# Electronic Supplementary Material (ESI) for CrystEngComm.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_LiHDTMP_anhydrous_publ
_database_code_depnum_ccdc_archive 'CCDC 1584815'
_audit_update_record             
;
2018-06-14 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_pd_block_id                     
2018-05-29T10:20|LiHDTMP_anhydrous|LiHDTMP_anhydrous|X'PERT

_audit_creation_method           'from EXP file using GSAS2CIF'
_audit_creation_date             2018-05-29T10:20

#=============================================================================
# 5. OVERALL REFINEMENT & COMPUTING DETAILS

_refine_special_details          
; ?
;
_pd_proc_ls_special_details      
; ?
;

# The following items are used to identify the programs used.
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_ls_weighting_scheme      ?
_refine_ls_weighting_details     ?
_refine_ls_hydrogen_treatment    ?
_refine_ls_extinction_method     ?
_refine_ls_extinction_coef       ?
_refine_ls_number_constraints    ?

_refine_ls_restrained_S_all      ?
_refine_ls_restrained_S_obs      ?

#==============================================================================
# 6. SAMPLE PREPARATION DATA

# (In the unusual case where multiple samples are used in a single
#  Rietveld study, this information should be moved into the phase
#  blocks)

# The following three fields describe the preparation of the material.
# The cooling rate is in K/min.  The pressure at which the sample was
# prepared is in kPa.  The temperature of preparation is in K.

_pd_prep_cool_rate               ?
_pd_prep_pressure                ?
_pd_prep_temperature             ?

_pd_char_colour                  ? # use ICDD colour descriptions
_refine_ls_shift/su_max          0.10
_refine_ls_shift/su_mean         0.02
_computing_structure_refinement  GSAS
_refine_ls_number_parameters     94
_refine_ls_goodness_of_fit_all   12.37
_refine_ls_number_restraints     33
_refine_ls_matrix_type           full
#==============================================================================
# 7. CHEMICAL, STRUCTURAL AND CRYSTAL DATA

_pd_char_particle_morphology     ?

_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_formula_moiety         ?

# If you change Z, be sure to change all 3 of the following
_chemical_formula_sum            'C5 Li N O6 P2'
_chemical_compound_source        ? # for minerals and
_chemical_formula_structural     ?
_chemical_formula_analytical     ?
_chemical_melting_point          ?

_diffrn_ambient_temperature      298
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
_chemical_absolute_configuration ?
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +x,+y,+z
-1 -x,-y,-z

_exptl_crystal_F_000             ?
_exptl_crystal_density_diffrn    ?
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?

_cell_measurement_temperature    298

_cell_special_details            
; ?
;

_geom_special_details            ?

# The following item identifies the program(s) used (if appropriate).
_computing_structure_solution    ?

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

# 8. Phase information from GSAS

_pd_phase_name                   LiHDTMP_anhydrous
_cell_length_a                   5.9014(4)
_cell_length_b                   9.2693(7)
_cell_length_c                   9.5123(7)
_cell_angle_alpha                85.902(4)
_cell_angle_beta                 77.676(5)
_cell_angle_gamma                85.588(6)
_cell_volume                     506.04(8)

# ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS


loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_thermal_displace_type
_atom_site_U_iso_or_equiv
_atom_site_symmetry_multiplicity
P P1 0.6220(16) 0.2214(9) 0.0511(9) 1.0 Uiso 0.0349(33) 2
P P2 0.8420(15) 0.6226(9) 0.3200(11) 1.0 Uiso 0.0396(32) 2
O O1 0.6806(29) 0.3448(17) -0.0608(16) 1.0 Uiso 0.0334(21) 2
O O2 0.4333(25) 0.1348(15) 0.0195(16) 1.0 Uiso 0.0334(21) 2
O O3 0.8276(28) 0.1121(17) 0.0643(18) 1.0 Uiso 0.0334(21) 2
O O4 0.6848(27) 0.6155(15) 0.4689(16) 1.0 Uiso 0.0334(21) 2
O O5 0.1018(24) 0.5696(15) 0.3231(19) 1.0 Uiso 0.0334(21) 2
O O6 0.8287(29) 0.7722(17) 0.2398(16) 1.0 Uiso 0.0334(21) 2
N N1 0.666(4) 0.3573(18) 0.2960(22) 1.0 Uiso 0.0334(21) 2
Li Li1 0.793(8) 0.921(5) 0.068(5) 1.0 Uiso 0.03 2
C C1 0.493(4) 0.2737(25) 0.2383(21) 1.0 Uiso 0.0334(21) 2
C C2 0.732(4) 0.4935(20) 0.2102(20) 1.0 Uiso 0.0334(21) 2
C C3 0.854(4) 0.2585(23) 0.3356(29) 1.0 Uiso 0.0334(21) 2
C C4 0.800(4) 0.1254(22) 0.4382(27) 1.0 Uiso 0.0334(21) 2
C C5 0.045(4) 0.0605(22) 0.4481(26) 1.0 Uiso 0.0334(21) 2
_chemical_formula_weight         238.95
_cell_formula_units_Z            2

# MOLECULAR GEOMETRY

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.514(16) . 1_555 N
P1 O2 1.513(15) . 1_555 N
P1 O3 1.540(15) . 1_555 N
P1 Li1 2.90(5) . 1_545 N
P1 C1 1.864(16) . 1_555 N
P2 O4 1.519(16) . 1_555 N
P2 O5 1.579(14) . 1_655 N
P2 O6 1.540(16) . 1_555 N
P2 C2 1.878(13) . 1_555 N
O1 P1 1.514(16) . 1_555 N
O2 P1 1.513(15) . 1_555 N
O2 Li1 1.84(4) . -1_665 N
O3 P1 1.540(15) . 1_555 N
O3 Li1 1.80(5) . 1_545 N
O3 Li1 2.33(5) . -1_765 N
O4 P2 1.519(16) . 1_555 N
O5 P2 1.579(14) . 1_455 N
O6 P2 1.540(16) . 1_555 N
O6 Li1 2.09(5) . 1_555 N
N1 C1 1.534(19) . 1_555 N
N1 C2 1.485(14) . 1_555 N
N1 C3 1.478(21) . 1_555 N
Li1 P1 2.90(5) . 1_565 N
Li1 O2 1.84(4) . -1_665 N
Li1 O3 1.80(5) . 1_565 N
Li1 O3 2.33(5) . -1_765 N
Li1 O6 2.09(5) . 1_555 N
Li1 Li1 2.95(10) . -1_775 N
C1 P1 1.864(16) . 1_555 N
C1 N1 1.534(19) . 1_555 N
C2 P2 1.878(13) . 1_555 N
C2 N1 1.485(14) . 1_555 N
C3 N1 1.478(21) . 1_555 N
C3 C4 1.527(24) . 1_555 N
C4 C3 1.527(24) . 1_555 N
C4 C5 1.544(24) . 1_655 N
C4 C5 2.212(32) . -1_656 N
C5 C4 1.544(24) . 1_455 N
C5 C4 2.212(32) . -1_656 N
C5 C5 1.492(15) . -1_556 N

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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 P1 O2 111.4(11) 1_555 . 1_555 N
O1 P1 O3 114.7(12) 1_555 . 1_555 N
O1 P1 C1 116.2(10) 1_555 . 1_555 N
O2 P1 O3 106.4(11) 1_555 . 1_555 N
O2 P1 C1 101.5(9) 1_555 . 1_555 N
O3 P1 C1 105.5(12) 1_555 . 1_555 N
O4 P2 O5 112.4(12) 1_555 . 1_655 N
O4 P2 O6 113.3(10) 1_555 . 1_555 N
O4 P2 C2 106.6(10) 1_555 . 1_555 N
O5 P2 O6 111.2(11) 1_655 . 1_555 N
O5 P2 C2 106.9(10) 1_655 . 1_555 N
O6 P2 C2 105.8(10) 1_555 . 1_555 N
P1 O2 Li1 160.3(21) 1_555 . -1_665 N
P1 O3 Li1 120.2(18) 1_555 . 1_545 N
P1 O3 Li1 133.8(16) 1_555 . -1_765 N
Li1 O3 Li1 90.4(23) 1_545 . -1_765 N
P2 O6 Li1 156.8(19) 1_555 . 1_555 N
C1 N1 C2 114.0(17) 1_555 . 1_555 N
C1 N1 C3 111.0(18) 1_555 . 1_555 N
C2 N1 C3 117.7(19) 1_555 . 1_555 N
O2 Li1 O3 116.4(27) -1_665 . 1_565 N
O2 Li1 O3 115.2(23) -1_665 . -1_765 N
O2 Li1 O6 109.4(27) -1_665 . 1_555 N
O2 Li1 Li1 127.4(30) -1_665 . -1_775 N
O3 Li1 O3 89.6(23) 1_565 . -1_765 N
O3 Li1 O6 125.1(25) 1_565 . 1_555 N
O3 Li1 Li1 52.1(17) 1_565 . -1_775 N
O3 Li1 O6 97.1(20) -1_765 . 1_555 N
O3 Li1 Li1 37.5(11) -1_765 . -1_775 N
O6 Li1 Li1 116.6(27) 1_555 . -1_775 N
P1 C1 N1 110.3(15) 1_555 . 1_555 N
P2 C2 N1 111.3(13) 1_555 . 1_555 N
N1 C3 C4 121.3(20) 1_555 . 1_555 N
C3 C4 C5 102.2(17) 1_555 . 1_655 N
C4 C5 C5 93.5(22) 1_455 . -1_556 N

# Powder diffraction data for histogram  1
#==============================================================================
# 9. INSTRUMENT CHARACTERIZATION

_exptl_special_details           
; ?
;

# if regions of the data are excluded, the reason(s) are supplied here:
_pd_proc_info_excluded_regions   
; ?
;

# The following item is used to identify the equipment used to record
# the powder pattern when the diffractogram was measured at a laboratory
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
; ?
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
; ?
;
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           ?
_diffrn_radiation_wavelength     0.18972
_diffrn_source                   synchrotron
_diffrn_source_type              ?
_diffrn_source_target            ?
_diffrn_measurement_device_type  synchrotron
_diffrn_detector                 ?
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             ? # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following two items identify the program(s) used (if appropriate).
_computing_data_collection       ?
_computing_data_reduction        ?

# Describe any processing performed on the data, prior to refinement.
# For example: a manual Lp correction or a precomputed absorption correction
_pd_proc_info_data_reduction     ?

# The following item is used for angular dispersive measurements only.

_diffrn_radiation_monochromator  ?

# The following items are used to define the size of the instrument.
# Not all distances are appropriate for all instrument types.

_pd_instr_dist_src/mono          ?
_pd_instr_dist_mono/spec         ?
_pd_instr_dist_src/spec          ?
_pd_instr_dist_spec/anal         ?
_pd_instr_dist_anal/detc         ?
_pd_instr_dist_spec/detc         ?

# 10. Specimen size and mounting information

# The next three fields give the specimen dimensions in mm.  The equatorial
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              ? # perpendicular to
# equatorial plane

_pd_spec_size_equat              ? # parallel to
# scattering vector
# in transmission

_pd_spec_size_thick              ? # parallel to
# scattering vector
# in reflection

_pd_spec_mounting                
# This field should be
# used to give details of the
# container.
; ?
;

_pd_spec_mount_mode              ? # options are 'reflection'
# or 'transmission'

_pd_spec_shape                   ? # options are 'cylinder'
# 'flat_sheet' or 'irregular'


loop_
_atom_type_symbol
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
P 4.0 0.000 0.000 6.43450 1.90670 4.17910 27.1570 1.78000 0.52600 1.49080
68.1645 1.11490 International_Tables_Vol_C
O 12.0 0.000 0.000 3.04850 13.2771 2.28680 5.70110 1.54630 0.32390 0.86700
32.9089 0.25080 International_Tables_Vol_C
N 2.0 0.000 0.000 12.2126 0.00570 3.13220 9.89330 2.01250 28.9975 1.16630
0.58260 -11.529 International_Tables_Vol_C
Li 2.0 0.000 0.000 1.12820 3.95460 0.75080 1.05240 0.61750 85.3905 0.46530
168.261 0.03770 International_Tables_Vol_C
C 10.0 0.000 0.000 2.31000 20.8439 1.02000 10.2075 1.58860 0.56870 0.86500
51.6512 0.21560 International_Tables_Vol_C
_diffrn_radiation_polarisn_ratio ?
_pd_proc_ls_prof_R_factor        0.0103
_pd_proc_ls_prof_wR_factor       0.0115
_pd_proc_ls_prof_wR_expected     0.0010
_refine_ls_R_Fsqd_factor         0.06962

_pd_proc_ls_background_function  
;   GSAS Background function number 7 with 36 terms.
 Linear interpolation
      1:    171967.     2:    145646.     3:    139408.     4:    187026.    
      5:    243999.     6:    220297.     7:    165809.     8:    132401.    
      9:    110613.    10:    98685.0    11:    89802.6    12:    87353.9    
     13:    77731.6    14:    72230.4    15:    66414.5    16:    63740.3    
     17:    62387.3    18:    63425.7    19:    66335.8    20:    67575.1    
     21:    67519.1    22:    65806.0    23:    62748.4    24:    60879.5    
     25:    56137.9    26:    52671.1    27:    49803.5    28:    47961.5    
     29:    46100.2    30:    44866.4    31:    43668.1    32:    42698.3    
     33:    41938.2    34:    41978.2    35:    41770.3    36:    41878.2    
;

_exptl_absorpt_process_details   
;   GSAS Absorption/surface roughness correction: function number 0
 No correction is applied.
;
_exptl_absorpt_correction_T_min  1.00000
_exptl_absorpt_correction_T_max  1.00000
_pd_proc_ls_pref_orient_corr     
;   March-Dollase
 AXIS  1 Ratio=   1.02304  h= 0.000  k= 0.000  l= 1.000
 Prefered orientation correction range: Min=   0.93396, Max=   1.03475
;

_pd_proc_ls_profile_function     
;
 CW Profile function number 3 with  19 terms
 Pseudovoigt profile coefficients as parameterized in
 P. Thompson, D.E. Cox & J.B. Hastings (1987). J. Appl. Cryst.,20,79-83.
 Asymmetry correction of L.W. Finger, D.E. Cox & A. P. Jephcoat (1994).
 J. Appl. Cryst.,27,892-900.
 #1(GU)   =    0.000 #2(GV)   =    0.000 #3(GW)   =    0.639
 #4(GP)   =    0.000 #5(LX)   =    0.000 #6(LY)   =   36.237
 #7(S/L)  =   0.0005 #8(H/L)  =   0.0013
 #9(trns) =     0.00 #10(shft)=   0.0000
 #11(stec)=     0.00 #12(ptec)=     0.00 #13(sfec)=     0.00
 #14(L11) =    0.000 #15(L22) =    0.000 #16(L33) =    0.000
 #17(L12) =    0.000 #18(L13) =    0.000 #19(L23) =    0.000
 Peak tails are ignored  where the intensity is below 0.0080 times the peak
   Aniso. broadening axis   0.0   0.0   1.0
;
_pd_proc_ls_peak_cutoff          0.00800
_pd_proc_info_datetime           2018-05-29T10:20:09
_pd_calc_method                  'Rietveld Refinement'

