time_
  8 omega   40.00   98.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  120.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   91.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000 -120.0000 85

#__ type_ start__ end____ width___ exp.time_
 11 omega   38.00  116.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000  -90.0000 78

#__ type_ start__ end____ width___ exp.time_
 12 omega   81.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   77.0000  -90.0000 95

#__ type_ start__ end____ width___ exp.time_
 13 omega  100.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000   90.0000 78

#__ type_ start__ end____ width___ exp.time_
 14 omega  100.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000 -180.0000 78

#__ type_ start__ end____ width___ exp.time_
 15 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -120.0000 84

#__ type_ start__ end____ width___ exp.time_
 16 omega   10.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   30.0000 94

#__ type_ start__ end____ width___ exp.time_
 17 omega  -33.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000  -30.0000 88

#__ type_ start__ end____ width___ exp.time_
 18 omega   20.00  104.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
 19 omega   18.00  106.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   38.0000  150.0000 88

#__ type_ start__ end____ width___ exp.time_
 20 omega   91.00  176.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000  150.0000 85

#__ type_ start__ end____ width___ exp.time_
 21 omega   87.00  178.00   1.0000    1.9200
omega____ theta____ kappa____ phi______ frames
    -      108.0000   30.0000   60.0000 91
;
_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      -0.0135186000
_diffrn_orient_matrix_UB_12      -0.0863845000
_diffrn_orient_matrix_UB_13      -0.0714689000
_diffrn_orient_matrix_UB_21      -0.0816157000
_diffrn_orient_matrix_UB_22      -0.0398187000
_diffrn_orient_matrix_UB_23      0.1369433000
_diffrn_orient_matrix_UB_31      -0.2607205000
_diffrn_orient_matrix_UB_32      0.0169459000
_diffrn_orient_matrix_UB_33      -0.0424697000
_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                1489
_reflns_number_total             1540
_reflns_odcompleteness_completeness 99.88
_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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS-1997 (Sheldrick, 2008)'
_refine_diff_density_max         1.362
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.206
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.120
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     121
_refine_ls_number_reflns         1540
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0395
_refine_ls_restrained_S_all      1.120
_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)+(0.0764P)²+0.0960P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1032
_refine_ls_wR_factor_ref         0.1046
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2.a Rotating group:
 OW1(HW1A,HW1B)
2.b Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.c Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.d Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_atom_sites_solution_hydrogens   mixed
_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
Cd1 Cd 0.29808(5) 0.33175(2) 0.93741(3) 0.01755(19) Uani 1 1 d . . . . .
P1 P 0.3075(2) 0.19603(7) 0.65010(11) 0.0170(3) Uani 1 1 d . . . . .
O1 O 0.3638(7) 0.2262(2) 0.7973(3) 0.0284(8) Uani 1 1 d . . . . .
O2 O 0.4921(6) 0.2244(2) 0.5484(4) 0.0270(8) Uani 1 1 d . . . . .
O3 O 0.0562(6) 0.2196(2) 0.6074(3) 0.0230(7) Uani 1 1 d . . . . .
O4 O 0.3131(6) 0.0963(2) 0.6579(3) 0.0253(7) Uani 1 1 d . . . . .
H4 H 0.4480 0.0796 0.6434 0.038 Uiso 1 1 calc GR . . . .
O5 O 0.5759(6) 0.4288(2) 0.8684(3) 0.0234(7) Uani 1 1 d . . . . .
O6 O 0.7457(7) 0.5497(2) 0.9280(3) 0.0241(7) Uani 1 1 d . . . . .
OW1 O 0.0141(7) 0.3726(2) 0.7616(4) 0.0310(8) Uani 1 1 d . . . . .
HW1A H -0.1156 0.3864 0.7993 0.047 Uiso 1 1 d GR . . . .
HW1B H -0.0104 0.3317 0.7066 0.047 Uiso 1 1 d GR . . . .
C1 C 0.5924(8) 0.4939(3) 0.9411(4) 0.0184(9) Uani 1 1 d . . . . .
C2 C 0.2731(10) 0.4214(4) 0.4282(5) 0.0313(12) Uani 1 1 d . . . . .
H2A H 0.1790 0.4163 0.5111 0.038 Uiso 1 1 calc R . . . .
H2B H 0.1908 0.4592 0.3645 0.038 Uiso 1 1 calc R . . . .
C3 C 0.5116(10) 0.4575(3) 0.4665(6) 0.0334(12) Uani 1 1 d . . . . .
H3A H 0.6059 0.4625 0.3836 0.040 Uiso 1 1 calc R . . . .
H3B H 0.5938 0.4198 0.5303 0.040 Uiso 1 1 calc R . . . .
N1 N 0.2968(9) 0.3382(2) 0.3623(5) 0.0243(9) Uani 1 1 d . . . . .
H1A H 0.3788 0.3431 0.2846 0.029 Uiso 1 1 calc GR . . . .
H1B H 0.1533 0.3177 0.3421 0.029 Uiso 1 1 calc GR . . . .
H1C H 0.3726 0.3036 0.4206 0.029 Uiso 1 1 calc GR . . . .


