# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_jli58_-3m1_corabs
_database_code_depnum_ccdc_archive 'CCDC 1469966'
_audit_update_record             
;
2016-03-21 deposited with the CCDC.
2016-07-01 downloaded from the CCDC.
;

_audit_creation_date             2015-06-10T13:26:46-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
 ?
;
_chemical_formula_sum            'H6 Mn5 O18 P6'
_chemical_formula_weight         754.57

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_H-M   'P -3 c 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'y, x, -z+1/2'
'x-y, -y, -z+1/2'
'-x, -x+y, -z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-y, -x, z-1/2'
'-x+y, y, z-1/2'
'x, x-y, z-1/2'

_cell_length_a                   10.37640(10)
_cell_length_b                   10.37640(10)
_cell_length_c                   9.40170(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_volume                     876.658(15)
_cell_formula_units_Z            2
_cell_measurement_temperature    100(2)
_cell_measurement_reflns_used    3545
_cell_measurement_theta_min      2.259
_cell_measurement_theta_max      27.95

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.0995
_exptl_crystal_size_mid          0.0706
_exptl_crystal_size_min          0.0377
_exptl_crystal_density_diffrn    2.859
_exptl_crystal_density_method    flotation
_exptl_crystal_density_meas      3.041(5)
_exptl_crystal_F_000             730
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 5 -12 0.0394
-8 12 7 0.0269
0 -5 12 0.0312
-11 -1 -5 0.0246
-9 -5 -2 0.0313
-14 5 3 0.0164
-15 8 -2 0.0131
-1 -7 -10 0.0579
0 13 0 0.0345
14 -4 -4 0.0197
1 -13 -4 0.0566
15 -7 0 0.0229
-1 6 12 0.0364
-13 1 1 0.0155
-8 -6 4 0.0364
14 -11 1 0.0405
-13 1 -2 0.0161
-14 10 -1 0.0183

_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.14
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
Analytical numeric absorption correction using a multifaceted crystal
                        model based on expressions derived by R.C. Clark & J.S.
        (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_correction_T_min  0.774
_exptl_absorpt_correction_T_max  0.899

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_ambient_temperature      100(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            Eos
_diffrn_detector_area_resol_mean 16.2439
_diffrn_orient_matrix_ub_11      -0.0712247
_diffrn_orient_matrix_ub_12      -0.0103609
_diffrn_orient_matrix_ub_13      0.0167364
_diffrn_orient_matrix_ub_21      -0.0013324
_diffrn_orient_matrix_ub_22      0.0324039
_diffrn_orient_matrix_ub_23      -0.0660294
_diffrn_orient_matrix_ub_31      -0.0339731
_diffrn_orient_matrix_ub_32      -0.0712111
_diffrn_orient_matrix_ub_33      -0.0324694
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_av_unetI/netI     0.0109
_diffrn_reflns_number            5399
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_theta_min         2.27
_diffrn_reflns_theta_max         25.65
_diffrn_reflns_theta_full        25.65
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_reflns_number_total             562
_reflns_number_gt                552
_reflns_threshold_expression     >2sigma(I)

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_cell_refinement       
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction        
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
        (compiled Aug 13 2014,18:06:01)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          SQUEEZE

# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material

loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 -0.043 55 39 'Li+ and H3O+ cations'
_platon_squeeze_details          
; ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0372P)²+17.4760P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    refall
_refine_ls_extinction_method     none
_refine_ls_number_reflns         562
_refine_ls_number_parameters     49
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0508
_refine_ls_R_factor_gt           0.0502
_refine_ls_wR_factor_ref         0.1238
_refine_ls_wR_factor_gt          0.1235
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_restrained_S_all      1.156
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         3.257
_refine_diff_density_min         -0.657
_refine_diff_density_rms         0.185