#---- raw/calc data loop -----
_pd_meas_2theta_range_min        0.187
_pd_meas_2theta_range_max        19.195
_pd_meas_2theta_range_inc        0.009
_pd_proc_2theta_range_min        0.18692
_pd_proc_2theta_range_max        19.19492
_pd_proc_2theta_range_inc        0.009


_reflns_number_total             2021
_reflns_limit_h_min              0
_reflns_limit_h_max              7
_reflns_limit_k_min              -11
_reflns_limit_k_max              11
_reflns_limit_l_min              -11
_reflns_limit_l_max              12
_reflns_d_resolution_high        0.807
_reflns_d_resolution_low         9.278

#--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--eof--#
####################################################################### 
# 
# 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_K-HDTMP
_database_code_depnum_ccdc_archive 'CCDC 1584817'
_audit_update_record             
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H42 K2 N2 O20 P4'
_chemical_formula_weight         712.53

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'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

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

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

_cell_length_a                   7.71780(10)
_cell_length_b                   33.0373(4)
_cell_length_c                   11.75770(10)
_cell_angle_alpha                90
_cell_angle_beta                 103.7090(10)
_cell_angle_gamma                90
_cell_volume                     2912.52(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9355
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      30.42

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.625
_exptl_crystal_F_000             1496
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_exptl_absorpt_coefficient_mu    0.628
_shelx_estimated_absorpt_T_min   0.744
_shelx_estimated_absorpt_T_max   0.969
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6695
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            70179
_diffrn_reflns_av_unetI/netI     0.0264
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_k_max       47
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.886
_diffrn_reflns_theta_max         30.509
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             8877
_reflns_number_gt                7448
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0325P)²+1.4230P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         8877
_refine_ls_number_parameters     409
_refine_ls_number_restraints     22
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0287
_refine_ls_wR_factor_ref         0.0714
_refine_ls_wR_factor_gt          0.0666
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_restrained_S_all      1.035
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.26379(4) 0.24401(2) 0.57726(2) 0.01215(6) Uani 1 1 d . . . . .
K2 K -0.16289(4) 0.26463(2) 0.65841(3) 0.01410(6) Uani 1 1 d . . . . .
P1 P 0.05483(4) 0.33420(2) 0.43847(3) 0.00737(6) Uani 1 1 d . . . . .
P2 P -0.36194(4) 0.41517(2) 0.59431(3) 0.00783(7) Uani 1 1 d . . . . .
P3 P 0.50011(4) 0.66415(2) 1.08548(3) 0.00852(7) Uani 1 1 d . . . . .
P4 P 0.89747(4) 0.58788(2) 0.90601(3) 0.00783(7) Uani 1 1 d . . . . .
O1 O 0.22322(12) 0.31762(3) 0.41227(8) 0.01059(18) Uani 1 1 d . . . . .
O2 O -0.05350(13) 0.30579(3) 0.49285(8) 0.01275(19) Uani 1 1 d . . . . .
O3 O -0.06777(12) 0.35331(3) 0.32498(8) 0.01104(18) Uani 1 1 d D . . . .
H3O H -0.011(2) 0.3606(5) 0.2797(14) 0.017 Uiso 1 1 d D U . . .
O4 O -0.36011(13) 0.38041(3) 0.67736(8) 0.01294(19) Uani 1 1 d . . . . .
O5 O -0.52313(12) 0.41082(3) 0.48599(8) 0.01264(19) Uani 1 1 d D . . . .
H5O H -0.582(2) 0.4306(5) 0.4590(16) 0.019 Uiso 1 1 d D U . . .
O6 O -0.34939(13) 0.45674(3) 0.64610(8) 0.01258(19) Uani 1 1 d . . . . .
O7 O 0.56936(13) 0.63427(3) 1.19026(8) 0.01324(19) Uani 1 1 d D . . . .
H7O H 0.498(2) 0.6283(6) 1.2269(15) 0.020 Uiso 1 1 d D U . . .
O8 O 0.34024(13) 0.68725(3) 1.10219(8) 0.0148(2) Uani 1 1 d . . . . .
O9 O 0.65755(13) 0.68737(3) 1.06555(8) 0.01447(19) Uani 1 1 d . . . . .
O10 O 0.90480(12) 0.62482(3) 0.83226(8) 0.01211(18) Uani 1 1 d . . . . .
O11 O 1.06005(12) 0.58873(3) 1.01486(8) 0.01173(18) Uani 1 1 d D . . . .
H11O H 1.101(2) 0.5681(5) 1.0441(15) 0.018 Uiso 1 1 d D U . . .
O12 O 0.87758(13) 0.54772(3) 0.84509(8) 0.01321(19) Uani 1 1 d . . . . .
O13 O 0.17605(13) 0.25458(3) 0.78268(9) 0.01323(19) Uani 1 1 d D . . . .
H13A H 0.236(2) 0.2723(5) 0.8245(15) 0.020 Uiso 1 1 d D U . . .
H13B H 0.193(2) 0.2331(5) 0.8143(16) 0.020 Uiso 1 1 d D U . . .
O14 O -0.03081(14) 0.19881(3) 0.56310(9) 0.0176(2) Uani 1 1 d D . . . .
H14A H 0.004(3) 0.1768(5) 0.5933(17) 0.026 Uiso 1 1 d D U . . .
H14B H -0.120(2) 0.1940(6) 0.5103(15) 0.026 Uiso 1 1 d D U . . .
O15 O 0.41516(13) 0.18076(3) 0.73577(8) 0.01284(19) Uani 1 1 d D . . . .
H15A H 0.501(2) 0.1948(5) 0.7678(15) 0.019 Uiso 1 1 d D U . . .
H15B H 0.359(2) 0.1766(6) 0.7826(14) 0.019 Uiso 1 1 d D U . . .
O16 O -0.31660(13) 0.23323(3) 0.82708(9) 0.01424(19) Uani 1 1 d D . . . .
H16A H -0.334(2) 0.2559(5) 0.8513(16) 0.021 Uiso 1 1 d D U . . .
H16B H -0.244(2) 0.2220(5) 0.8801(15) 0.021 Uiso 1 1 d D U . . .
O17 O -0.47565(14) 0.30366(3) 0.58536(9) 0.0170(2) Uani 1 1 d D . . . .
H17A H -0.443(3) 0.3250(5) 0.6172(16) 0.026 Uiso 1 1 d D U . . .
H17B H -0.553(2) 0.3109(6) 0.5274(15) 0.026 Uiso 1 1 d D U . . .
O18 O -0.03085(14) 0.33388(3) 0.78593(9) 0.0157(2) Uani 1 1 d D . . . .
H18A H 0.056(2) 0.3276(6) 0.8367(15) 0.024 Uiso 1 1 d D U . . .
H18B H -0.107(2) 0.3386(6) 0.8182(16) 0.024 Uiso 1 1 d D U . . .
O19 O 0.22905(14) 0.52833(3) 0.11816(9) 0.0162(2) Uani 1 1 d D . . . .
H19A H 0.187(2) 0.5063(5) 0.1218(17) 0.024 Uiso 1 1 d D U . . .
H19B H 0.275(2) 0.5345(6) 0.1871(13) 0.024 Uiso 1 1 d D U . . .
O20 O 0.73776(14) 0.96581(3) 0.11150(9) 0.0152(2) Uani 1 1 d D . . . .
H20A H 0.706(2) 0.9895(5) 0.1146(17) 0.023 Uiso 1 1 d D U . . .
H20B H 0.784(2) 0.9603(6) 0.1803(13) 0.023 Uiso 1 1 d D U . . .
N1 N -0.01192(14) 0.38944(3) 0.60579(9) 0.00753(19) Uani 1 1 d D . . . .
H1N H -0.035(2) 0.3686(4) 0.6433(14) 0.011 Uiso 1 1 d D U . . .
N2 N 0.55154(14) 0.61546(3) 0.89700(9) 0.00784(19) Uani 1 1 d D . . . .
H2N H 0.586(2) 0.6360(4) 0.8637(14) 0.012 Uiso 1 1 d D U . . .
C1 C 0.12407(16) 0.37615(4) 0.54085(11) 0.0102(2) Uani 1 1 d . . . . .
H1A H 0.2317 0.3682 0.5976 0.012 Uiso 1 1 calc R U . . .
H1B H 0.1537 0.3991 0.4977 0.012 Uiso 1 1 calc R U . . .
C2 C -0.17885(16) 0.40479(4) 0.52483(10) 0.0087(2) Uani 1 1 d . . . . .
H2A H -0.2187 0.3850 0.4633 0.010 Uiso 1 1 calc R U . . .
H2B H -0.1508 0.4295 0.4882 0.010 Uiso 1 1 calc R U . . .
C3 C 0.41640(16) 0.63151(4) 0.95874(11) 0.0107(2) Uani 1 1 d . . . . .
H3A H 0.3564 0.6086 0.9842 0.013 Uiso 1 1 calc R U . . .
H3B H 0.3275 0.6465 0.9024 0.013 Uiso 1 1 calc R U . . .
C4 C 0.71315(16) 0.59713(4) 0.97655(11) 0.0088(2) Uani 1 1 d . . . . .
H4A H 0.6795 0.5717 1.0064 0.011 Uiso 1 1 calc R U . . .
H4B H 0.7545 0.6150 1.0428 0.011 Uiso 1 1 calc R U . . .
C5 C 0.06842(16) 0.41903(4) 0.70278(10) 0.0087(2) Uani 1 1 d . . . . .
H5A H -0.0171 0.4236 0.7500 0.010 Uiso 1 1 calc R U . . .
H5B H 0.1732 0.4067 0.7528 0.010 Uiso 1 1 calc R U . . .
C6 C 0.12149(17) 0.45972(4) 0.66165(11) 0.0112(2) Uani 1 1 d . . . . .
H6A H 0.0156 0.4751 0.6259 0.013 Uiso 1 1 calc R U . . .
H6B H 0.1906 0.4558 0.6035 0.013 Uiso 1 1 calc R U . . .
C7 C 0.23264(17) 0.48292(4) 0.76679(11) 0.0114(2) Uani 1 1 d . . . . .
H7A H 0.1639 0.4858 0.8255 0.014 Uiso 1 1 calc R U . . .
H7B H 0.3389 0.4674 0.8011 0.014 Uiso 1 1 calc R U . . .
C8 C 0.28734(18) 0.52463(4) 0.73313(11) 0.0118(2) Uani 1 1 d . . . . .
H8A H 0.1811 0.5405 0.7018 0.014 Uiso 1 1 calc R U . . .
H8B H 0.3518 0.5218 0.6720 0.014 Uiso 1 1 calc R U . . .
C9 C 0.40462(17) 0.54708(4) 0.83694(11) 0.0109(2) Uani 1 1 d . . . . .
H9A H 0.3389 0.5512 0.8968 0.013 Uiso 1 1 calc R U . . .
H9B H 0.5092 0.5309 0.8704 0.013 Uiso 1 1 calc R U . . .
C10 C 0.46196(17) 0.58774(4) 0.79807(10) 0.0093(2) Uani 1 1 d . . . . .
H10A H 0.5434 0.5831 0.7480 0.011 Uiso 1 1 calc R U . . .
H10B H 0.3577 0.6014 0.7515 0.011 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
K1 O9 2.6782(10) 2_646 ?
K1 O13 2.6813(10) . ?
K1 O14 2.6922(11) . ?
K1 O17 2.8012(11) 1_655 ?
K1 O15 2.8588(11) . ?
K1 O1 3.0801(10) . ?
K1 O2 3.1615(10) . ?
K1 O13 3.3682(10) 4_565 ?
K1 P1 3.5909(4) . ?
K1 K2 3.7024(4) . ?
K1 K2 4.3533(4) 1_655 ?
K2 O2 2.6702(10) . ?
K2 O17 2.6915(11) . ?
K2 O13 2.6974(10) . ?
K2 O16 2.7444(11) . ?
K2 O14 2.7504(11) . ?
K2 O18 2.7922(11) . ?
K2 K1 4.3533(4) 1_455 ?
P1 O2 1.4974(10) . ?
P1 O1 1.5079(9) . ?
P1 O3 1.5735(10) . ?
P1 C1 1.8305(13) . ?
P2 O6 1.4961(10) . ?
P2 O4 1.5054(10) . ?
P2 O5 1.5619(10) . ?
P2 C2 1.8246(13) . ?
P3 O9 1.5016(10) . ?
P3 O8 1.5027(10) . ?
P3 O7 1.5702(10) . ?
P3 C3 1.8288(13) . ?
P4 O12 1.4984(10) . ?
P4 O10 1.5059(10) . ?
P4 O11 1.5659(10) . ?
P4 C4 1.8341(13) . ?
O9 K1 2.6782(10) 2_656 ?
O13 K1 3.3683(10) 4_566 ?
O17 K1 2.8011(11) 1_455 ?
N1 C2 1.4973(15) . ?
N1 C1 1.5023(16) . ?
N1 C5 1.5184(15) . ?
N2 C4 1.4982(15) . ?
N2 C3 1.5016(16) . ?
N2 C10 1.5128(15) . ?
C5 C6 1.5175(18) . ?
C6 C7 1.5326(17) . ?
C7 C8 1.5208(19) . ?
C8 C9 1.5284(17) . ?
C9 C10 1.5182(18) . ?