_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
Cd1 O1 2.191(3) . ?
Cd1 O2 2.232(3) 4_566 ?
Cd1 O3 2.317(3) 4_666 ?
Cd1 O5 2.308(3) . ?
Cd1 O6 2.307(3) 3_667 ?
Cd1 OW1 2.395(4) . ?
P1 O1 1.523(3) . ?
P1 O2 1.511(3) . ?
P1 O3 1.514(4) . ?
P1 O4 1.592(3) . ?
O2 Cd1 2.232(3) 4_665 ?
O3 Cd1 2.317(3) 4_565 ?
O4 H4 0.8200 . ?
O5 C1 1.254(6) . ?
O6 Cd1 2.307(3) 3_667 ?
O6 C1 1.248(6) . ?
OW1 HW1A 0.8504 . ?
OW1 HW1B 0.8505 . ?
C1 C1 1.566(8) 3_667 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.501(8) . ?
C2 N1 1.478(7) . ?
C3 C3 1.507(10) 3_666 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

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 Cd1 O2 97.34(13) . 4_566 ?
O1 Cd1 O3 92.96(12) . 4_666 ?
O1 Cd1 O5 102.36(13) . . ?
O1 Cd1 O6 174.40(13) . 3_667 ?
O1 Cd1 OW1 83.88(13) . . ?
O2 Cd1 O3 90.05(12) 4_566 4_666 ?
O2 Cd1 O5 160.17(12) 4_566 . ?
O2 Cd1 O6 88.16(12) 4_566 3_667 ?
O2 Cd1 OW1 86.29(13) 4_566 . ?
O3 Cd1 OW1 174.81(12) 4_666 . ?
O5 Cd1 O3 91.14(12) . 4_666 ?
O5 Cd1 OW1 93.55(13) . . ?
O6 Cd1 O3 88.05(13) 3_667 4_666 ?
O6 Cd1 O5 72.09(11) 3_667 . ?
O6 Cd1 OW1 95.50(13) 3_667 . ?
O1 P1 O4 105.6(2) . . ?
O2 P1 O1 111.9(2) . . ?
O2 P1 O3 113.7(2) . . ?
O2 P1 O4 108.44(19) . . ?
O3 P1 O1 110.51(19) . . ?
O3 P1 O4 106.2(2) . . ?
P1 O1 Cd1 141.2(2) . . ?
P1 O2 Cd1 137.5(2) . 4_665 ?
P1 O3 Cd1 132.43(19) . 4_565 ?
P1 O4 H4 109.5 . . ?
C1 O5 Cd1 116.0(3) . . ?
C1 O6 Cd1 116.4(3) . 3_667 ?
Cd1 OW1 HW1A 109.7 . . ?
Cd1 OW1 HW1B 109.2 . . ?
HW1A OW1 HW1B 109.4 . . ?
O5 C1 C1 117.6(5) . 3_667 ?
O6 C1 O5 125.3(4) . . ?
O6 C1 C1 117.1(5) . 3_667 ?
H2A C2 H2B 108.0 . . ?
C3 C2 H2A 109.4 . . ?
C3 C2 H2B 109.4 . . ?
N1 C2 H2A 109.4 . . ?
N1 C2 H2B 109.4 . . ?
N1 C2 C3 111.2(5) . . ?
C2 C3 C3 111.4(6) . 3_666 ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C3 C3 H3A 109.4 3_666 . ?
C3 C3 H3B 109.4 3_666 . ?
H3A C3 H3B 108.0 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

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
Cd1 O5 C1 O6 173.2(4) . . . . ?
Cd1 O5 C1 C1 -6.2(7) . . . 3_667 ?
Cd1 O6 C1 O5 173.6(4) 3_667 . . . ?
Cd1 O6 C1 C1 -7.1(7) 3_667 . . 3_667 ?
O1 P1 O2 Cd1 103.6(3) . . . 4_665 ?
O1 P1 O3 Cd1 -159.6(3) . . . 4_565 ?
O2 P1 O1 Cd1 90.4(4) . . . . ?
O2 P1 O3 Cd1 73.5(3) . . . 4_565 ?
O3 P1 O1 Cd1 -37.5(4) . . . . ?
O3 P1 O2 Cd1 -130.3(3) . . . 4_665 ?
O4 P1 O1 Cd1 -151.8(3) . . . . ?
O4 P1 O2 Cd1 -12.5(4) . . . 4_665 ?
O4 P1 O3 Cd1 -45.6(3) . . . 4_565 ?
N1 C2 C3 C3 179.9(6) . . . 3_666 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1062254'
_audit_update_record             
;
2015-06-27 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-27
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '0.5(C8 H16 Ga8 O76 P14), 2(C4 H14 N2)'
_chemical_formula_sum            'C12 H41 Ga4 N4 O38 P7'
_chemical_formula_weight         1345.16
_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'
Ga Ga -1.2846 0.7763 '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'

_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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   6.21517(5)
_cell_length_b                   18.83913(15)
_cell_length_c                   16.65678(13)
_cell_angle_alpha                90
_cell_angle_beta                 92.2293(7)
_cell_angle_gamma                90
_cell_volume                     1948.84(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    10276
_cell_measurement_temperature    293
_cell_measurement_theta_max      72.5860
_cell_measurement_theta_min      4.6790
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    7.109
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79632
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.292
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_F_000             1348
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.08
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0927
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            20197
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.069
_diffrn_reflns_theta_max         67.069
_diffrn_reflns_theta_min         4.694
_diffrn_ambient_temperature      293
_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      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -33.00  106.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421    0.0000  120.0000 139

#__ type_ start__ end____ width___ exp.time_
  2 omega   10.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  3 omega  -31.00   53.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  -60.0000 84

#__ type_ start__ end____ width___ exp.time_
  4 omega   20.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega   23.00   90.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000  -60.0000 67

#__ type_ start__ end____ width___ exp.time_
  6 omega   10.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   60.0000 94

#__ type_ start__ end____ width___ exp.time_
  7 omega   23.00   90.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421 -125.0000  150.0000 67

#__ type_ start__ end____ width___ exp.time_
  8 omega  -31.00   53.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000 -150.0000 84

#__ type_ start__ end____ width___ exp.time_
  9 omega   38.00   91.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000 -150.0000 53

#__ type_ start__ end____ width___ exp.time_
 10 omega   39.00  109.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000 -180.0000 70

#__ type_ start__ end____ width___ exp.time_
 11 omega   91.00  176.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   45.0000   30.0000 85

#__ type_ start__ end____ width___ exp.time_
 12 omega   38.00   91.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000  -30.0000 53