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.006 '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'
Mn Mn 0.3368 0.7283 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Mn1 Mn 0.37918(16) 0.37918(16) 0.75 0.0174(4) Uani 1 2 d S . .
Mn2 Mn 0.3333 0.6667 0.66508(17) 0.0104(4) Uani 1 3 d S . .
P1 P 0.5893(2) 0.7011(2) 0.91290(16) 0.0136(5) Uani 1 1 d . . .
O1 O 0.4587(6) 0.6076(6) 0.8135(5) 0.0164(10) Uani 1 1 d . . .
O2 O 0.1718(6) 0.3113(6) 0.8567(5) 0.0275(13) Uani 1 1 d . . .
O3 O 0.3065(5) 0.4638(5) 0.5666(4) 0.0153(10) Uani 1 1 d . . .
H1 H 0.666(8) 0.638(8) 0.911(7) 0.009(18) Uiso 1 1 d . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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 O2 2.149(6) . ?
Mn1 O2 2.149(6) 4_556 ?
Mn1 O1 2.168(5) . ?
Mn1 O1 2.168(5) 4_556 ?
Mn1 O3 2.230(4) 4_556 ?
Mn1 O3 2.230(4) . ?
Mn2 O3 2.186(5) 3_565 ?
Mn2 O3 2.186(5) 2_665 ?
Mn2 O3 2.186(5) . ?
Mn2 O1 2.194(5) . ?
Mn2 O1 2.194(5) 2_665 ?
Mn2 O1 2.194(5) 3_565 ?
P1 O1 1.528(5) . ?
P1 O3 1.535(4) 10_666 ?
P1 O2 1.540(6) 2_665 ?
P1 H1 1.26(7) . ?
O2 P1 1.540(6) 3_565 ?
O3 P1 1.535(4) 10_665 ?

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
O2 Mn1 O2 96.7(3) . 4_556 ?
O2 Mn1 O1 90.0(2) . . ?
O2 Mn1 O1 168.10(19) 4_556 . ?
O2 Mn1 O1 168.10(19) . 4_556 ?
O2 Mn1 O1 90.0(2) 4_556 4_556 ?
O1 Mn1 O1 85.1(3) . 4_556 ?
O2 Mn1 O3 91.57(19) . 4_556 ?
O2 Mn1 O3 90.5(2) 4_556 4_556 ?
O1 Mn1 O3 99.08(17) . 4_556 ?
O1 Mn1 O3 78.54(17) 4_556 4_556 ?
O2 Mn1 O3 90.5(2) . . ?
O2 Mn1 O3 91.57(19) 4_556 . ?
O1 Mn1 O3 78.54(17) . . ?
O1 Mn1 O3 99.08(17) 4_556 . ?
O3 Mn1 O3 176.8(3) 4_556 . ?
O3 Mn2 O3 103.36(14) 3_565 2_665 ?
O3 Mn2 O3 103.36(14) 3_565 . ?
O3 Mn2 O3 103.36(14) 2_665 . ?
O3 Mn2 O1 162.71(18) 3_565 . ?
O3 Mn2 O1 92.57(18) 2_665 . ?
O3 Mn2 O1 78.96(17) . . ?
O3 Mn2 O1 92.57(18) 3_565 2_665 ?
O3 Mn2 O1 78.96(17) 2_665 2_665 ?
O3 Mn2 O1 162.71(18) . 2_665 ?
O1 Mn2 O1 83.84(18) . 2_665 ?
O3 Mn2 O1 78.96(17) 3_565 3_565 ?
O3 Mn2 O1 162.71(18) 2_665 3_565 ?
O3 Mn2 O1 92.57(18) . 3_565 ?
O1 Mn2 O1 83.84(18) . 3_565 ?
O1 Mn2 O1 83.84(18) 2_665 3_565 ?
O1 P1 O3 111.2(3) . 10_666 ?
O1 P1 O2 112.1(3) . 2_665 ?
O3 P1 O2 114.1(3) 10_666 2_665 ?
O1 P1 H1 105(3) . . ?
O3 P1 H1 107(3) 10_666 . ?
O2 P1 H1 107(3) 2_665 . ?
P1 O1 Mn1 126.4(3) . . ?
P1 O1 Mn2 132.3(3) . . ?
Mn1 O1 Mn2 100.09(19) . . ?
P1 O2 Mn1 127.9(3) 3_565 . ?
P1 O3 Mn2 134.7(3) 10_665 . ?
P1 O3 Mn1 123.6(3) 10_665 . ?
Mn2 O3 Mn1 98.42(18) . . ?