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
O9 K1 O13 143.03(3) 2_646 . ?
O9 K1 O14 83.53(3) 2_646 . ?
O13 K1 O14 74.82(3) . . ?
O9 K1 O17 104.20(3) 2_646 1_655 ?
O13 K1 O17 102.14(3) . 1_655 ?
O14 K1 O17 168.92(3) . 1_655 ?
O9 K1 O15 77.27(3) 2_646 . ?
O13 K1 O15 70.09(3) . . ?
O14 K1 O15 81.00(3) . . ?
O17 K1 O15 108.24(3) 1_655 . ?
O9 K1 O1 99.27(3) 2_646 . ?
O13 K1 O1 117.05(3) . . ?
O14 K1 O1 116.15(3) . . ?
O17 K1 O1 55.31(3) 1_655 . ?
O15 K1 O1 162.27(3) . . ?
O9 K1 O2 121.87(3) 2_646 . ?
O13 K1 O2 81.75(3) . . ?
O14 K1 O2 76.04(3) . . ?
O17 K1 O2 93.03(3) 1_655 . ?
O15 K1 O2 147.46(3) . . ?
O1 K1 O2 48.47(2) . . ?
O9 K1 O13 52.06(3) 2_646 4_565 ?
O13 K1 O13 153.17(4) . 4_565 ?
O14 K1 O13 89.03(3) . 4_565 ?
O17 K1 O13 89.60(3) 1_655 4_565 ?
O15 K1 O13 129.19(3) . 4_565 ?
O1 K1 O13 51.38(2) . 4_565 ?
O2 K1 O13 73.52(2) . 4_565 ?
O9 K1 P1 116.04(2) 2_646 . ?
O13 K1 P1 96.84(2) . . ?
O14 K1 P1 98.65(2) . . ?
O17 K1 P1 70.92(2) 1_655 . ?
O15 K1 P1 166.63(2) . . ?
O1 K1 P1 24.632(17) . . ?
O2 K1 P1 24.582(17) . . ?
O13 K1 P1 64.028(19) 4_565 . ?
O9 K1 K2 129.62(2) 2_646 . ?
O13 K1 K2 46.68(2) . . ?
O14 K1 K2 47.80(2) . . ?
O17 K1 K2 122.48(2) 1_655 . ?
O15 K1 K2 102.56(2) . . ?
O1 K1 K2 93.048(19) . . ?
O2 K1 K2 44.933(18) . . ?
O13 K1 K2 106.74(2) 4_565 . ?
P1 K1 K2 68.490(9) . . ?
O9 K1 K2 82.94(2) 2_646 1_655 ?
O13 K1 K2 104.05(2) . 1_655 ?
O14 K1 K2 154.15(3) . 1_655 ?
O17 K1 K2 36.70(2) 1_655 1_655 ?
O15 K1 K2 74.60(2) . 1_655 ?
O1 K1 K2 87.756(18) . 1_655 ?
O2 K1 K2 129.733(19) . 1_655 ?
O13 K1 K2 99.754(19) 4_565 1_655 ?
P1 K1 K2 107.066(9) . 1_655 ?
K2 K1 K2 146.578(12) . 1_655 ?
O2 K2 O17 86.44(3) . . ?
O2 K2 O13 91.37(3) . . ?
O17 K2 O13 155.93(3) . . ?
O2 K2 O16 170.00(3) . . ?
O17 K2 O16 84.44(3) . . ?
O13 K2 O16 95.27(3) . . ?
O2 K2 O14 83.91(3) . . ?
O17 K2 O14 129.77(3) . . ?
O13 K2 O14 73.62(3) . . ?
O16 K2 O14 105.13(3) . . ?
O2 K2 O18 80.56(3) . . ?
O17 K2 O18 87.96(3) . . ?
O13 K2 O18 68.05(3) . . ?
O16 K2 O18 94.98(3) . . ?
O14 K2 O18 138.01(3) . . ?
O2 K2 K1 56.75(2) . . ?
O17 K2 K1 142.29(3) . . ?
O13 K2 K1 46.32(2) . . ?
O16 K2 K1 132.84(2) . . ?
O14 K2 K1 46.48(2) . . ?
O18 K2 K1 93.18(2) . . ?
O2 K2 K1 113.61(2) . 1_455 ?
O17 K2 K1 38.46(2) . 1_455 ?
O13 K2 K1 154.72(2) . 1_455 ?
O16 K2 K1 60.54(2) . 1_455 ?
O14 K2 K1 104.04(2) . 1_455 ?
O18 K2 K1 117.94(2) . 1_455 ?
K1 K2 K1 146.578(11) . 1_455 ?
O2 P1 O1 117.06(6) . . ?
O2 P1 O3 109.22(5) . . ?
O1 P1 O3 110.29(5) . . ?
O2 P1 C1 107.42(6) . . ?
O1 P1 C1 106.14(5) . . ?
O3 P1 C1 106.09(6) . . ?
O2 P1 K1 61.44(4) . . ?
O1 P1 K1 58.36(4) . . ?
O3 P1 K1 146.44(4) . . ?
C1 P1 K1 107.44(4) . . ?
O6 P2 O4 116.53(6) . . ?
O6 P2 O5 112.24(6) . . ?
O4 P2 O5 110.00(6) . . ?
O6 P2 C2 111.87(6) . . ?
O4 P2 C2 104.94(6) . . ?
O5 P2 C2 99.75(5) . . ?
O9 P3 O8 118.74(6) . . ?
O9 P3 O7 107.82(6) . . ?
O8 P3 O7 110.73(6) . . ?
O9 P3 C3 108.46(6) . . ?
O8 P3 C3 105.28(6) . . ?
O7 P3 C3 104.92(6) . . ?
O12 P4 O10 117.12(6) . . ?
O12 P4 O11 112.22(6) . . ?
O10 P4 O11 108.89(5) . . ?
O12 P4 C4 111.17(6) . . ?
O10 P4 C4 105.33(6) . . ?
O11 P4 C4 100.63(5) . . ?
P1 O1 K1 97.01(4) . . ?
P1 O2 K2 159.31(6) . . ?
P1 O2 K1 93.98(4) . . ?
K2 O2 K1 78.32(3) . . ?
P3 O9 K1 140.07(6) . 2_656 ?
K1 O13 K2 87.00(3) . . ?
K1 O13 K1 153.62(4) . 4_566 ?
K2 O13 K1 119.22(3) . 4_566 ?
K1 O14 K2 85.72(3) . . ?
K2 O17 K1 104.84(4) . 1_455 ?
C2 N1 C1 112.05(9) . . ?
C2 N1 C5 113.33(10) . . ?
C1 N1 C5 111.08(9) . . ?
C4 N2 C3 114.32(9) . . ?
C4 N2 C10 113.35(10) . . ?
C3 N2 C10 110.01(9) . . ?
N1 C1 P1 115.16(8) . . ?
N1 C2 P2 114.84(8) . . ?
N2 C3 P3 116.77(8) . . ?
N2 C4 P4 113.90(8) . . ?
C6 C5 N1 115.09(10) . . ?
C5 C6 C7 109.13(10) . . ?
C8 C7 C6 112.34(11) . . ?
C7 C8 C9 112.35(11) . . ?
C10 C9 C8 110.41(10) . . ?
N2 C10 C9 114.64(10) . . ?

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
C5 H5B O7 0.97 2.37 3.2910(16) 159.4 3_667
C4 H4B O9 0.97 2.54 3.2219(16) 127.6 .
C4 H4B O7 0.97 2.57 3.2207(16) 124.2 .
C3 H3A O11 0.97 2.49 3.2949(16) 140.6 1_455
C2 H2A O3 0.97 2.45 3.1787(16) 131.8 .
C1 H1B O5 0.97 2.56 3.1582(16) 120.0 1_655
C1 H1A O7 0.97 2.60 3.4881(16) 151.9 3_667
N2 H2N O15 0.854(13) 1.886(14) 2.7105(15) 161.8(16) 2_656
N2 H2N O10 0.854(13) 2.602(16) 3.0153(14) 111.0(13) .
N1 H1N O18 0.860(13) 2.025(14) 2.8325(15) 156.1(15) .
O20 H20B O12 0.823(14) 1.919(15) 2.7391(14) 174(2) 4_575
O20 H20A O6 0.825(14) 1.883(15) 2.7008(14) 171.2(19) 4_675
O19 H19B O6 0.829(15) 1.931(15) 2.7511(14) 170(2) 3_566
O19 H19A O12 0.802(15) 1.917(15) 2.7101(14) 170(2) 3_666
O18 H18A O9 0.814(14) 2.288(15) 3.0754(15) 162.9(18) 3_667
O17 H17B O1 0.829(15) 1.937(15) 2.7411(13) 163.5(19) 1_455
O16 H16B O2 0.822(14) 1.959(15) 2.7763(14) 173.0(19) 4_566
O15 H15B O1 0.790(14) 2.053(15) 2.8215(13) 164.3(19) 4_566
O13 H13A O9 0.833(14) 1.901(15) 2.7249(14) 170.1(18) 3_667
O11 H11O O19 0.795(14) 1.747(14) 2.5314(14) 168.8(19) 1_656
O7 H7O O4 0.797(14) 1.749(14) 2.5411(13) 172(2) 3_567
O5 H5O O20 0.817(14) 1.735(14) 2.5413(14) 169.0(19) 2_545
O3 H3O O10 0.804(14) 1.773(14) 2.5738(13) 173.9(18) 3_666

_refine_diff_density_max         0.527
_refine_diff_density_min         -0.331
_refine_diff_density_rms         0.068

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Li-HDTMP
_database_code_depnum_ccdc_archive 'CCDC 1584820'
_audit_update_record             
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H34 Li2 N2 O16 P4'
_chemical_formula_weight         576.15

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   5.9728(6)
_cell_length_b                   9.4557(9)
_cell_length_c                   11.0182(11)
_cell_angle_alpha                74.418(7)
_cell_angle_beta                 76.170(7)
_cell_angle_gamma                84.313(7)
_cell_volume                     581.62(10)
_cell_formula_units_Z            1
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    1719
_cell_measurement_theta_min      2.58
_cell_measurement_theta_max      24.64

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_F_000             302
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.040
_exptl_absorpt_coefficient_mu    0.402
_shelx_estimated_absorpt_T_min   0.917
_shelx_estimated_absorpt_T_max   0.984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.9167
_exptl_absorpt_correction_T_max  0.9841
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'fine-focus sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            10054
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_theta_min         1.968
_diffrn_reflns_theta_max         26.569
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             2408
_reflns_number_gt                1693
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1018P)²+0.0500P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         2408
_refine_ls_number_parameters     175
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0903
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_ref         0.1596
_refine_ls_wR_factor_gt          0.1399
_refine_ls_goodness_of_fit_ref   0.985
_refine_ls_restrained_S_all      0.984
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.60640(16) 0.30309(10) 0.10071(9) 0.0190(3) Uani 1 1 d . . . . .
P2 P 0.83435(16) 0.65387(10) 0.35544(9) 0.0197(3) Uani 1 1 d . . . . .
O1 O 0.7942(4) 0.4145(3) 0.0147(3) 0.0255(6) Uani 1 1 d D . . . .
H1O H 0.732(7) 0.497(3) -0.004(4) 0.031 Uiso 1 1 d D U . . .
O2 O 0.3924(4) 0.3244(3) 0.0476(3) 0.0270(6) Uani 1 1 d . . . . .
O3 O 0.7186(4) 0.1542(3) 0.1251(3) 0.0261(6) Uani 1 1 d . . . . .
O4 O 0.7265(4) 0.5743(3) 0.4917(2) 0.0238(6) Uani 1 1 d . . . . .
O5 O 1.1051(4) 0.6265(3) 0.3341(3) 0.0270(6) Uani 1 1 d D . . . .
H5O H 1.151(8) 0.561(4) 0.389(3) 0.032 Uiso 1 1 d D U . . .
O6 O 0.7832(5) 0.8123(3) 0.3098(3) 0.0348(7) Uani 1 1 d . . . . .
O7 O 0.8241(5) 0.8855(3) 0.0052(3) 0.0320(7) Uani 1 1 d D . . . .
H7A H 0.758(7) 0.825(4) -0.012(4) 0.038 Uiso 1 1 d D U . . .
H7B H 0.964(4) 0.866(5) -0.017(4) 0.038 Uiso 1 1 d D U . . .
O8 O 0.3552(6) 0.9011(4) 0.1852(4) 0.0460(9) Uani 1 1 d D . . . .
H8A H 0.277(8) 0.951(5) 0.134(4) 0.055 Uiso 1 1 d D U . . .
H8B H 0.294(8) 0.822(3) 0.217(5) 0.055 Uiso 1 1 d D U . . .
N1 N 0.6663(5) 0.4103(3) 0.3141(3) 0.0176(6) Uani 1 1 d D . . . .
H1N H 0.592(6) 0.421(4) 0.389(2) 0.021 Uiso 1 1 d D U . . .
Li1 Li 0.6738(13) 0.9436(7) 0.1696(6) 0.0294(15) Uani 1 1 d . . . . .
C1 C 0.5025(6) 0.3594(4) 0.2515(3) 0.0199(8) Uani 1 1 d . . . . .
H1A H 0.3874 0.4380 0.2363 0.024 Uiso 1 1 calc R U . . .
H1B H 0.4229 0.2771 0.3148 0.024 Uiso 1 1 calc R U . . .
C2 C 0.7403(7) 0.5648(4) 0.2488(4) 0.0227(8) Uani 1 1 d . . . . .
H2A H 0.6125 0.6223 0.2175 0.027 Uiso 1 1 calc R U . . .
H2B H 0.8658 0.5633 0.1747 0.027 Uiso 1 1 calc R U . . .
C3 C 0.8711(6) 0.3073(4) 0.3317(4) 0.0223(8) Uani 1 1 d . . . . .
H3A H 0.9771 0.3530 0.3627 0.027 Uiso 1 1 calc R U . . .
H3B H 0.9506 0.2911 0.2486 0.027 Uiso 1 1 calc R U . . .
C4 C 0.8070(7) 0.1610(4) 0.4252(4) 0.0285(9) Uani 1 1 d . . . . .
H4A H 0.7196 0.1078 0.3892 0.034 Uiso 1 1 calc R U . . .
H4B H 0.7111 0.1761 0.5055 0.034 Uiso 1 1 calc R U . . .
C5 C 1.0239(7) 0.0723(4) 0.4511(4) 0.0287(9) Uani 1 1 d . . . . .
H5A H 1.1152 0.0546 0.3707 0.034 Uiso 1 1 calc R U . . .
H5B H 1.1146 0.1295 0.4816 0.034 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O3 1.483(3) . ?
P1 O2 1.503(3) . ?
P1 O1 1.567(3) . ?
P1 C1 1.829(4) . ?
P2 O6 1.473(3) . ?
P2 O4 1.504(3) . ?
P2 O5 1.583(3) . ?
P2 C2 1.829(4) . ?
O1 H1O 0.827(19) . ?
O3 Li1 1.948(7) 1_545 ?
O5 H5O 0.819(19) . ?
O6 Li1 1.909(7) . ?
O7 Li1 2.012(7) . ?
O7 H7A 0.815(19) . ?
O7 H7B 0.828(19) . ?
O8 Li1 1.942(8) . ?
O8 H8A 0.831(19) . ?
O8 H8B 0.81(2) . ?
N1 C1 1.502(4) . ?
N1 C2 1.503(4) . ?
N1 C3 1.503(4) . ?
N1 H1N 0.861(18) . ?
Li1 O3 1.949(7) 1_565 ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.507(5) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.515(5) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C5 1.500(7) 2_756 ?
C5 H5A 0.9700 . ?
C5 H5B 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
O3 P1 O2 117.98(16) . . ?
O3 P1 O1 107.99(15) . . ?
O2 P1 O1 111.50(16) . . ?
O3 P1 C1 110.71(16) . . ?
O2 P1 C1 101.89(16) . . ?
O1 P1 C1 106.08(16) . . ?
O6 P2 O4 119.34(16) . . ?
O6 P2 O5 108.85(17) . . ?
O4 P2 O5 108.21(14) . . ?
O6 P2 C2 106.45(17) . . ?
O4 P2 C2 106.80(16) . . ?
O5 P2 C2 106.49(17) . . ?
P1 O1 H1O 109(3) . . ?
P1 O3 Li1 145.9(3) . 1_545 ?
P2 O5 H5O 116(3) . . ?
P2 O6 Li1 138.4(3) . . ?
Li1 O7 H7A 116(3) . . ?
Li1 O7 H7B 125(3) . . ?
H7A O7 H7B 106(4) . . ?
Li1 O8 H8A 122(4) . . ?
Li1 O8 H8B 127(4) . . ?
H8A O8 H8B 107(5) . . ?
C1 N1 C2 113.1(3) . . ?
C1 N1 C3 114.0(3) . . ?
C2 N1 C3 111.1(3) . . ?
C1 N1 H1N 109(3) . . ?
C2 N1 H1N 100(3) . . ?
C3 N1 H1N 109(2) . . ?
O6 Li1 O8 108.4(4) . . ?
O6 Li1 O3 121.5(4) . 1_565 ?
O8 Li1 O3 111.7(3) . 1_565 ?
O6 Li1 O7 109.0(3) . . ?
O8 Li1 O7 100.3(3) . . ?
O3 Li1 O7 103.6(3) 1_565 . ?
N1 C1 P1 121.0(2) . . ?
N1 C1 H1A 107.1 . . ?
P1 C1 H1A 107.1 . . ?
N1 C1 H1B 107.1 . . ?
P1 C1 H1B 107.1 . . ?
H1A C1 H1B 106.8 . . ?
N1 C2 P2 113.1(2) . . ?
N1 C2 H2A 109.0 . . ?
P2 C2 H2A 109.0 . . ?
N1 C2 H2B 109.0 . . ?
P2 C2 H2B 109.0 . . ?
H2A C2 H2B 107.8 . . ?
N1 C3 C4 113.1(3) . . ?
N1 C3 H3A 109.0 . . ?
C4 C3 H3A 109.0 . . ?
N1 C3 H3B 109.0 . . ?
C4 C3 H3B 109.0 . . ?
H3A C3 H3B 107.8 . . ?
C3 C4 C5 109.6(3) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 C5 C4 113.3(4) 2_756 . ?
C5 C5 H5A 108.9 2_756 . ?
C4 C5 H5A 108.9 . . ?
C5 C5 H5B 108.9 2_756 . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.7 . . ?