#__ type_ start__ end____ width___ exp.time_
 13 omega   41.00  126.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000 -180.0000 85

#__ type_ start__ end____ width___ exp.time_
 14 omega   40.00   98.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000   30.0000 58

#__ type_ start__ end____ width___ exp.time_
 15 omega   70.00  178.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   15.0000  -90.0000 108

#__ type_ start__ end____ width___ exp.time_
 16 omega  100.00  178.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  111.0000  -90.0000 78

#__ type_ start__ end____ width___ exp.time_
 17 omega   57.00  150.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  178.0000 -120.0000 93

#__ type_ start__ end____ width___ exp.time_
 18 omega   91.00  177.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  129.0000   54.0000 86

#__ type_ start__ end____ width___ exp.time_
 19 omega   39.00  109.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -94.0000  -60.0000 70

#__ type_ start__ end____ width___ exp.time_
 20 omega   40.00   98.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -45.0000  -90.0000 58

#__ type_ start__ end____ width___ exp.time_
 21 omega   41.00  126.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -61.0000  -60.0000 85

#__ type_ start__ end____ width___ exp.time_
 22 omega   90.00  175.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000   61.0000  -30.0000 85

#__ type_ start__ end____ width___ exp.time_
 23 omega   38.00   91.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000  -30.0000   90.0000 53

#__ type_ start__ end____ width___ exp.time_
 24 omega   38.00  116.00   1.0000    4.4000
omega____ theta____ kappa____ phi______ frames
    -      108.0000 -111.0000   60.0000 78

#__ type_ start__ end____ width___ exp.time_
 25 omega   10.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000  -30.0000 94

#__ type_ start__ end____ width___ exp.time_
 26 omega   10.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000 -180.0000 94

#__ type_ start__ end____ width___ exp.time_
 27 omega  -31.00   53.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -57.0000  120.0000 84

#__ type_ start__ end____ width___ exp.time_
 28 omega   10.00  104.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421   77.0000   90.0000 94