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
O3 P1 O1 Mn1 -94.5(4) 10_666 . . . ?
O2 P1 O1 Mn1 136.5(3) 2_665 . . . ?
O3 P1 O1 Mn2 100.2(4) 10_666 . . . ?
O2 P1 O1 Mn2 -28.9(5) 2_665 . . . ?
O2 Mn1 O1 P1 115.6(4) . . . . ?
O2 Mn1 O1 P1 -119.6(9) 4_556 . . . ?
O1 Mn1 O1 P1 -53.6(3) 4_556 . . . ?
O3 Mn1 O1 P1 24.0(4) 4_556 . . . ?
O3 Mn1 O1 P1 -153.9(4) . . . . ?
O2 Mn1 O1 Mn2 -75.4(2) . . . . ?
O2 Mn1 O1 Mn2 49.5(11) 4_556 . . . ?
O1 Mn1 O1 Mn2 115.5(2) 4_556 . . . ?
O3 Mn1 O1 Mn2 -167.00(18) 4_556 . . . ?
O3 Mn1 O1 Mn2 15.13(18) . . . . ?
O3 Mn2 O1 P1 -107.9(6) 3_565 . . . ?
O3 Mn2 O1 P1 49.5(4) 2_665 . . . ?
O3 Mn2 O1 P1 152.6(4) . . . . ?
O1 Mn2 O1 P1 -29.1(4) 2_665 . . . ?
O1 Mn2 O1 P1 -113.5(3) 3_565 . . . ?
O3 Mn2 O1 Mn1 84.1(6) 3_565 . . . ?
O3 Mn2 O1 Mn1 -118.5(2) 2_665 . . . ?
O3 Mn2 O1 Mn1 -15.42(18) . . . . ?
O1 Mn2 O1 Mn1 162.9(2) 2_665 . . . ?
O1 Mn2 O1 Mn1 78.4(3) 3_565 . . . ?
O2 Mn1 O2 P1 -156.6(5) 4_556 . . 3_565 ?
O1 Mn1 O2 P1 13.6(4) . . . 3_565 ?
O1 Mn1 O2 P1 79.1(11) 4_556 . . 3_565 ?
O3 Mn1 O2 P1 112.7(4) 4_556 . . 3_565 ?
O3 Mn1 O2 P1 -65.0(4) . . . 3_565 ?
O3 Mn2 O3 P1 53.5(4) 3_565 . . 10_665 ?
O3 Mn2 O3 P1 -54.0(4) 2_665 . . 10_665 ?
O1 Mn2 O3 P1 -144.0(4) . . . 10_665 ?
O1 Mn2 O3 P1 -149.8(5) 2_665 . . 10_665 ?
O1 Mn2 O3 P1 132.8(4) 3_565 . . 10_665 ?
O3 Mn2 O3 Mn1 -147.6(2) 3_565 . . . ?
O3 Mn2 O3 Mn1 104.9(3) 2_665 . . . ?
O1 Mn2 O3 Mn1 14.91(18) . . . . ?
O1 Mn2 O3 Mn1 9.2(7) 2_665 . . . ?
O1 Mn2 O3 Mn1 -68.30(19) 3_565 . . . ?
O2 Mn1 O3 P1 -123.0(3) . . . 10_665 ?
O2 Mn1 O3 P1 -26.3(4) 4_556 . . 10_665 ?
O1 Mn1 O3 P1 147.0(4) . . . 10_665 ?
O1 Mn1 O3 P1 64.0(4) 4_556 . . 10_665 ?
O3 Mn1 O3 P1 105.3(3) 4_556 . . 10_665 ?
O2 Mn1 O3 Mn2 74.8(2) . . . . ?
O2 Mn1 O3 Mn2 171.6(2) 4_556 . . . ?
O1 Mn1 O3 Mn2 -15.11(18) . . . . ?
O1 Mn1 O3 Mn2 -98.14(19) 4_556 . . . ?
O3 Mn1 O3 Mn2 -56.81(14) 4_556 . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
_exptl_crystal_recrystallization_method 'Hydrothermal synthesis'