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
O2 P1 O3 Li1 -29.0(5) . . . 1_545 ?
O1 P1 O3 Li1 -156.5(4) . . . 1_545 ?
C1 P1 O3 Li1 87.7(5) . . . 1_545 ?
O4 P2 O6 Li1 -126.8(4) . . . . ?
O5 P2 O6 Li1 108.4(4) . . . . ?
C2 P2 O6 Li1 -6.0(5) . . . . ?
C2 N1 C1 P1 77.2(3) . . . . ?
C3 N1 C1 P1 -51.0(4) . . . . ?
O3 P1 C1 N1 76.6(3) . . . . ?
O2 P1 C1 N1 -157.0(3) . . . . ?
O1 P1 C1 N1 -40.3(3) . . . . ?
C1 N1 C2 P2 156.1(2) . . . . ?
C3 N1 C2 P2 -74.3(3) . . . . ?
O6 P2 C2 N1 -150.7(3) . . . . ?
O4 P2 C2 N1 -22.2(3) . . . . ?
O5 P2 C2 N1 93.2(3) . . . . ?
C1 N1 C3 C4 -65.5(4) . . . . ?
C2 N1 C3 C4 165.4(3) . . . . ?
N1 C3 C4 C5 -172.3(3) . . . . ?
C3 C4 C5 C5 177.0(4) . . . 2_756 ?

_refine_diff_density_max         0.853
_refine_diff_density_min         -0.755
_refine_diff_density_rms         0.116

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Na-HDTMP
_database_code_depnum_ccdc_archive 'CCDC 1584819'
_audit_update_record             
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H48 N2 Na2 O23 P4'
_chemical_formula_weight         734.36

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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 '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'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   7.66820(10)
_cell_length_b                   11.53350(10)
_cell_length_c                   18.0768(2)
_cell_angle_alpha                97.3780(10)
_cell_angle_beta                 94.7920(10)
_cell_angle_gamma                101.7050(10)
_cell_volume                     1542.61(3)
_cell_formula_units_Z            2
_cell_measurement_temperature    296(2)
_cell_measurement_reflns_used    9940
_cell_measurement_theta_min      2.29
_cell_measurement_theta_max      29.95