#__ type_ start__ end____ width___ exp.time_
 29 omega  -33.00   55.00   1.0000    1.1000
omega____ theta____ kappa____ phi______ frames
    -       36.5421  -38.0000   30.0000 88
;
_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      0.0141809000
_diffrn_orient_matrix_UB_12      0.0776276000
_diffrn_orient_matrix_UB_13      -0.0283704000
_diffrn_orient_matrix_UB_21      -0.0092068000
_diffrn_orient_matrix_UB_22      0.0254712000
_diffrn_orient_matrix_UB_23      0.0876776000
_diffrn_orient_matrix_UB_31      0.2475220000
_diffrn_orient_matrix_UB_32      -0.0035056000
_diffrn_orient_matrix_UB_33      0.0084871000
_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                3323
_reflns_number_total             3486
_reflns_odcompleteness_completeness 99.92
_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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.094
_refine_diff_density_min         -0.877
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         3486
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.056
_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)+(0.0960P)²+4.1587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1352
_refine_ls_wR_factor_ref         0.1377
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All N(H,H,H) groups, All O(H) groups
2. Others
 Fixed Sof: P4(0.5) O14(0.5) O15(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B)
3.b Me refined with riding coordinates:
 N1(H1A,H1B,H1C), N2(H2A,H2B,H2C)
3.c Tetrahedral OH refined with riding coordinates:
 O2(H2), O7(H7), O8(H8), O10(H10)
;
_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
Ga1 Ga 0.76728(7) 0.44126(2) 0.59771(3) 0.00708(18) Uani 1 1 d . . . . .
Ga2 Ga 0.71357(7) 0.65813(2) 0.88290(3) 0.01055(18) Uani 1 1 d . . . . .
P1 P 0.74114(14) 0.55873(4) 0.44932(5) 0.0072(2) Uani 1 1 d . . . . .
P2 P 0.83625(16) 0.53572(5) 0.76108(6) 0.0128(2) Uani 1 1 d . . . . .
P3 P 0.22093(15) 0.69046(5) 0.92124(6) 0.0130(2) Uani 1 1 d . . . . .
P4 P 0.8129(4) 0.53097(11) 1.01756(12) 0.0176(4) Uani 0.5 1 d . . P . .
O1 O 0.7577(4) 0.49210(15) 0.49951(16) 0.0144(6) Uani 1 1 d . . . . .
O2 O 0.7391(5) 0.62326(15) 0.50768(17) 0.0169(6) Uani 1 1 d . . . . .
H2 H 0.7302 0.6601 0.4816 0.025 Uiso 1 1 calc R . . . .
O3 O 0.5397(4) 0.55833(14) 0.39467(16) 0.0142(6) Uani 1 1 d . . . . .
O4 O 0.9258(4) 0.56496(14) 0.39187(16) 0.0123(6) Uani 1 1 d . . . . .
O5 O 0.7735(5) 0.51849(15) 0.67576(17) 0.0167(6) Uani 1 1 d . . . . .
O6 O 0.6983(4) 0.59471(15) 0.79144(17) 0.0186(6) Uani 1 1 d . . . . .
O7 O 0.8157(7) 0.46763(17) 0.8122(2) 0.0347(9) Uani 1 1 d . . . . .
H7 H 0.8497 0.4765 0.8592 0.052 Uiso 1 1 calc R . . . .
O8 O 1.0791(5) 0.55873(17) 0.7660(2) 0.0256(7) Uani 1 1 d . . . . .
H8 H 1.1147 0.5683 0.8127 0.038 Uiso 1 1 calc R . . . .
O9 O 0.4085(5) 0.6581(2) 0.8789(2) 0.0348(9) Uani 1 1 d . . . . .
O10 O 0.2334(7) 0.6719(2) 1.0128(2) 0.0382(9) Uani 1 1 d . . . . .
H10 H 0.2407 0.6288 1.0185 0.057 Uiso 1 1 calc R . . . .
O11 O 0.0257(5) 0.65072(15) 0.88353(18) 0.0192(6) Uani 1 1 d . . . . .
O12 O 0.2079(6) 0.76901(17) 0.9139(2) 0.0298(8) Uani 1 1 d . . . . .
O13 O 0.7089(7) 0.58321(19) 0.9655(2) 0.0400(10) Uani 1 1 d . . . . .
O14 O 0.8906(12) 0.4678(3) 0.9684(4) 0.0296(15) Uani 0.5 1 d . . P . .
O15 O 0.9923(11) 0.5687(4) 1.0651(4) 0.0292(15) Uani 0.5 1 d . . P . .
O16 O 0.6390(10) 0.5064(3) 1.0896(3) 0.0732(17) Uani 1 1 d . . . . .
O17 O 0.7234(5) 0.74359(14) 0.80784(16) 0.0166(6) Uani 1 1 d . . . . .
O18 O 0.7368(4) 0.86175(14) 0.81574(16) 0.0125(5) Uani 1 1 d . . . . .
O19 O 0.7281(4) 0.73486(14) 0.96682(16) 0.0124(6) Uani 1 1 d . . . . .
O20 O 0.7411(4) 0.85303(14) 0.97444(16) 0.0117(5) Uani 1 1 d . . . . .
C1 C 0.7312(6) 0.8008(2) 0.8449(2) 0.0121(8) Uani 1 1 d . . . . .
C2 C 0.7337(6) 0.7959(2) 0.9375(2) 0.0100(7) Uani 1 1 d . . . . .
C3 C 0.7421(11) 0.6690(3) 0.2265(3) 0.0432(14) Uani 1 1 d . . . . .
H3A H 0.8940 0.6705 0.2153 0.052 Uiso 1 1 calc R . . . .
H3B H 0.7217 0.6954 0.2757 0.052 Uiso 1 1 calc R . . . .
C4 C 0.6148(10) 0.7034(3) 0.1589(3) 0.0401(13) Uani 1 1 d . . . . .
H4A H 0.4633 0.6928 0.1640 0.048 Uiso 1 1 calc R . . . .
H4B H 0.6591 0.6838 0.1082 0.048 Uiso 1 1 calc R . . . .
C5 C 0.6460(10) 0.7833(3) 0.1581(3) 0.0426(13) Uani 1 1 d . . . . .
H5A H 0.5596 0.8029 0.1137 0.051 Uiso 1 1 calc R . . . .
H5B H 0.5914 0.8027 0.2073 0.051 Uiso 1 1 calc R . . . .
C6 C 0.8761(10) 0.8081(3) 0.1506(3) 0.0402(13) Uani 1 1 d . . . . .
H6A H 0.9592 0.7961 0.1992 0.048 Uiso 1 1 calc R . . . .
H6B H 0.9399 0.7839 0.1060 0.048 Uiso 1 1 calc R . . . .
N1 N 0.6759(9) 0.5942(3) 0.2382(3) 0.0483(13) Uani 1 1 d . . . . .
H1A H 0.7542 0.5753 0.2787 0.072 Uiso 1 1 calc R . . . .
H1B H 0.5372 0.5927 0.2494 0.072 Uiso 1 1 calc R . . . .
H1C H 0.6968 0.5697 0.1935 0.072 Uiso 1 1 calc R . . . .
N2 N 0.8846(8) 0.8866(2) 0.1373(2) 0.0339(10) Uani 1 1 d . . . . .
H2A H 1.0209 0.9001 0.1330 0.051 Uiso 1 1 calc R . . . .
H2B H 0.8100 0.8975 0.0923 0.051 Uiso 1 1 calc R . . . .
H2C H 0.8280 0.9089 0.1786 0.051 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ga1 O1 1.894(3) . ?
Ga1 O3 1.917(3) 3_666 ?
Ga1 O4 1.913(3) 3_766 ?
Ga1 O5 1.950(3) . ?
Ga1 O18 2.080(3) 2_646 ?
Ga1 O20 2.051(3) 2_646 ?
Ga2 O6 1.935(3) . ?
Ga2 O9 1.895(3) . ?
Ga2 O11 1.945(3) 1_655 ?
Ga2 O13 1.972(3) . ?
Ga2 O17 2.041(3) . ?
Ga2 O19 2.011(3) . ?
P1 O1 1.510(3) . ?
P1 O2 1.557(3) . ?
P1 O3 1.519(3) . ?
P1 O4 1.527(3) . ?
P2 O5 1.495(3) . ?
P2 O6 1.503(3) . ?
P2 O7 1.547(3) . ?
P2 O8 1.570(3) . ?
P3 O9 1.514(3) . ?
P3 O10 1.564(4) . ?
P3 O11 1.539(3) . ?
P3 O12 1.487(3) . ?
P4 P4 2.687(4) 3_767 ?
P4 O13 1.447(4) . ?
P4 O14 1.848(8) 3_767 ?
P4 O14 1.534(7) . ?
P4 O15 1.519(7) . ?
P4 O16 1.710(6) . ?
O2 H2 0.8200 . ?
O3 Ga1 1.917(3) 3_666 ?
O4 Ga1 1.912(3) 3_766 ?
O7 H7 0.8200 . ?
O8 H8 0.8200 . ?
O10 H10 0.8200 . ?
O11 Ga2 1.945(3) 1_455 ?
O14 P4 1.848(7) 3_767 ?
O14 O15 1.159(10) 3_767 ?
O15 O14 1.159(10) 3_767 ?
O17 C1 1.243(5) . ?
O18 Ga1 2.080(3) 2_656 ?
O18 C1 1.247(5) . ?
O19 C2 1.251(5) . ?
O20 Ga1 2.051(3) 2_656 ?
O20 C2 1.240(5) . ?
C1 C2 1.544(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C3 C4 1.499(8) . ?
C3 N1 1.483(8) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C4 C5 1.519(8) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C5 C6 1.514(9) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C6 N2 1.497(7) . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?
N2 H2A 0.8900 . ?
N2 H2B 0.8900 . ?
N2 H2C 0.8900 . ?

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 93.29(11) . 3_666 ?
O1 Ga1 O4 96.14(11) . 3_766 ?
O1 Ga1 O5 101.39(12) . . ?
O1 Ga1 O18 164.12(12) . 2_646 ?
O1 Ga1 O20 84.53(11) . 2_646 ?
O3 Ga1 O5 86.96(12) 3_666 . ?
O3 Ga1 O18 85.30(11) 3_666 2_646 ?
O3 Ga1 O20 92.25(11) 3_666 2_646 ?
O4 Ga1 O3 170.42(11) 3_766 3_666 ?
O4 Ga1 O5 89.50(12) 3_766 . ?
O4 Ga1 O18 86.09(11) 3_766 2_646 ?
O4 Ga1 O20 90.35(11) 3_766 2_646 ?
O5 Ga1 O18 94.34(12) . 2_646 ?
O5 Ga1 O20 174.06(11) . 2_646 ?
O20 Ga1 O18 79.73(10) 2_646 2_646 ?
O6 Ga2 O11 88.75(12) . 1_655 ?
O6 Ga2 O13 96.08(14) . . ?
O6 Ga2 O17 90.37(12) . . ?
O6 Ga2 O19 172.15(12) . . ?
O9 Ga2 O6 87.34(13) . . ?
O9 Ga2 O11 175.52(13) . 1_655 ?
O9 Ga2 O13 89.00(19) . . ?
O9 Ga2 O17 91.85(15) . . ?
O9 Ga2 O19 92.44(12) . . ?
O11 Ga2 O13 89.24(16) 1_655 . ?
O11 Ga2 O17 90.37(13) 1_655 . ?
O11 Ga2 O19 91.73(11) 1_655 . ?
O13 Ga2 O17 173.53(14) . . ?
O13 Ga2 O19 91.77(14) . . ?
O19 Ga2 O17 81.79(11) . . ?
O1 P1 O2 107.78(16) . . ?
O1 P1 O3 111.39(16) . . ?
O1 P1 O4 111.97(15) . . ?
O3 P1 O2 110.58(16) . . ?
O3 P1 O4 104.29(16) . . ?
O4 P1 O2 110.85(15) . . ?
O5 P2 O6 110.45(17) . . ?
O5 P2 O7 108.59(18) . . ?
O5 P2 O8 108.95(17) . . ?
O6 P2 O7 111.56(19) . . ?
O6 P2 O8 109.76(17) . . ?
O7 P2 O8 107.4(2) . . ?
O9 P3 O10 110.8(2) . . ?
O9 P3 O11 102.88(18) . . ?
O11 P3 O10 107.34(19) . . ?
O12 P3 O9 113.8(2) . . ?
O12 P3 O10 107.6(2) . . ?
O12 P3 O11 114.27(19) . . ?
O13 P4 P4 122.4(2) . 3_767 ?
O13 P4 O14 110.5(3) . . ?
O13 P4 O14 119.2(3) . 3_767 ?
O13 P4 O15 107.2(3) . . ?
O13 P4 O16 108.9(3) . . ?
O14 P4 P4 41.7(3) . 3_767 ?
O14 P4 P4 33.5(2) 3_767 3_767 ?
O14 P4 O14 75.2(4) . 3_767 ?
O14 P4 O16 112.7(4) . . ?
O15 P4 P4 72.1(3) . 3_767 ?
O15 P4 O14 38.7(3) . 3_767 ?
O15 P4 O14 113.7(4) . . ?
O15 P4 O16 103.4(3) . . ?
O16 P4 P4 127.7(3) . 3_767 ?
O16 P4 O14 124.6(3) . 3_767 ?
P1 O1 Ga1 153.88(19) . . ?
P1 O2 H2 109.5 . . ?
P1 O3 Ga1 139.42(17) . 3_666 ?
P1 O4 Ga1 135.21(17) . 3_766 ?
P2 O5 Ga1 142.51(19) . . ?
P2 O6 Ga2 135.24(18) . . ?
P2 O7 H7 109.5 . . ?
P2 O8 H8 109.5 . . ?
P3 O9 Ga2 140.4(2) . . ?
P3 O10 H10 109.5 . . ?
P3 O11 Ga2 137.55(18) . 1_455 ?
P4 O13 Ga2 152.4(3) . . ?
P4 O14 P4 104.8(4) . 3_767 ?
O15 O14 P4 55.1(4) 3_767 3_767 ?
O15 O14 P4 159.0(7) 3_767 . ?
O14 O15 P4 86.2(6) 3_767 . ?
C1 O17 Ga2 112.5(2) . . ?
C1 O18 Ga1 113.1(2) . 2_656 ?
C2 O19 Ga2 113.0(2) . . ?
C2 O20 Ga1 114.4(2) . 2_656 ?
O17 C1 O18 127.3(3) . . ?
O17 C1 C2 116.2(3) . . ?
O18 C1 C2 116.4(3) . . ?
O19 C2 C1 116.5(3) . . ?
O20 C2 O19 127.2(3) . . ?
O20 C2 C1 116.3(3) . . ?
H3A C3 H3B 108.0 . . ?
C4 C3 H3A 109.3 . . ?
C4 C3 H3B 109.3 . . ?
N1 C3 H3A 109.3 . . ?
N1 C3 H3B 109.3 . . ?
N1 C3 C4 111.6(5) . . ?
C3 C4 H4A 109.3 . . ?
C3 C4 H4B 109.3 . . ?
C3 C4 C5 111.8(5) . . ?
H4A C4 H4B 107.9 . . ?
C5 C4 H4A 109.3 . . ?
C5 C4 H4B 109.3 . . ?
C4 C5 H5A 108.4 . . ?
C4 C5 H5B 108.4 . . ?
H5A C5 H5B 107.5 . . ?
C6 C5 C4 115.3(5) . . ?
C6 C5 H5A 108.4 . . ?
C6 C5 H5B 108.4 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
H6A C6 H6B 108.1 . . ?
N2 C6 C5 110.8(5) . . ?
N2 C6 H6A 109.5 . . ?
N2 C6 H6B 109.5 . . ?
C3 N1 H1A 109.5 . . ?
C3 N1 H1B 109.5 . . ?
C3 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?
C6 N2 H2A 109.5 . . ?
C6 N2 H2B 109.5 . . ?
C6 N2 H2C 109.5 . . ?
H2A N2 H2B 109.5 . . ?
H2A N2 H2C 109.5 . . ?
H2B N2 H2C 109.5 . . ?