_exptl_crystal_description       plate
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.581
_exptl_crystal_F_000             776
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.025
_exptl_absorpt_coefficient_mu    0.363
_shelx_estimated_absorpt_T_min   0.854
_shelx_estimated_absorpt_T_max   0.991
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6899
_exptl_absorpt_correction_T_max  0.7462
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      296(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'sealed tube'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            74089
_diffrn_reflns_av_unetI/netI     0.0371
_diffrn_reflns_av_R_equivalents  0.0590
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_theta_min         1.824
_diffrn_reflns_theta_max         31.028
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measured_fraction_theta_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_point_group_measured_fraction_full 0.999
_reflns_number_total             9784
_reflns_number_gt                7728
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0404P)²+1.1108P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         9784
_refine_ls_number_parameters     457
_refine_ls_number_restraints     28
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0368
_refine_ls_wR_factor_ref         0.0981
_refine_ls_wR_factor_gt          0.0905
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_restrained_S_all      1.052
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Na1 Na 0.0000 0.0000 1.0000 0.0162(2) Uani 1 2 d S . P . .
Na2 Na -0.36336(8) -0.03213(6) 1.07122(4) 0.01232(13) Uani 1 1 d . . . . .
Na3 Na 1.0000 0.5000 1.0000 0.01305(18) Uani 1 2 d S . P . .
P1 P 0.56533(5) 0.43674(3) 0.20636(2) 0.00898(8) Uani 1 1 d . . . . .
P2 P 0.14120(5) 0.60557(3) 0.33826(2) 0.00876(8) Uani 1 1 d . . . . .
P3 P -0.05114(5) 0.04699(3) 0.81549(2) 0.00835(8) Uani 1 1 d . . . . .
P4 P 0.35806(5) -0.10337(3) 0.65714(2) 0.00837(8) Uani 1 1 d . . . . .
O1 O 0.67237(15) 0.35278(10) 0.17087(6) 0.0113(2) Uani 1 1 d . . . . .
O2 O 0.43714(15) 0.48014(11) 0.15482(7) 0.0143(2) Uani 1 1 d . . . . .
O3 O 0.69031(15) 0.54642(11) 0.25723(7) 0.0154(2) Uani 1 1 d D . . . .
H3O H 0.793(2) 0.544(2) 0.2587(13) 0.023 Uiso 1 1 d D U . . .
O4 O 0.01769(15) 0.55288(10) 0.26725(6) 0.0134(2) Uani 1 1 d . . . . .
O5 O 0.22646(16) 0.73925(10) 0.33473(7) 0.0128(2) Uani 1 1 d D . . . .
H5O H 0.241(3) 0.7877(18) 0.3722(10) 0.019 Uiso 1 1 d D U . . .
O6 O 0.06662(15) 0.58827(10) 0.41107(7) 0.0134(2) Uani 1 1 d . . . . .
O7 O 0.07278(15) -0.00296(10) 0.86523(6) 0.0124(2) Uani 1 1 d . . . . .
O8 O -0.17472(15) -0.06180(10) 0.76139(7) 0.0122(2) Uani 1 1 d D . . . .
H8O H -0.271(2) -0.052(2) 0.7462(12) 0.018 Uiso 1 1 d D U . . .
O9 O -0.15933(15) 0.12824(10) 0.85249(6) 0.0118(2) Uani 1 1 d . . . . .
O10 O 0.50192(14) -0.05571(10) 0.72189(6) 0.0127(2) Uani 1 1 d . . . . .
O11 O 0.27482(15) -0.23837(10) 0.65882(7) 0.0125(2) Uani 1 1 d D . . . .
H11O H 0.258(3) -0.2842(18) 0.6205(10) 0.019 Uiso 1 1 d D U . . .
O12 O 0.40766(15) -0.08058(10) 0.58137(6) 0.0132(2) Uani 1 1 d . . . . .
O13 O 0.26233(16) 0.14485(11) 1.02851(7) 0.0144(2) Uani 1 1 d D . . . .
H13A H 0.321(3) 0.136(2) 1.0655(10) 0.022 Uiso 1 1 d D U . . .
H13B H 0.246(3) 0.2140(15) 1.0339(13) 0.022 Uiso 1 1 d D U . . .
O14 O -0.27810(19) 0.10979(11) 0.98941(7) 0.0197(3) Uani 1 1 d D . . . .
H14A H -0.249(3) 0.111(2) 0.9468(10) 0.030 Uiso 1 1 d D U . . .
H14B H -0.272(3) 0.1808(15) 1.0045(13) 0.030 Uiso 1 1 d D U . . .
O15 O -0.48060(15) -0.15581(11) 1.15855(7) 0.0129(2) Uani 1 1 d D . . . .
H15A H -0.475(3) -0.2191(15) 1.1373(12) 0.019 Uiso 1 1 d D U . . .
H15B H -0.583(2) -0.157(2) 1.1646(12) 0.019 Uiso 1 1 d D U . . .
O16 O 0.72902(17) 0.35786(11) 1.02285(7) 0.0164(2) Uani 1 1 d D . . . .
H16A H 0.712(3) 0.357(2) 1.0661(9) 0.025 Uiso 1 1 d D U . . .
H16B H 0.635(2) 0.363(2) 0.9990(12) 0.025 Uiso 1 1 d D U . . .
O17 O 1.00987(19) 0.37995(12) 0.88274(7) 0.0208(3) Uani 1 1 d D . . . .
H17A H 0.950(3) 0.3118(16) 0.8761(14) 0.031 Uiso 1 1 d D U . . .
H17B H 0.984(3) 0.396(2) 0.8403(10) 0.031 Uiso 1 1 d D U . . .
O18 O 0.84162(17) 0.63592(11) 0.94538(7) 0.0157(2) Uani 1 1 d D . . . .
H18A H 0.758(3) 0.5978(19) 0.9167(12) 0.024 Uiso 1 1 d D U . . .
H18B H 0.909(3) 0.661(2) 0.9146(11) 0.024 Uiso 1 1 d D U . . .
O19 O 0.00404(16) 0.72312(11) 0.82346(7) 0.0157(2) Uani 1 1 d D . . . .
H19A H 0.094(2) 0.701(2) 0.8160(13) 0.024 Uiso 1 1 d D U . . .
H19B H 0.028(3) 0.7944(14) 0.8328(13) 0.024 Uiso 1 1 d D U . . .
O20 O 0.20539(17) 0.58694(11) 0.55368(7) 0.0162(2) Uani 1 1 d D . . . .
H20A H 0.136(3) 0.5322(18) 0.5655(13) 0.024 Uiso 1 1 d D U . . .
H20B H 0.173(3) 0.595(2) 0.5108(10) 0.024 Uiso 1 1 d D U . . .
O21 O 0.28898(16) 0.91717(11) 0.43714(7) 0.0159(2) Uani 1 1 d D . . . .
H21A H 0.312(3) 0.907(2) 0.4809(10) 0.024 Uiso 1 1 d D U . . .
H21B H 0.372(3) 0.9678(18) 0.4290(13) 0.024 Uiso 1 1 d D U . . .
O22 O 0.58032(17) 0.64441(11) 0.07457(8) 0.0177(2) Uani 1 1 d D . . . .
H22A H 0.684(2) 0.641(2) 0.0667(13) 0.027 Uiso 1 1 d D U . . .
H22B H 0.548(3) 0.5897(18) 0.0990(12) 0.027 Uiso 1 1 d D U . . .
O23 O -0.47485(16) 0.11764(11) 1.13699(7) 0.0136(2) Uani 1 1 d D . . . .
H23A H -0.480(3) 0.100(2) 1.1798(9) 0.020 Uiso 1 1 d D U . . .
H23B H -0.423(3) 0.1873(15) 1.1457(12) 0.020 Uiso 1 1 d D U . . .
N1 N 0.27878(17) 0.40608(11) 0.29525(7) 0.0088(2) Uani 1 1 d D . . . .
H1 H 0.206(2) 0.3992(19) 0.2560(10) 0.013 Uiso 1 1 d D U . . .
N2 N 0.22400(17) 0.08946(11) 0.71926(7) 0.0083(2) Uani 1 1 d D . . . .
H2 H 0.303(2) 0.0936(18) 0.7557(10) 0.012 Uiso 1 1 d D U . . .
C1 C 0.4325(2) 0.35490(14) 0.26959(9) 0.0121(3) Uani 1 1 d . . . . .
H1A H 0.3854 0.2735 0.2447 0.015 Uiso 1 1 calc R U . . .
H1B H 0.5115 0.3509 0.3136 0.015 Uiso 1 1 calc R U . . .
C2 C 0.33294(19) 0.53642(13) 0.32708(9) 0.0100(3) Uani 1 1 d . . . . .
H2A H 0.4088 0.5781 0.2942 0.012 Uiso 1 1 calc R U . . .
H2B H 0.4027 0.5453 0.3756 0.012 Uiso 1 1 calc R U . . .
C3 C 0.0756(2) 0.13693(14) 0.75345(9) 0.0101(3) Uani 1 1 d . . . . .
H3A H -0.0082 0.1475 0.7129 0.012 Uiso 1 1 calc R U . . .
H3B H 0.1269 0.2156 0.7817 0.012 Uiso 1 1 calc R U . . .
C4 C 0.17010(19) -0.03893(13) 0.68389(9) 0.0095(3) Uani 1 1 d . . . . .
H4A H 0.0862 -0.0454 0.6396 0.011 Uiso 1 1 calc R U . . .
H4B H 0.1086 -0.0852 0.7188 0.011 Uiso 1 1 calc R U . . .
C5 C 0.1816(2) 0.32945(13) 0.34776(8) 0.0097(3) Uani 1 1 d . . . . .
H5A H 0.1551 0.2464 0.3243 0.012 Uiso 1 1 calc R U . . .
H5B H 0.0683 0.3523 0.3545 0.012 Uiso 1 1 calc R U . . .
C6 C 0.2857(2) 0.33953(14) 0.42452(9) 0.0118(3) Uani 1 1 d . . . . .
H6A H 0.2937 0.4185 0.4524 0.014 Uiso 1 1 calc R U . . .
H6B H 0.4065 0.3294 0.4185 0.014 Uiso 1 1 calc R U . . .
C7 C 0.1932(2) 0.24421(14) 0.46839(9) 0.0125(3) Uani 1 1 d . . . . .
H7A H 0.0707 0.2523 0.4722 0.015 Uiso 1 1 calc R U . . .
H7B H 0.1896 0.1654 0.4412 0.015 Uiso 1 1 calc R U . . .
C8 C 0.2895(2) 0.25501(14) 0.54673(9) 0.0120(3) Uani 1 1 d . . . . .
H8A H 0.2927 0.3338 0.5738 0.014 Uiso 1 1 calc R U . . .
H8B H 0.4122 0.2475 0.5427 0.014 Uiso 1 1 calc R U . . .
C9 C 0.1999(2) 0.16032(14) 0.59137(9) 0.0113(3) Uani 1 1 d . . . . .
H9A H 0.0802 0.1711 0.5991 0.014 Uiso 1 1 calc R U . . .
H9B H 0.1897 0.0812 0.5634 0.014 Uiso 1 1 calc R U . . .
C10 C 0.30998(19) 0.17092(13) 0.66676(8) 0.0093(3) Uani 1 1 d . . . . .
H10A H 0.4255 0.1530 0.6581 0.011 Uiso 1 1 calc R U . . .
H10B H 0.3314 0.2532 0.6913 0.011 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Na1 O13 2.3120(12) . ?
Na1 O13 2.3120(12) 2_557 ?
Na1 O7 2.5418(11) 2_557 ?
Na1 O7 2.5419(11) . ?
Na1 O14 2.6977(14) . ?
Na1 O14 2.6977(14) 2_557 ?
Na1 Na2 3.1402(6) 2_557 ?
Na1 Na2 3.1402(6) . ?
Na1 P3 3.4501(4) . ?
Na1 P3 3.4502(4) 2_557 ?
Na2 O23 2.3174(14) . ?
Na2 O7 2.3528(13) 2_557 ?
Na2 O13 2.3623(14) 2_557 ?
Na2 O15 2.3729(14) . ?
Na2 O14 2.3754(14) . ?
Na2 O14 2.7942(16) 2_457 ?
Na2 Na2 3.4334(13) 2_457 ?
Na2 H15A 2.63(2) . ?
Na2 H23A 2.66(2) . ?
Na3 O17 2.3941(13) . ?
Na3 O17 2.3941(13) 2_767 ?
Na3 O18 2.4243(12) . ?
Na3 O18 2.4243(12) 2_767 ?
Na3 O16 2.4720(13) . ?
Na3 O16 2.4720(13) 2_767 ?
P1 O2 1.5005(12) . ?
P1 O1 1.5080(12) . ?
P1 O3 1.5577(12) . ?
P1 C1 1.8210(16) . ?
P2 O6 1.4986(12) . ?
P2 O4 1.5089(12) . ?
P2 O5 1.5595(12) . ?
P2 C2 1.8229(16) . ?
P3 O7 1.5019(12) . ?
P3 O9 1.5036(12) . ?
P3 O8 1.5737(12) . ?
P3 C3 1.8304(16) . ?
P4 O12 1.4929(12) . ?
P4 O10 1.5039(11) . ?
P4 O11 1.5635(12) . ?
P4 C4 1.8228(15) . ?
O3 H3O 0.793(16) . ?
O5 H5O 0.805(15) . ?
O7 Na2 2.3528(13) 2_557 ?
O8 H8O 0.797(15) . ?
O11 H11O 0.800(15) . ?
O13 Na2 2.3622(14) 2_557 ?
O13 H13A 0.804(16) . ?
O13 H13B 0.827(16) . ?
O14 Na2 2.7942(16) 2_457 ?
O14 H14A 0.822(16) . ?
O14 H14B 0.820(16) . ?
O15 H15A 0.791(16) . ?
O15 H15B 0.802(16) . ?
O16 H16A 0.805(16) . ?
O16 H16B 0.824(16) . ?
O17 H17A 0.815(16) . ?
O17 H17B 0.829(16) . ?
O18 H18A 0.805(16) . ?
O18 H18B 0.828(16) . ?
O19 H19A 0.801(16) . ?
O19 H19B 0.798(16) . ?
O20 H20A 0.802(16) . ?
O20 H20B 0.816(16) . ?
O21 H21A 0.824(16) . ?
O21 H21B 0.807(16) . ?
O22 H22A 0.828(16) . ?
O22 H22B 0.825(16) . ?
O23 H23A 0.826(16) . ?
O23 H23B 0.809(16) . ?
N1 C2 1.4994(19) . ?
N1 C1 1.502(2) . ?
N1 C5 1.5180(19) . ?
N1 H1 0.849(15) . ?
N2 C4 1.4956(19) . ?
N2 C3 1.5033(19) . ?
N2 C10 1.5167(19) . ?
N2 H2 0.845(15) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C6 1.521(2) . ?
C5 H5A 0.9700 . ?
C5 H5B 0.9700 . ?
C6 C7 1.530(2) . ?
C6 H6A 0.9700 . ?
C6 H6B 0.9700 . ?
C7 C8 1.519(2) . ?
C7 H7A 0.9700 . ?
C7 H7B 0.9700 . ?
C8 C9 1.527(2) . ?
C8 H8A 0.9700 . ?
C8 H8B 0.9700 . ?
C9 C10 1.519(2) . ?
C9 H9A 0.9700 . ?
C9 H9B 0.9700 . ?
C10 H10A 0.9700 . ?
C10 H10B 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
O13 Na1 O13 180.0 . 2_557 ?
O13 Na1 O7 95.32(4) . 2_557 ?
O13 Na1 O7 84.68(4) 2_557 2_557 ?
O13 Na1 O7 84.68(4) . . ?
O13 Na1 O7 95.32(4) 2_557 . ?
O7 Na1 O7 180.0 2_557 . ?
O13 Na1 O14 108.56(4) . . ?
O13 Na1 O14 71.44(4) 2_557 . ?
O7 Na1 O14 81.99(4) 2_557 . ?
O7 Na1 O14 98.01(4) . . ?
O13 Na1 O14 71.44(4) . 2_557 ?
O13 Na1 O14 108.56(4) 2_557 2_557 ?
O7 Na1 O14 98.01(4) 2_557 2_557 ?
O7 Na1 O14 81.99(4) . 2_557 ?
O14 Na1 O14 180.00(3) . 2_557 ?
O13 Na1 Na2 48.47(3) . 2_557 ?
O13 Na1 Na2 131.53(3) 2_557 2_557 ?
O7 Na1 Na2 132.51(3) 2_557 2_557 ?
O7 Na1 Na2 47.49(3) . 2_557 ?
O14 Na1 Na2 132.73(3) . 2_557 ?
O14 Na1 Na2 47.27(3) 2_557 2_557 ?
O13 Na1 Na2 131.52(3) . . ?
O13 Na1 Na2 48.48(3) 2_557 . ?
O7 Na1 Na2 47.49(3) 2_557 . ?
O7 Na1 Na2 132.51(3) . . ?
O14 Na1 Na2 47.27(3) . . ?
O14 Na1 Na2 132.73(3) 2_557 . ?
Na2 Na1 Na2 180.0 2_557 . ?
O13 Na1 P3 93.12(3) . . ?
O13 Na1 P3 86.88(3) 2_557 . ?
O7 Na1 P3 156.70(3) 2_557 . ?
O7 Na1 P3 23.30(3) . . ?
O14 Na1 P3 74.73(3) . . ?
O14 Na1 P3 105.27(3) 2_557 . ?
Na2 Na1 P3 67.722(13) 2_557 . ?
Na2 Na1 P3 112.279(13) . . ?
O13 Na1 P3 86.88(3) . 2_557 ?
O13 Na1 P3 93.12(3) 2_557 2_557 ?
O7 Na1 P3 23.30(3) 2_557 2_557 ?
O7 Na1 P3 156.70(3) . 2_557 ?
O14 Na1 P3 105.27(3) . 2_557 ?
O14 Na1 P3 74.73(3) 2_557 2_557 ?
Na2 Na1 P3 112.278(13) 2_557 2_557 ?
Na2 Na1 P3 67.721(13) . 2_557 ?
P3 Na1 P3 180.000(13) . 2_557 ?
O23 Na2 O7 100.64(5) . 2_557 ?
O23 Na2 O13 160.36(5) . 2_557 ?
O7 Na2 O13 87.94(5) 2_557 2_557 ?
O23 Na2 O15 86.67(5) . . ?
O7 Na2 O15 91.31(4) 2_557 . ?
O13 Na2 O15 110.96(5) 2_557 . ?
O23 Na2 O14 85.07(5) . . ?
O7 Na2 O14 93.33(5) 2_557 . ?
O13 Na2 O14 76.75(5) 2_557 . ?
O15 Na2 O14 171.16(5) . . ?
O23 Na2 O14 82.16(4) . 2_457 ?
O7 Na2 O14 169.31(5) 2_557 2_457 ?
O13 Na2 O14 92.67(5) 2_557 2_457 ?
O15 Na2 O14 78.50(4) . 2_457 ?
O14 Na2 O14 97.19(5) . 2_457 ?
O23 Na2 Na1 126.46(4) . . ?
O7 Na2 Na1 52.79(3) 2_557 . ?
O13 Na2 Na1 47.12(3) 2_557 . ?
O15 Na2 Na1 131.81(4) . . ?
O14 Na2 Na1 56.54(4) . . ?
O14 Na2 Na1 133.19(4) 2_457 . ?
O23 Na2 Na2 80.19(4) . 2_457 ?
O7 Na2 Na2 147.13(5) 2_557 2_457 ?
O13 Na2 Na2 83.07(4) 2_557 2_457 ?
O15 Na2 Na2 121.43(4) . 2_457 ?
O14 Na2 Na2 53.84(4) . 2_457 ?
O14 Na2 Na2 43.35(3) 2_457 2_457 ?
Na1 Na2 Na2 100.11(3) . 2_457 ?
O23 Na2 H15A 103.4(4) . . ?
O7 Na2 H15A 92.2(5) 2_557 . ?
O13 Na2 H15A 93.7(4) 2_557 . ?
O15 Na2 H15A 17.3(4) . . ?
O14 Na2 H15A 168.8(4) . . ?
O14 Na2 H15A 77.1(5) 2_457 . ?
Na1 Na2 H15A 120.8(4) . . ?
Na2 Na2 H15A 119.8(5) 2_457 . ?
O23 Na2 H23A 17.5(4) . . ?
O7 Na2 H23A 93.1(5) 2_557 . ?
O13 Na2 H23A 177.8(4) 2_557 . ?
O15 Na2 H23A 70.9(4) . . ?
O14 Na2 H23A 101.3(4) . . ?
O14 Na2 H23A 86.6(5) 2_457 . ?
Na1 Na2 H23A 132.5(5) . . ?
Na2 Na2 H23A 95.0(4) 2_457 . ?
H15A Na2 H23A 88.1(6) . . ?
O17 Na3 O17 180.00(6) . 2_767 ?
O17 Na3 O18 94.87(5) . . ?
O17 Na3 O18 85.13(5) 2_767 . ?
O17 Na3 O18 85.13(5) . 2_767 ?
O17 Na3 O18 94.87(5) 2_767 2_767 ?
O18 Na3 O18 180.00(3) . 2_767 ?
O17 Na3 O16 90.63(4) . . ?
O17 Na3 O16 89.37(4) 2_767 . ?
O18 Na3 O16 95.91(4) . . ?
O18 Na3 O16 84.09(4) 2_767 . ?
O17 Na3 O16 89.37(4) . 2_767 ?
O17 Na3 O16 90.63(4) 2_767 2_767 ?
O18 Na3 O16 84.09(4) . 2_767 ?
O18 Na3 O16 95.91(4) 2_767 2_767 ?
O16 Na3 O16 180.0 . 2_767 ?
O2 P1 O1 117.18(7) . . ?
O2 P1 O3 109.19(7) . . ?
O1 P1 O3 111.05(6) . . ?
O2 P1 C1 106.88(7) . . ?
O1 P1 C1 106.21(7) . . ?
O3 P1 C1 105.57(7) . . ?
O6 P2 O4 116.89(7) . . ?
O6 P2 O5 112.58(7) . . ?
O4 P2 O5 109.43(7) . . ?
O6 P2 C2 111.98(7) . . ?
O4 P2 C2 103.15(7) . . ?
O5 P2 C2 101.30(7) . . ?
O7 P3 O9 117.83(7) . . ?
O7 P3 O8 107.34(7) . . ?
O9 P3 O8 111.42(6) . . ?
O7 P3 C3 110.34(7) . . ?
O9 P3 C3 104.31(7) . . ?
O8 P3 C3 104.86(7) . . ?
O7 P3 Na1 42.03(5) . . ?
O9 P3 Na1 77.92(5) . . ?
O8 P3 Na1 113.82(5) . . ?
C3 P3 Na1 137.47(5) . . ?
O12 P4 O10 116.28(7) . . ?
O12 P4 O11 112.37(7) . . ?
O10 P4 O11 110.24(7) . . ?
O12 P4 C4 112.95(7) . . ?
O10 P4 C4 104.16(7) . . ?
O11 P4 C4 99.26(7) . . ?
P1 O3 H3O 112.8(17) . . ?
P2 O5 H5O 119.4(17) . . ?
P3 O7 Na2 144.57(7) . 2_557 ?
P3 O7 Na1 114.67(6) . . ?
Na2 O7 Na1 79.71(4) 2_557 . ?
P3 O8 H8O 116.0(16) . . ?
P4 O11 H11O 118.8(17) . . ?
Na1 O13 Na2 84.41(4) . 2_557 ?
Na1 O13 H13A 112.1(17) . . ?
Na2 O13 H13A 104.4(17) 2_557 . ?
Na1 O13 H13B 113.5(16) . . ?
Na2 O13 H13B 131.4(16) 2_557 . ?
H13A O13 H13B 109(2) . . ?
Na2 O14 Na1 76.19(4) . . ?
Na2 O14 Na2 82.81(5) . 2_457 ?
Na1 O14 Na2 133.35(5) . 2_457 ?
Na2 O14 H14A 138.9(18) . . ?
Na1 O14 H14A 80.5(18) . . ?
Na2 O14 H14A 89.4(17) 2_457 . ?
Na2 O14 H14B 118.7(18) . . ?
Na1 O14 H14B 124.3(18) . . ?
Na2 O14 H14B 102.4(17) 2_457 . ?
H14A O14 H14B 102(2) . . ?
Na2 O15 H15A 99.8(17) . . ?
Na2 O15 H15B 114.8(16) . . ?
H15A O15 H15B 109(2) . . ?
Na3 O16 H16A 116.2(17) . . ?
Na3 O16 H16B 114.9(17) . . ?
H16A O16 H16B 108(2) . . ?
Na3 O17 H17A 116.7(18) . . ?
Na3 O17 H17B 126.7(18) . . ?
H17A O17 H17B 97(2) . . ?
Na3 O18 H18A 109.3(17) . . ?
Na3 O18 H18B 101.9(17) . . ?
H18A O18 H18B 99(2) . . ?
H19A O19 H19B 108(2) . . ?
H20A O20 H20B 108(2) . . ?
H21A O21 H21B 106(2) . . ?
H22A O22 H22B 105(2) . . ?
Na2 O23 H23A 105.2(16) . . ?
Na2 O23 H23B 124.2(16) . . ?
H23A O23 H23B 102(2) . . ?
C2 N1 C1 113.05(11) . . ?
C2 N1 C5 113.43(12) . . ?
C1 N1 C5 109.96(12) . . ?
C2 N1 H1 107.7(14) . . ?
C1 N1 H1 105.4(14) . . ?
C5 N1 H1 106.7(14) . . ?
C4 N2 C3 113.83(11) . . ?
C4 N2 C10 112.85(12) . . ?
C3 N2 C10 110.83(12) . . ?
C4 N2 H2 107.1(14) . . ?
C3 N2 H2 105.0(14) . . ?
C10 N2 H2 106.5(14) . . ?
N1 C1 P1 115.81(10) . . ?
N1 C1 H1A 108.3 . . ?
P1 C1 H1A 108.3 . . ?
N1 C1 H1B 108.3 . . ?
P1 C1 H1B 108.3 . . ?
H1A C1 H1B 107.4 . . ?
N1 C2 P2 112.62(10) . . ?
N1 C2 H2A 109.1 . . ?
P2 C2 H2A 109.1 . . ?
N1 C2 H2B 109.1 . . ?
P2 C2 H2B 109.1 . . ?
H2A C2 H2B 107.8 . . ?
N2 C3 P3 117.25(10) . . ?
N2 C3 H3A 108.0 . . ?
P3 C3 H3A 108.0 . . ?
N2 C3 H3B 108.0 . . ?
P3 C3 H3B 108.0 . . ?
H3A C3 H3B 107.2 . . ?
N2 C4 P4 113.61(10) . . ?
N2 C4 H4A 108.8 . . ?
P4 C4 H4A 108.8 . . ?
N2 C4 H4B 108.8 . . ?
P4 C4 H4B 108.8 . . ?
H4A C4 H4B 107.7 . . ?
N1 C5 C6 114.20(12) . . ?
N1 C5 H5A 108.7 . . ?
C6 C5 H5A 108.7 . . ?
N1 C5 H5B 108.7 . . ?
C6 C5 H5B 108.7 . . ?
H5A C5 H5B 107.6 . . ?
C5 C6 C7 110.49(12) . . ?
C5 C6 H6A 109.6 . . ?
C7 C6 H6A 109.6 . . ?
C5 C6 H6B 109.6 . . ?
C7 C6 H6B 109.6 . . ?
H6A C6 H6B 108.1 . . ?
C8 C7 C6 111.91(13) . . ?
C8 C7 H7A 109.2 . . ?
C6 C7 H7A 109.2 . . ?
C8 C7 H7B 109.2 . . ?
C6 C7 H7B 109.2 . . ?
H7A C7 H7B 107.9 . . ?
C7 C8 C9 112.78(13) . . ?
C7 C8 H8A 109.0 . . ?
C9 C8 H8A 109.0 . . ?
C7 C8 H8B 109.0 . . ?
C9 C8 H8B 109.0 . . ?
H8A C8 H8B 107.8 . . ?
C10 C9 C8 109.93(12) . . ?
C10 C9 H9A 109.7 . . ?
C8 C9 H9A 109.7 . . ?
C10 C9 H9B 109.7 . . ?
C8 C9 H9B 109.7 . . ?
H9A C9 H9B 108.2 . . ?
N2 C10 C9 114.54(12) . . ?
N2 C10 H10A 108.6 . . ?
C9 C10 H10A 108.6 . . ?
N2 C10 H10B 108.6 . . ?
C9 C10 H10B 108.6 . . ?
H10A C10 H10B 107.6 . . ?