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
Ga1 O18 C1 O17 176.9(3) 2_656 . . . ?
Ga1 O18 C1 C2 -2.9(4) 2_656 . . . ?
Ga1 O20 C2 O19 -177.0(3) 2_656 . . . ?
Ga1 O20 C2 C1 3.0(4) 2_656 . . . ?
Ga2 O17 C1 O18 -179.4(3) . . . . ?
Ga2 O17 C1 C2 0.4(4) . . . . ?
Ga2 O19 C2 O20 179.3(3) . . . . ?
Ga2 O19 C2 C1 -0.7(4) . . . . ?
P4 P4 O13 Ga2 -25.9(7) 3_767 . . . ?
P4 P4 O14 O15 -15.5(16) 3_767 . . 3_767 ?
P4 P4 O15 O14 3.9(4) 3_767 . . 3_767 ?
O1 P1 O3 Ga1 64.2(3) . . . 3_666 ?
O1 P1 O4 Ga1 -50.8(3) . . . 3_766 ?
O2 P1 O1 Ga1 4.7(5) . . . . ?
O2 P1 O3 Ga1 -55.6(3) . . . 3_666 ?
O2 P1 O4 Ga1 69.6(3) . . . 3_766 ?
O3 Ga1 O1 P1 81.5(4) 3_666 . . . ?
O3 P1 O1 Ga1 -116.8(4) . . . . ?
O3 P1 O4 Ga1 -171.3(2) . . . 3_766 ?
O4 Ga1 O1 P1 -96.8(4) 3_766 . . . ?
O4 P1 O1 Ga1 126.9(4) . . . . ?
O4 P1 O3 Ga1 -174.8(2) . . . 3_666 ?
O5 Ga1 O1 P1 -6.0(4) . . . . ?
O5 P2 O6 Ga2 -165.0(2) . . . . ?
O6 Ga2 O9 P3 -178.9(4) . . . . ?
O6 P2 O5 Ga1 -151.6(3) . . . . ?
O7 P2 O5 Ga1 -29.0(4) . . . . ?
O7 P2 O6 Ga2 74.1(3) . . . . ?
O8 P2 O5 Ga1 87.8(3) . . . . ?
O8 P2 O6 Ga2 -44.9(3) . . . . ?
O9 P3 O11 Ga2 -170.0(3) . . . 1_455 ?
O10 P3 O9 Ga2 -57.5(5) . . . . ?
O10 P3 O11 Ga2 73.1(3) . . . 1_455 ?
O11 P3 O9 Ga2 -172.0(4) . . . . ?
O12 P3 O9 Ga2 63.8(5) . . . . ?
O12 P3 O11 Ga2 -46.1(4) . . . 1_455 ?
O13 Ga2 O9 P3 85.0(4) . . . . ?
O13 P4 O14 P4 116.1(3) . . . 3_767 ?
O13 P4 O14 O15 100.6(18) . . . 3_767 ?
O13 P4 O15 O14 -115.4(5) . . . 3_767 ?
O14 P4 O13 Ga2 13.1(7) 3_767 . . . ?
O14 P4 O13 Ga2 -71.0(7) . . . . ?
O14 P4 O14 P4 -0.001(1) 3_767 . . 3_767 ?
O14 P4 O14 O15 -15.5(16) 3_767 . . 3_767 ?
O14 P4 O15 O14 7.1(7) . . . 3_767 ?
O15 P4 O13 Ga2 53.4(7) . . . . ?
O15 P4 O14 P4 -4.6(5) . . . 3_767 ?
O15 P4 O14 O15 -20(2) . . . 3_767 ?
O16 P4 O13 Ga2 164.7(5) . . . . ?
O16 P4 O14 P4 -121.8(3) . . . 3_767 ?
O16 P4 O14 O15 -137.3(17) . . . 3_767 ?
O16 P4 O15 O14 129.6(5) . . . 3_767 ?
O17 Ga2 O9 P3 -88.6(4) . . . . ?
O17 C1 C2 O19 0.1(5) . . . . ?
O17 C1 C2 O20 -179.9(3) . . . . ?
O18 Ga1 O1 P1 165.9(3) 2_646 . . . ?
O18 C1 C2 O19 180.0(3) . . . . ?
O18 C1 C2 O20 0.0(5) . . . . ?
O19 Ga2 O9 P3 -6.8(4) . . . . ?
O20 Ga1 O1 P1 173.5(4) 2_646 . . . ?
C3 C4 C5 C6 58.7(7) . . . . ?
C4 C5 C6 N2 171.0(4) . . . . ?
N1 C3 C4 C5 167.6(5) . . . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1
_database_code_depnum_ccdc_archive 'CCDC 1062255'
_audit_update_record             
;
2015-06-11 deposited with the CCDC.
2015-07-01 downloaded from the CCDC.
;
_audit_creation_date             2015-06-03
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C H3 In O10 P2, C2 H7 N'
_chemical_formula_sum            'C3 H10 In N O10 P2'
_chemical_formula_weight         396.88
_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 0.0033 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'
In In -0.7276 1.3100 '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                   7.6595(6)
_cell_length_b                   8.4550(4)
_cell_length_c                   9.6469(6)
_cell_angle_alpha                91.768(5)
_cell_angle_beta                 111.205(6)
_cell_angle_gamma                115.495(6)
_cell_volume                     512.64(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3941
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.0340
_cell_measurement_theta_min      3.9440
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    2.667
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66963
_exptl_absorpt_correction_type   multi-scan
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.571
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             388
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6283
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.367
_diffrn_reflns_theta_min         3.398
_diffrn_ambient_temperature      293
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9595
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
#__ type_ start__ end____ width___ exp.time_
  1 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000   90.0000 84