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
O9 P3 O7 Na2 -87.75(13) . . . 2_557 ?
O8 P3 O7 Na2 145.56(11) . . . 2_557 ?
C3 P3 O7 Na2 31.84(14) . . . 2_557 ?
Na1 P3 O7 Na2 -107.85(14) . . . 2_557 ?
O9 P3 O7 Na1 20.10(9) . . . . ?
O8 P3 O7 Na1 -106.59(7) . . . . ?
C3 P3 O7 Na1 139.69(6) . . . . ?
C2 N1 C1 P1 -51.72(16) . . . . ?
C5 N1 C1 P1 -179.62(10) . . . . ?
O2 P1 C1 N1 -37.92(13) . . . . ?
O1 P1 C1 N1 -163.75(11) . . . . ?
O3 P1 C1 N1 78.26(12) . . . . ?
C1 N1 C2 P2 167.01(10) . . . . ?
C5 N1 C2 P2 -66.93(14) . . . . ?
O6 P2 C2 N1 84.93(12) . . . . ?
O4 P2 C2 N1 -41.60(12) . . . . ?
O5 P2 C2 N1 -154.87(10) . . . . ?
C4 N2 C3 P3 48.91(15) . . . . ?
C10 N2 C3 P3 177.39(10) . . . . ?
O7 P3 C3 N2 41.03(13) . . . . ?
O9 P3 C3 N2 168.50(11) . . . . ?
O8 P3 C3 N2 -74.27(12) . . . . ?
Na1 P3 C3 N2 80.87(13) . . . . ?
C3 N2 C4 P4 -169.95(10) . . . . ?
C10 N2 C4 P4 62.61(14) . . . . ?
O12 P4 C4 N2 -85.46(12) . . . . ?
O10 P4 C4 N2 41.60(12) . . . . ?
O11 P4 C4 N2 155.34(11) . . . . ?
C2 N1 C5 C6 -56.23(17) . . . . ?
C1 N1 C5 C6 71.45(16) . . . . ?
N1 C5 C6 C7 -170.21(13) . . . . ?
C5 C6 C7 C8 -177.60(14) . . . . ?
C6 C7 C8 C9 -179.72(13) . . . . ?
C7 C8 C9 C10 176.08(14) . . . . ?
C4 N2 C10 C9 53.13(17) . . . . ?
C3 N2 C10 C9 -75.89(16) . . . . ?
C8 C9 C10 N2 174.07(13) . . . . ?

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
C10 H10B O3 0.97 2.42 3.3718(19) 166.3 2_666
C5 H5A O8 0.97 2.51 3.4318(19) 159.7 2_556
C4 H4B O8 0.97 2.42 3.0748(19) 124.6 .
C3 H3A O5 0.97 2.49 3.3549(19) 148.9 2_566
C2 H2A O3 0.97 2.40 3.0991(19) 129.0 .
C1 H1B O11 0.97 2.35 3.115(2) 135.5 2_656
C1 H1A O8 0.97 2.62 3.5024(19) 150.7 2_556
N2 H2 O15 0.845(15) 1.935(15) 2.7504(17) 162(2) 2_557
N1 H1 O19 0.849(15) 2.196(17) 2.9357(18) 145.5(19) 2_566
N1 H1 O4 0.849(15) 2.50(2) 2.9253(17) 111.7(16) .
O23 H23B O1 0.809(16) 1.882(16) 2.6870(16) 173(2) 1_456
O22 H22B O2 0.825(16) 1.837(17) 2.6509(17) 169(2) .
O22 H22A O18 0.828(16) 2.59(2) 3.2063(18) 132(2) 1_554
O22 H22A O17 0.828(16) 2.516(19) 3.249(2) 148(2) 2_766
O21 H21B O12 0.807(16) 1.953(16) 2.7548(16) 172(2) 2_666
O21 H21A O12 0.824(16) 1.878(17) 2.6839(17) 166(2) 1_565
O20 H20B O6 0.816(16) 1.902(16) 2.7088(17) 170(2) .
O20 H20A O6 0.802(16) 1.978(16) 2.7717(17) 170(2) 2_566
O19 H19B O7 0.798(16) 2.283(16) 3.0780(17) 175(2) 1_565
O19 H19A O1 0.801(16) 2.015(17) 2.7921(17) 164(2) 2_666
O18 H18B O19 0.828(16) 2.015(17) 2.8179(18) 163(2) 1_655
O18 H18A O2 0.805(16) 1.882(16) 2.6854(17) 175(2) 2_666
O17 H17B O4 0.829(16) 2.104(17) 2.9166(18) 167(2) 2_666
O17 H17A O9 0.815(16) 2.087(17) 2.8906(17) 169(3) 1_655
O16 H16B O22 0.824(16) 2.014(16) 2.8273(19) 169(2) 2_666
O16 H16A O1 0.805(16) 1.948(16) 2.7524(17) 179(3) 1_556
O15 H15B O9 0.802(16) 2.070(17) 2.8363(16) 160(2) 2_457
O14 H14B O16 0.820(16) 2.025(17) 2.8357(19) 170(2) 1_455
O14 H14A O9 0.822(16) 1.908(17) 2.7267(17) 174(2) .
O13 H13B O18 0.827(16) 1.984(16) 2.7974(18) 168(2) 2_667
O13 H13A O23 0.804(16) 2.007(17) 2.7857(17) 163(2) 1_655
O11 H11O O20 0.800(15) 1.745(16) 2.5233(17) 164(2) 1_545
O8 H8O O10 0.797(15) 1.754(16) 2.5399(16) 169(2) 1_455
O5 H5O O21 0.805(15) 1.732(16) 2.5189(17) 165(2) .
O3 H3O O4 0.793(16) 1.697(16) 2.4870(16) 174(3) 1_655

_refine_diff_density_max         0.548
_refine_diff_density_min         -0.434
_refine_diff_density_rms         0.084

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Rb-HDTMP
_database_code_depnum_ccdc_archive 'CCDC 1584816'
_audit_update_record             
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H35 N2 O16 P4 Rb'
_chemical_formula_weight         648.75

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'
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'
Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 2/c'
_space_group_name_Hall           '-C 2yc'

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

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

_cell_length_a                   6.14310(10)
_cell_length_b                   14.1093(2)
_cell_length_c                   28.9515(4)
_cell_angle_alpha                90
_cell_angle_beta                 94.0160(10)
_cell_angle_gamma                90
_cell_volume                     2503.20(6)
_cell_formula_units_Z            4
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    9952
_cell_measurement_theta_min      2.97
_cell_measurement_theta_max      31.37

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.721
_exptl_crystal_F_000             1336
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.090
_exptl_absorpt_coefficient_mu    2.307
_shelx_estimated_absorpt_T_min   0.392
_shelx_estimated_absorpt_T_max   0.819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.5635
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            43201
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_l_min       -44
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_theta_min         1.410
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measured_fraction_theta_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_point_group_measured_fraction_full 1.000
_reflns_number_total             4773
_reflns_number_gt                3984
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0388P)²+2.2257P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4773
_refine_ls_number_parameters     189
_refine_ls_number_restraints     10
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0328
_refine_ls_wR_factor_ref         0.0838
_refine_ls_wR_factor_gt          0.0791
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_restrained_S_all      1.038
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Rb1 Rb 0.5000 0.25464(2) 0.2500 0.04322(8) Uani 1 2 d S T P . .
P1 P 0.42175(6) 0.25601(2) 0.39976(2) 0.02323(7) Uani 1 1 d . . . . .
P2 P 0.31586(6) 0.52948(2) 0.30949(2) 0.02282(7) Uani 1 1 d . . . . .
O1 O 0.5209(2) 0.22169(8) 0.35678(4) 0.0395(3) Uani 1 1 d . . . . .
O2 O 0.17518(19) 0.22774(9) 0.39766(4) 0.0346(2) Uani 1 1 d D . . . .
H2O H 0.127(4) 0.2196(16) 0.4227(6) 0.042 Uiso 1 1 d D U . . .
O3 O 0.5346(2) 0.23103(9) 0.44540(5) 0.0396(3) Uani 1 1 d . . . . .
O4 O 0.28628(19) 0.43381(8) 0.28864(4) 0.0339(2) Uani 1 1 d . . . . .
O5 O 0.35967(19) 0.61258(8) 0.27778(4) 0.0347(2) Uani 1 1 d D . . . .
H5O H 0.465(5) 0.606(3) 0.2641(13) 0.042 Uiso 0.5 1 d D U P A -1
O6 O 0.11515(19) 0.55568(8) 0.33654(4) 0.0352(3) Uani 1 1 d D . . . .
H6O H 0.095(4) 0.6098(12) 0.3448(7) 0.042 Uiso 1 1 d D U . . .
O7A O 0.8234(4) 0.3747(2) 0.29649(9) 0.0341(5) Uani 0.5 1 d D . P B 1
H7A1 H 0.786(7) 0.402(3) 0.2724(10) 0.041 Uiso 0.5 1 d D U P C 1
H7A2 H 0.955(3) 0.379(4) 0.3021(18) 0.041 Uiso 0.5 1 d D U P D 1
O7B O 0.8775(6) 0.3359(2) 0.30858(11) 0.0407(6) Uani 0.5 1 d D . P B 2
H7B1 H 0.985(6) 0.347(4) 0.2946(16) 0.049 Uiso 0.5 1 d D U P E 2
H7B2 H 0.920(8) 0.286(2) 0.3200(16) 0.049 Uiso 0.5 1 d D U P F 2
O8 O 0.9619(2) 0.19085(12) 0.46747(5) 0.0476(3) Uani 1 1 d D . . . .
H8A H 0.835(3) 0.2021(19) 0.4607(9) 0.057 Uiso 1 1 d D U . . .
H8B H 0.980(4) 0.2175(19) 0.4923(7) 0.057 Uiso 1 1 d D U . . .
N1 N 0.59457(17) 0.42692(7) 0.37145(4) 0.01915(18) Uani 1 1 d D . . . .
H1N H 0.627(3) 0.3944(12) 0.3478(5) 0.023 Uiso 1 1 d D U . . .
C1 C 0.4023(2) 0.38401(9) 0.39245(5) 0.0219(2) Uani 1 1 d . . . . .
H1A H 0.2717 0.3986 0.3730 0.026 Uiso 1 1 calc R U . . .
H1B H 0.3870 0.4129 0.4224 0.026 Uiso 1 1 calc R U . . .
C2 C 0.5500(2) 0.52434(10) 0.35203(5) 0.0292(3) Uani 1 1 d . . . . .
H2A H 0.6785 0.5464 0.3376 0.035 Uiso 1 1 calc R U . . .
H2B H 0.5246 0.5672 0.3773 0.035 Uiso 1 1 calc R U . . .
C3 C 0.7998(2) 0.42536(10) 0.40350(4) 0.0223(2) Uani 1 1 d . . . . .
H3A H 0.9162 0.4554 0.3879 0.027 Uiso 1 1 calc R U . . .
H3B H 0.8415 0.3599 0.4092 0.027 Uiso 1 1 calc R U . . .
C4 C 0.7809(2) 0.47424(11) 0.44978(5) 0.0280(3) Uani 1 1 d . . . . .
H4A H 0.6799 0.4397 0.4678 0.034 Uiso 1 1 calc R U . . .
H4B H 0.7249 0.5380 0.4448 0.034 Uiso 1 1 calc R U . . .
C5 C 1.0046(2) 0.47823(11) 0.47611(5) 0.0277(3) Uani 1 1 d . . . . .
H5A H 1.0631 0.4145 0.4792 0.033 Uiso 1 1 calc R U . . .
H5B H 1.1027 0.5152 0.4584 0.033 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rb1 O7A 2.873(3) . ?
Rb1 O7A 2.873(3) 2_655 ?
Rb1 O7B 3.003(3) . ?
Rb1 O7B 3.003(3) 2_655 ?
Rb1 O5 3.0492(11) 4_545 ?
Rb1 O5 3.0492(11) 3_545 ?
Rb1 O4 3.0937(11) . ?
Rb1 O4 3.0938(11) 2_655 ?
Rb1 O1 3.1198(13) 2_655 ?
Rb1 O1 3.1198(13) . ?
Rb1 P2 4.0443(4) 4_545 ?
Rb1 P2 4.0443(4) 3_545 ?
Rb1 H7A1 2.76(4) . ?
Rb1 H7B2 3.20(5) . ?
P1 O3 1.4908(13) . ?
P1 O1 1.5033(12) . ?
P1 O2 1.5634(12) . ?
P1 C1 1.8213(13) . ?
P2 O4 1.4847(11) . ?
P2 O5 1.5248(11) . ?
P2 O6 1.5510(11) . ?
P2 C2 1.8284(15) . ?
P2 Rb1 4.0444(4) 3_455 ?
O2 H2O 0.810(15) . ?
O5 Rb1 3.0492(11) 3_455 ?
O5 H5O 0.789(18) . ?
O6 H6O 0.812(16) . ?
O7A H7A1 0.815(19) . ?
O7A H7A2 0.817(19) . ?
O7B H7B1 0.812(19) . ?
O7B H7B2 0.816(19) . ?
O8 H8A 0.805(17) . ?
O8 H8B 0.812(17) . ?
N1 C1 1.4940(16) . ?
N1 C2 1.5028(17) . ?
N1 C3 1.5121(16) . ?
N1 H1N 0.860(14) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.5187(18) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.525(2) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C5 1.518(3) 5_766 ?
C5 H5A 0.9700 . ?
C5 H5B 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
O7A Rb1 O7A 107.74(13) . 2_655 ?
O7B Rb1 O7B 135.09(14) . 2_655 ?
O7A Rb1 O5 167.35(6) . 4_545 ?
O7A Rb1 O5 78.43(7) 2_655 4_545 ?
O7B Rb1 O5 156.44(7) . 4_545 ?
O7B Rb1 O5 65.52(7) 2_655 4_545 ?
O7A Rb1 O5 78.43(7) . 3_545 ?
O7A Rb1 O5 167.35(6) 2_655 3_545 ?
O7B Rb1 O5 65.51(7) . 3_545 ?
O7B Rb1 O5 156.44(7) 2_655 3_545 ?
O5 Rb1 O5 97.80(5) 4_545 3_545 ?
O7A Rb1 O4 69.26(6) . . ?
O7A Rb1 O4 52.46(6) 2_655 . ?
O7B Rb1 O4 79.29(7) . . ?
O7B Rb1 O4 64.00(7) 2_655 . ?
O5 Rb1 O4 108.33(3) 4_545 . ?
O5 Rb1 O4 139.45(3) 3_545 . ?
O7A Rb1 O4 52.46(6) . 2_655 ?
O7A Rb1 O4 69.26(6) 2_655 2_655 ?
O7B Rb1 O4 64.00(7) . 2_655 ?
O7B Rb1 O4 79.29(7) 2_655 2_655 ?
O5 Rb1 O4 139.44(3) 4_545 2_655 ?
O5 Rb1 O4 108.33(3) 3_545 2_655 ?
O4 Rb1 O4 70.41(5) . 2_655 ?
O7A Rb1 O1 122.09(6) . 2_655 ?
O7A Rb1 O1 69.17(6) 2_655 2_655 ?
O7B Rb1 O1 126.37(6) . 2_655 ?
O7B Rb1 O1 61.37(6) 2_655 2_655 ?
O5 Rb1 O1 70.24(3) 4_545 2_655 ?
O5 Rb1 O1 98.17(3) 3_545 2_655 ?
O4 Rb1 O1 119.41(3) . 2_655 ?
O4 Rb1 O1 75.67(3) 2_655 2_655 ?
O7A Rb1 O1 69.18(6) . . ?
O7A Rb1 O1 122.09(6) 2_655 . ?
O7B Rb1 O1 61.37(6) . . ?
O7B Rb1 O1 126.37(6) 2_655 . ?
O5 Rb1 O1 98.17(3) 4_545 . ?
O5 Rb1 O1 70.24(3) 3_545 . ?
O4 Rb1 O1 75.67(3) . . ?
O4 Rb1 O1 119.41(3) 2_655 . ?
O1 Rb1 O1 162.86(4) 2_655 . ?
O7A Rb1 P2 163.36(6) . 4_545 ?
O7A Rb1 P2 88.18(6) 2_655 4_545 ?
O7B Rb1 P2 150.35(7) . 4_545 ?
O7B Rb1 P2 74.40(7) 2_655 4_545 ?
O5 Rb1 P2 18.93(2) 4_545 4_545 ?
O5 Rb1 P2 85.02(3) 3_545 4_545 ?
O4 Rb1 P2 126.35(2) . 4_545 ?
O4 Rb1 P2 133.70(2) 2_655 4_545 ?
O1 Rb1 P2 58.38(2) 2_655 4_545 ?
O1 Rb1 P2 106.87(2) . 4_545 ?
O7A Rb1 P2 88.18(6) . 3_545 ?
O7A Rb1 P2 163.36(6) 2_655 3_545 ?
O7B Rb1 P2 74.40(7) . 3_545 ?
O7B Rb1 P2 150.35(7) 2_655 3_545 ?
O5 Rb1 P2 85.02(3) 4_545 3_545 ?
O5 Rb1 P2 18.93(2) 3_545 3_545 ?
O4 Rb1 P2 133.71(2) . 3_545 ?
O4 Rb1 P2 126.35(2) 2_655 3_545 ?
O1 Rb1 P2 106.87(2) 2_655 3_545 ?
O1 Rb1 P2 58.38(2) . 3_545 ?
P2 Rb1 P2 76.462(11) 4_545 3_545 ?
O7A Rb1 H7A1 16.5(4) . . ?
O7A Rb1 H7A1 94.2(6) 2_655 . ?
O5 Rb1 H7A1 172.5(7) 4_545 . ?
O5 Rb1 H7A1 89.7(7) 3_545 . ?
O4 Rb1 H7A1 65.2(9) . . ?
O4 Rb1 H7A1 36.2(4) 2_655 . ?
O1 Rb1 H7A1 109.0(6) 2_655 . ?
O1 Rb1 H7A1 84.2(5) . . ?
P2 Rb1 H7A1 165.2(8) 4_545 . ?
P2 Rb1 H7A1 102.2(6) 3_545 . ?
O7B Rb1 H7B2 14.7(5) . . ?
O7B Rb1 H7B2 149.6(5) 2_655 . ?
O5 Rb1 H7B2 142.7(5) 4_545 . ?
O5 Rb1 H7B2 52.1(6) 3_545 . ?
O4 Rb1 H7B2 90.2(7) . . ?
O4 Rb1 H7B2 76.8(6) 2_655 . ?
O1 Rb1 H7B2 128.6(9) 2_655 . ?
O1 Rb1 H7B2 54.4(8) . . ?
P2 Rb1 H7B2 136.0(5) 4_545 . ?
P2 Rb1 H7B2 59.8(5) 3_545 . ?
O3 P1 O1 117.87(8) . . ?
O3 P1 O2 111.29(7) . . ?
O1 P1 O2 109.47(8) . . ?
O3 P1 C1 111.11(7) . . ?
O1 P1 C1 104.50(6) . . ?
O2 P1 C1 101.12(6) . . ?
O4 P2 O5 118.42(7) . . ?
O4 P2 O6 110.06(7) . . ?
O5 P2 O6 107.51(6) . . ?
O4 P2 C2 107.82(7) . . ?
O5 P2 C2 105.81(7) . . ?
O6 P2 C2 106.57(8) . . ?
O4 P2 Rb1 119.97(5) . 3_455 ?
O5 P2 Rb1 40.46(4) . 3_455 ?
O6 P2 Rb1 69.70(5) . 3_455 ?
C2 P2 Rb1 130.49(5) . 3_455 ?
P1 O1 Rb1 141.38(7) . . ?
P1 O2 H2O 114.3(16) . . ?
P2 O4 Rb1 147.88(7) . . ?
P2 O5 Rb1 120.61(6) . 3_455 ?
P2 O5 H5O 114(3) . . ?
Rb1 O5 H5O 123(3) 3_455 . ?
P2 O6 H6O 120.8(16) . . ?
Rb1 O7A H7A1 74(3) . . ?
Rb1 O7A H7A2 141(3) . . ?
H7A1 O7A H7A2 111(5) . . ?
Rb1 O7B H7B1 114(4) . . ?
Rb1 O7B H7B2 96(4) . . ?
H7B1 O7B H7B2 97(5) . . ?
H8A O8 H8B 101(3) . . ?
C1 N1 C2 113.23(10) . . ?
C1 N1 C3 113.16(10) . . ?
C2 N1 C3 111.41(10) . . ?
C1 N1 H1N 110.1(12) . . ?
C2 N1 H1N 103.7(12) . . ?
C3 N1 H1N 104.5(12) . . ?
N1 C1 P1 113.69(8) . . ?
N1 C1 H1A 108.8 . . ?
P1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 P2 113.72(9) . . ?
N1 C2 H2A 108.8 . . ?
P2 C2 H2A 108.8 . . ?
N1 C2 H2B 108.8 . . ?
P2 C2 H2B 108.8 . . ?
H2A C2 H2B 107.7 . . ?
N1 C3 C4 115.02(11) . . ?
N1 C3 H3A 108.5 . . ?
C4 C3 H3A 108.5 . . ?
N1 C3 H3B 108.5 . . ?
C4 C3 H3B 108.5 . . ?
H3A C3 H3B 107.5 . . ?
C3 C4 C5 109.64(11) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 C5 C4 112.39(15) 5_766 . ?
C5 C5 H5A 109.1 5_766 . ?
C4 C5 H5A 109.1 . . ?
C5 C5 H5B 109.1 5_766 . ?
C4 C5 H5B 109.1 . . ?
H5A C5 H5B 107.9 . . ?

_refine_diff_density_max         0.616
_refine_diff_density_min         -0.954
_refine_diff_density_rms         0.066

_shelxl_version_number           2014/6

####################################################################### 
# 
# 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_Cs-HDTMP
_database_code_depnum_ccdc_archive 'CCDC 1584818'
_audit_update_record             
;
2017-11-09 deposited with the CCDC.
2018-09-17 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2014/6
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H35 Cs N2 O16 P4'
_chemical_formula_weight         696.19

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'
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'
Cs Cs -0.3680 2.1192 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'

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

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.0072(2)
_cell_length_b                   7.6864(2)
_cell_length_c                   14.8250(4)
_cell_angle_alpha                86.677(2)
_cell_angle_beta                 78.906(2)
_cell_angle_gamma                67.611(2)
_cell_volume                     621.01(3)
_cell_formula_units_Z            1
_cell_measurement_temperature    297(2)
_cell_measurement_reflns_used    3273
_cell_measurement_theta_min      2.87
_cell_measurement_theta_max      27.91

_exptl_crystal_description       prism
_exptl_crystal_colour            colourless
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.862
_exptl_crystal_F_000             352
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.070
_exptl_crystal_size_min          0.030
_exptl_absorpt_coefficient_mu    1.822
_shelx_estimated_absorpt_T_min   0.839
_shelx_estimated_absorpt_T_max   0.947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.6778
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_process_details   sadabs
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      297(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   ?
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_detector_area_resol_mean ?
_diffrn_reflns_number            16513
_diffrn_reflns_av_unetI/netI     0.0421
_diffrn_reflns_av_R_equivalents  0.0483
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_theta_min         2.801
_diffrn_reflns_theta_max         30.506
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_point_group_measured_fraction_full 0.998
_reflns_number_total             3748
_reflns_number_gt                2722
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