#__ type_ start__ end____ width___ exp.time_
  2 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  3 omega  -11.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   77.0000  -90.0000 94

#__ type_ start__ end____ width___ exp.time_
  4 omega  -52.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -57.0000 -180.0000 84

#__ type_ start__ end____ width___ exp.time_
  5 omega   -1.00   83.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694   57.0000    0.0000 84

#__ type_ start__ end____ width___ exp.time_
  6 omega   35.00   88.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  178.0000    0.0000 53

#__ type_ start__ end____ width___ exp.time_
  7 omega   35.00   72.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  178.0000 -180.0000 37

#__ type_ start__ end____ width___ exp.time_
  8 omega  -20.00   55.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       15.5694  -99.0000   30.0000 75
;
_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      -0.0443074000
_diffrn_orient_matrix_UB_12      0.0281177000
_diffrn_orient_matrix_UB_13      -0.0663521000
_diffrn_orient_matrix_UB_21      0.0679969000
_diffrn_orient_matrix_UB_22      0.0910515000
_diffrn_orient_matrix_UB_23      0.0397527000
_diffrn_orient_matrix_UB_31      0.0783388000
_diffrn_orient_matrix_UB_32      0.0019084000
_diffrn_orient_matrix_UB_33      -0.0236302000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1994
_reflns_number_total             2090
_reflns_odcompleteness_completeness 99.71
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_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_data_reduction        
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.33 (release 27-03-2014 CrysAlis171 .NET)
(compiled Mar 27 2014,17:12:48)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.101
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2090
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0246
_refine_ls_R_factor_gt           0.0232
_refine_ls_restrained_S_all      1.101
_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)+(0.0268P)²+0.3111P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0593
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C3(H3A,H3B)
2.b Idealised Me refined as rotating group:
 N1(H1A,H1B,H1C)
2.c Idealised tetrahedral OH refined as rotating group:
 O4(H4), O7(H7), O8(H8)
;
_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
In1 In 0.31418(3) 0.52882(3) 0.70205(2) 0.01314(9) Uani 1 1 d . . . . .
P1 P 0.20679(12) 0.76453(10) 0.43817(9) 0.01335(17) Uani 1 1 d . . . . .
P2 P 0.38903(14) 0.64715(11) 1.05605(9) 0.01832(18) Uani 1 1 d . . . . .
O1 O 0.2246(4) 0.7089(3) 0.5899(2) 0.0185(5) Uani 1 1 d . . . . .
O2 O 0.3867(3) 0.7792(3) 0.3983(2) 0.0177(5) Uani 1 1 d . . . . .
O3 O -0.0101(3) 0.6432(3) 0.3086(2) 0.0193(5) Uani 1 1 d . . . . .
O4 O 0.2195(4) 0.9567(3) 0.4588(3) 0.0196(5) Uani 1 1 d . . . . .
H4 H 0.3442 1.0339 0.5037 0.029 Uiso 1 1 calc GR . . . .
O5 O 0.4072(4) 0.6936(3) 0.9111(3) 0.0213(5) Uani 1 1 d . . . . .
O6 O 0.5800(4) 0.6404(3) 1.1701(3) 0.0212(5) Uani 1 1 d . . . . .
O7 O 0.3618(5) 0.7948(4) 1.1314(3) 0.0332(6) Uani 1 1 d . . . . .
H7 H 0.3687 0.7812 1.2167 0.050 Uiso 1 1 calc GR . . . .
O8 O 0.1866(4) 0.4619(3) 1.0207(3) 0.0347(6) Uani 1 1 d . . . . .
H8 H 0.1100 0.4321 0.9291 0.052 Uiso 1 1 calc GR . . . .
O9 O 0.6126(3) 0.6529(3) 0.6727(2) 0.0183(5) Uani 1 1 d . . . . .
O10 O 0.7536(3) 0.6398(3) 0.5106(3) 0.0192(5) Uani 1 1 d . . . . .
C1 C 0.6049(5) 0.5838(4) 0.5529(3) 0.0146(6) Uani 1 1 d . . . . .
C2 C 1.1087(6) 0.9215(5) 0.8772(4) 0.0226(7) Uani 1 1 d . . . . .
H2A H 1.2503 0.9596 0.9553 0.027 Uiso 1 1 calc R . . . .
H2B H 1.0246 0.7932 0.8652 0.027 Uiso 1 1 calc R . . . .
C3 C 1.0089(6) 1.0192(5) 0.9257(4) 0.0246(7) Uani 1 1 d . . . . .
H3A H 0.8684 0.9824 0.8465 0.030 Uiso 1 1 calc R . . . .
H3B H 1.0942 1.1475 0.9385 0.030 Uiso 1 1 calc R . . . .
N1 N 1.1217(5) 0.9595(4) 0.7303(3) 0.0234(6) Uani 1 1 d . . . . .
H1A H 0.9922 0.9279 0.6596 0.028 Uiso 1 1 calc GR . . . .
H1B H 1.1752 0.8969 0.7006 0.028 Uiso 1 1 calc GR . . . .
H1C H 1.2054 1.0763 0.7430 0.028 Uiso 1 1 calc GR . . . .