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

_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick 2014)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0304P)²+0.1847P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   mixed
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3748
_refine_ls_number_parameters     176
_refine_ls_number_restraints     8
_refine_ls_R_factor_all          0.0580
_refine_ls_R_factor_gt           0.0344
_refine_ls_wR_factor_ref         0.0759
_refine_ls_wR_factor_gt          0.0676
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_restrained_S_all      1.023
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cs1 Cs 0.5000 1.0000 0.5000 0.04444(10) Uani 1 2 d S . P . .
P1 P 0.40629(11) 0.96649(8) 0.79782(4) 0.02161(13) Uani 1 1 d . . . . .
P2 P 0.81079(11) 0.37653(9) 0.62076(4) 0.02351(13) Uani 1 1 d . . . . .
O1 O 0.2872(4) 1.0481(2) 0.71667(13) 0.0367(4) Uani 1 1 d . . . . .
O2 O 0.6322(3) 1.0213(3) 0.79486(12) 0.0314(4) Uani 1 1 d D . . . .
H2O H 0.645(6) 1.058(4) 0.8442(15) 0.038 Uiso 1 1 d D U . . .
O3 O 0.2473(3) 1.0040(3) 0.89069(12) 0.0346(4) Uani 1 1 d . . . . .
O4 O 0.7988(3) 0.5387(3) 0.55528(12) 0.0339(4) Uani 1 1 d D . . . .
H4O H 0.931(7) 0.520(10) 0.522(4) 0.041 Uiso 0.5 1 d D U P A -1
O5 O 0.8576(3) 0.1942(2) 0.57633(11) 0.0302(4) Uani 1 1 d . . . . .
O6 O 0.9986(4) 0.3609(3) 0.68208(15) 0.0403(5) Uani 1 1 d D . . . .
H6O H 1.076(5) 0.253(3) 0.697(2) 0.048 Uiso 1 1 d D U . . .
O7 O 0.0919(4) 0.8118(3) 0.61384(13) 0.0421(5) Uani 1 1 d D . . . .
H7A H 0.011(6) 0.925(3) 0.618(2) 0.051 Uiso 1 1 d D U . . .
H7B H 0.131(6) 0.788(5) 0.5587(13) 0.051 Uiso 1 1 d D U . . .
O8 O 0.7499(4) 0.1215(3) 0.93238(14) 0.0451(5) Uani 1 1 d D . . . .
H8A H 0.897(4) 0.101(5) 0.916(2) 0.054 Uiso 1 1 d D U . . .
H8B H 0.713(6) 0.090(5) 0.9850(15) 0.054 Uiso 1 1 d D U . . .
N1 N 0.3900(3) 0.6375(3) 0.73543(12) 0.0184(4) Uani 1 1 d D . . . .
H1N H 0.321(5) 0.707(3) 0.6929(15) 0.029(7) Uiso 1 1 d D . . . .
C1 C 0.5520(4) 0.7160(3) 0.76971(15) 0.0208(4) Uani 1 1 d . . . . .
H1A H 0.6977 0.6944 0.7231 0.025 Uiso 1 1 calc R U . . .
H1B H 0.6034 0.6483 0.8241 0.025 Uiso 1 1 calc R U . . .
C2 C 0.5153(5) 0.4414(3) 0.69546(16) 0.0257(5) Uani 1 1 d . . . . .
H2A H 0.4053 0.4195 0.6615 0.031 Uiso 1 1 calc R U . . .
H2B H 0.5335 0.3549 0.7463 0.031 Uiso 1 1 calc R U . . .
C3 C 0.1661(4) 0.6474(3) 0.80641(14) 0.0217(5) Uani 1 1 d . . . . .
H3A H 0.0639 0.7788 0.8199 0.026 Uiso 1 1 calc R U . . .
H3B H 0.0727 0.5924 0.7794 0.026 Uiso 1 1 calc R U . . .
C4 C 0.2177(5) 0.5503(4) 0.89592(15) 0.0277(5) Uani 1 1 d . . . . .
H4A H 0.2852 0.6174 0.9293 0.033 Uiso 1 1 calc R U . . .
H4B H 0.3372 0.4230 0.8835 0.033 Uiso 1 1 calc R U . . .
C5 C -0.0172(5) 0.5450(4) 0.95367(16) 0.0305(6) Uani 1 1 d . . . . .
H5A H -0.1376 0.6726 0.9633 0.037 Uiso 1 1 calc R U . . .
H5B H -0.0812 0.4755 0.9201 0.037 Uiso 1 1 calc R U . . .


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

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cs1 O1 3.2072(19) . ?
Cs1 O1 3.2073(19) 2_676 ?
Cs1 O5 3.4204(19) 2_666 ?
Cs1 O5 3.4204(19) 1_565 ?
Cs1 O7 3.431(2) . ?
Cs1 O7 3.431(2) 2_676 ?
Cs1 O4 3.4421(18) . ?
Cs1 O4 3.4421(18) 2_676 ?
Cs1 O5 3.5393(18) 1_465 ?
Cs1 O5 3.5393(18) 2_766 ?
Cs1 P2 4.1644(6) 1_465 ?
Cs1 P2 4.1644(6) 2_766 ?
Cs1 H7A 3.35(3) . ?
Cs1 H7B 3.19(3) . ?
P1 O3 1.4904(18) . ?
P1 O1 1.5015(18) . ?
P1 O2 1.5594(19) . ?
P1 C1 1.821(2) . ?
P2 O5 1.4873(18) . ?
P2 O4 1.5228(18) . ?
P2 O6 1.547(2) . ?
P2 C2 1.805(2) . ?
P2 Cs1 4.1645(6) 1_645 ?
O2 H2O 0.827(17) . ?
O4 H4O 0.816(19) . ?
O5 Cs1 3.4204(18) 1_545 ?
O5 Cs1 3.5393(18) 1_645 ?
O6 H6O 0.826(18) . ?
O7 H7A 0.820(18) . ?
O7 H7B 0.817(18) . ?
O8 H8A 0.826(18) . ?
O8 H8B 0.816(18) . ?
N1 C1 1.497(3) . ?
N1 C2 1.503(3) . ?
N1 C3 1.519(3) . ?
N1 H1N 0.864(16) . ?
C1 H1A 0.9700 . ?
C1 H1B 0.9700 . ?
C2 H2A 0.9700 . ?
C2 H2B 0.9700 . ?
C3 C4 1.510(3) . ?
C3 H3A 0.9700 . ?
C3 H3B 0.9700 . ?
C4 C5 1.517(3) . ?
C4 H4A 0.9700 . ?
C4 H4B 0.9700 . ?
C5 C5 1.516(5) 2_567 ?
C5 H5A 0.9700 . ?
C5 H5B 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 Cs1 O1 180.00(7) . 2_676 ?
O1 Cs1 O5 102.47(5) . 2_666 ?
O1 Cs1 O5 77.53(5) 2_676 2_666 ?
O1 Cs1 O5 77.53(5) . 1_565 ?
O1 Cs1 O5 102.47(5) 2_676 1_565 ?
O5 Cs1 O5 180.0 2_666 1_565 ?
O1 Cs1 O7 55.62(5) . . ?
O1 Cs1 O7 124.38(5) 2_676 . ?
O5 Cs1 O7 47.84(4) 2_666 . ?
O5 Cs1 O7 132.16(4) 1_565 . ?
O1 Cs1 O7 124.38(5) . 2_676 ?
O1 Cs1 O7 55.62(5) 2_676 2_676 ?
O5 Cs1 O7 132.16(4) 2_666 2_676 ?
O5 Cs1 O7 47.84(4) 1_565 2_676 ?
O7 Cs1 O7 180.0 . 2_676 ?
O1 Cs1 O4 83.39(4) . . ?
O1 Cs1 O4 96.61(4) 2_676 . ?
O5 Cs1 O4 81.09(5) 2_666 . ?
O5 Cs1 O4 98.91(5) 1_565 . ?
O7 Cs1 O4 69.10(5) . . ?
O7 Cs1 O4 110.90(5) 2_676 . ?
O1 Cs1 O4 96.61(4) . 2_676 ?
O1 Cs1 O4 83.39(4) 2_676 2_676 ?
O5 Cs1 O4 98.91(5) 2_666 2_676 ?
O5 Cs1 O4 81.09(5) 1_565 2_676 ?
O7 Cs1 O4 110.90(5) . 2_676 ?
O7 Cs1 O4 69.10(5) 2_676 2_676 ?
O4 Cs1 O4 180.0 . 2_676 ?
O1 Cs1 O5 61.09(4) . 1_465 ?
O1 Cs1 O5 118.91(4) 2_676 1_465 ?
O5 Cs1 O5 60.67(5) 2_666 1_465 ?
O5 Cs1 O5 119.33(5) 1_565 1_465 ?
O7 Cs1 O5 47.49(4) . 1_465 ?
O7 Cs1 O5 132.51(4) 2_676 1_465 ?
O4 Cs1 O5 116.52(4) . 1_465 ?
O4 Cs1 O5 63.48(4) 2_676 1_465 ?
O1 Cs1 O5 118.91(4) . 2_766 ?
O1 Cs1 O5 61.09(4) 2_676 2_766 ?
O5 Cs1 O5 119.33(5) 2_666 2_766 ?
O5 Cs1 O5 60.67(5) 1_565 2_766 ?
O7 Cs1 O5 132.51(4) . 2_766 ?
O7 Cs1 O5 47.49(4) 2_676 2_766 ?
O4 Cs1 O5 63.48(4) . 2_766 ?
O4 Cs1 O5 116.52(4) 2_676 2_766 ?
O5 Cs1 O5 180.0 1_465 2_766 ?
O1 Cs1 P2 54.80(3) . 1_465 ?
O1 Cs1 P2 125.20(3) 2_676 1_465 ?
O5 Cs1 P2 80.50(3) 2_666 1_465 ?
O5 Cs1 P2 99.50(3) 1_565 1_465 ?
O7 Cs1 P2 62.91(4) . 1_465 ?
O7 Cs1 P2 117.09(4) 2_676 1_465 ?
O4 Cs1 P2 128.49(3) . 1_465 ?
O4 Cs1 P2 51.51(3) 2_676 1_465 ?
O5 Cs1 P2 20.25(3) 1_465 1_465 ?
O5 Cs1 P2 159.75(3) 2_766 1_465 ?
O1 Cs1 P2 125.20(3) . 2_766 ?
O1 Cs1 P2 54.80(3) 2_676 2_766 ?
O5 Cs1 P2 99.50(3) 2_666 2_766 ?
O5 Cs1 P2 80.50(3) 1_565 2_766 ?
O7 Cs1 P2 117.09(4) . 2_766 ?
O7 Cs1 P2 62.91(4) 2_676 2_766 ?
O4 Cs1 P2 51.51(3) . 2_766 ?
O4 Cs1 P2 128.49(3) 2_676 2_766 ?
O5 Cs1 P2 159.75(3) 1_465 2_766 ?
O5 Cs1 P2 20.25(3) 2_766 2_766 ?
P2 Cs1 P2 180.0 1_465 2_766 ?
O1 Cs1 H7A 51.3(6) . . ?
O1 Cs1 H7A 128.7(6) 2_676 . ?
O5 Cs1 H7A 51.5(6) 2_666 . ?
O5 Cs1 H7A 128.5(6) 1_565 . ?
O7 Cs1 H7A 13.8(3) . . ?
O7 Cs1 H7A 166.2(3) 2_676 . ?
O4 Cs1 H7A 82.4(3) . . ?
O4 Cs1 H7A 97.6(3) 2_676 . ?
O5 Cs1 H7A 34.2(3) 1_465 . ?
O5 Cs1 H7A 145.8(3) 2_766 . ?
P2 Cs1 H7A 49.1(3) 1_465 . ?
P2 Cs1 H7A 130.9(3) 2_766 . ?
O1 Cs1 H7B 69.1(3) . . ?
O1 Cs1 H7B 110.9(3) 2_676 . ?
O5 Cs1 H7B 34.8(4) 2_666 . ?
O5 Cs1 H7B 145.2(4) 1_565 . ?
O7 Cs1 H7B 13.5(3) . . ?
O7 Cs1 H7B 166.5(3) 2_676 . ?
O4 Cs1 H7B 68.1(6) . . ?
O4 Cs1 H7B 111.9(6) 2_676 . ?
O5 Cs1 H7B 51.2(6) 1_465 . ?
O5 Cs1 H7B 128.8(6) 2_766 . ?
P2 Cs1 H7B 69.4(6) 1_465 . ?
P2 Cs1 H7B 110.6(5) 2_766 . ?
H7A Cs1 H7B 22.8(6) . . ?
O3 P1 O1 117.62(12) . . ?
O3 P1 O2 111.15(10) . . ?
O1 P1 O2 109.54(11) . . ?
O3 P1 C1 112.10(11) . . ?
O1 P1 C1 103.23(10) . . ?
O2 P1 C1 101.82(10) . . ?
O5 P2 O4 115.28(10) . . ?
O5 P2 O6 112.78(11) . . ?
O4 P2 O6 107.95(12) . . ?
O5 P2 C2 106.23(11) . . ?
O4 P2 C2 107.23(11) . . ?
O6 P2 C2 106.90(12) . . ?
O5 P2 Cs1 55.43(8) . 1_645 ?
O4 P2 Cs1 97.59(7) . 1_645 ?
O6 P2 Cs1 70.47(8) . 1_645 ?
C2 P2 Cs1 154.31(8) . 1_645 ?
P1 O1 Cs1 131.31(10) . . ?
P1 O2 H2O 116(2) . . ?
P2 O4 Cs1 148.78(9) . . ?
P2 O4 H4O 112(5) . . ?
Cs1 O4 H4O 98(5) . . ?
P2 O5 Cs1 134.72(10) . 1_545 ?
P2 O5 Cs1 104.32(9) . 1_645 ?
Cs1 O5 Cs1 119.33(5) 1_545 1_645 ?
P2 O6 H6O 115(2) . . ?
Cs1 O7 H7A 77(2) . . ?
Cs1 O7 H7B 66(2) . . ?
H7A O7 H7B 105(3) . . ?
H8A O8 H8B 114(4) . . ?
C1 N1 C2 115.41(18) . . ?
C1 N1 C3 113.42(17) . . ?
C2 N1 C3 109.06(17) . . ?
C1 N1 H1N 111.4(18) . . ?
C2 N1 H1N 105.8(18) . . ?
C3 N1 H1N 100.5(18) . . ?
N1 C1 P1 113.72(15) . . ?
N1 C1 H1A 108.8 . . ?
P1 C1 H1A 108.8 . . ?
N1 C1 H1B 108.8 . . ?
P1 C1 H1B 108.8 . . ?
H1A C1 H1B 107.7 . . ?
N1 C2 P2 119.43(15) . . ?
N1 C2 H2A 107.5 . . ?
P2 C2 H2A 107.5 . . ?
N1 C2 H2B 107.5 . . ?
P2 C2 H2B 107.5 . . ?
H2A C2 H2B 107.0 . . ?
C4 C3 N1 115.68(19) . . ?
C4 C3 H3A 108.4 . . ?
N1 C3 H3A 108.4 . . ?
C4 C3 H3B 108.4 . . ?
N1 C3 H3B 108.4 . . ?
H3A C3 H3B 107.4 . . ?
C3 C4 C5 109.8(2) . . ?
C3 C4 H4A 109.7 . . ?
C5 C4 H4A 109.7 . . ?
C3 C4 H4B 109.7 . . ?
C5 C4 H4B 109.7 . . ?
H4A C4 H4B 108.2 . . ?
C5 C5 C4 113.2(3) 2_567 . ?
C5 C5 H5A 108.9 2_567 . ?
C4 C5 H5A 108.9 . . ?
C5 C5 H5B 108.9 2_567 . ?
C4 C5 H5B 108.9 . . ?
H5A C5 H5B 107.8 . . ?

_refine_diff_density_max         0.418
_refine_diff_density_min         -0.591
_refine_diff_density_rms         0.090

_shelxl_version_number           2014/6