_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
In1 O1 2.103(2) . ?
In1 O3 2.110(2) 2_566 ?
In1 O5 2.109(2) . ?
In1 O6 2.147(2) 2_667 ?
In1 O9 2.197(2) . ?
In1 O10 2.219(2) 2_666 ?
P1 O1 1.528(2) . ?
P1 O2 1.517(2) . ?
P1 O3 1.525(2) . ?
P1 O4 1.588(2) . ?
P2 O5 1.502(2) . ?
P2 O6 1.505(2) . ?
P2 O7 1.552(2) . ?
P2 O8 1.571(3) . ?
O3 In1 2.110(2) 2_566 ?
O4 H4 0.8200 . ?
O6 In1 2.147(2) 2_667 ?
O7 H7 0.8200 . ?
O8 H8 0.8200 . ?
O9 C1 1.249(4) . ?
O10 In1 2.219(2) 2_666 ?
O10 C1 1.254(4) . ?
C1 C1 1.548(6) 2_666 ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C2 C3 1.505(5) . ?
C2 N1 1.492(4) . ?
C3 C3 1.521(6) 2_777 ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
N1 H1A 0.8900 . ?
N1 H1B 0.8900 . ?
N1 H1C 0.8900 . ?

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 In1 O3 95.04(9) . 2_566 ?
O1 In1 O5 88.39(9) . . ?
O1 In1 O6 176.14(8) . 2_667 ?
O1 In1 O9 89.77(8) . . ?
O1 In1 O10 94.16(8) . 2_666 ?
O3 In1 O6 86.71(9) 2_566 2_667 ?
O3 In1 O9 166.11(8) 2_566 . ?
O3 In1 O10 91.27(8) 2_566 2_666 ?
O5 In1 O3 92.97(9) . 2_566 ?
O5 In1 O6 88.08(9) . 2_667 ?
O5 In1 O9 100.20(9) . . ?
O5 In1 O10 174.85(8) . 2_666 ?
O6 In1 O9 89.31(8) 2_667 . ?
O6 In1 O10 89.24(9) 2_667 2_666 ?
O9 In1 O10 75.36(8) . 2_666 ?
O1 P1 O4 105.98(12) . . ?
O2 P1 O1 112.39(12) . . ?
O2 P1 O3 111.68(13) . . ?
O2 P1 O4 108.84(12) . . ?
O3 P1 O1 112.18(13) . . ?
O3 P1 O4 105.30(13) . . ?
O5 P2 O6 114.36(14) . . ?
O5 P2 O7 107.27(13) . . ?
O5 P2 O8 110.56(14) . . ?
O6 P2 O7 107.70(15) . . ?
O6 P2 O8 108.65(14) . . ?
O7 P2 O8 108.08(16) . . ?
P1 O1 In1 135.43(13) . . ?
P1 O3 In1 134.30(13) . 2_566 ?
P1 O4 H4 109.5 . . ?
P2 O5 In1 131.11(14) . . ?
P2 O6 In1 144.20(14) . 2_667 ?
P2 O7 H7 109.5 . . ?
P2 O8 H8 109.5 . . ?
C1 O9 In1 115.06(19) . . ?
C1 O10 In1 114.55(18) . 2_666 ?
O9 C1 O10 125.2(3) . . ?
O9 C1 C1 117.7(3) . 2_666 ?
O10 C1 C1 117.0(3) . 2_666 ?
H2A C2 H2B 108.1 . . ?
C3 C2 H2A 109.6 . . ?
C3 C2 H2B 109.6 . . ?
N1 C2 H2A 109.6 . . ?
N1 C2 H2B 109.6 . . ?
N1 C2 C3 110.3(3) . . ?
C2 C3 C3 111.4(4) . 2_777 ?
C2 C3 H3A 109.4 . . ?
C2 C3 H3B 109.4 . . ?
C3 C3 H3A 109.4 2_777 . ?
C3 C3 H3B 109.4 2_777 . ?
H3A C3 H3B 108.0 . . ?
C2 N1 H1A 109.5 . . ?
C2 N1 H1B 109.5 . . ?
C2 N1 H1C 109.5 . . ?
H1A N1 H1B 109.5 . . ?
H1A N1 H1C 109.5 . . ?
H1B N1 H1C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O4 H4 O2 0.82 1.83 2.644(3) 174.8 2_676
N1 H1A O10 0.89 2.32 2.917(4) 124.3 .
N1 H1B O1 0.89 2.12 2.996(3) 165.9 1_655
N1 H1C O6 0.89 2.15 3.024(4) 166.3 2_777

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
In1 O9 C1 O10 176.2(2) . . . . ?
In1 O9 C1 C1 -3.6(4) . . . 2_666 ?
In1 O10 C1 O9 176.4(2) 2_666 . . . ?
In1 O10 C1 C1 -3.9(4) 2_666 . . 2_666 ?
O1 P1 O3 In1 21.9(2) . . . 2_566 ?
O2 P1 O1 In1 -39.1(2) . . . . ?
O2 P1 O3 In1 149.10(17) . . . 2_566 ?
O3 P1 O1 In1 87.8(2) . . . . ?
O4 P1 O1 In1 -157.84(17) . . . . ?
O4 P1 O3 In1 -92.93(19) . . . 2_566 ?
O5 P2 O6 In1 -120.6(2) . . . 2_667 ?
O6 P2 O5 In1 91.8(2) . . . . ?
O7 P2 O5 In1 -148.86(19) . . . . ?
O7 P2 O6 In1 120.3(2) . . . 2_667 ?
O8 P2 O5 In1 -31.2(2) . . . . ?
O8 P2 O6 In1 3.5(3) . . . 2_667 ?
N1 C2 C3 C3 179.2(4) . . . 2_777 ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
