# Supplementary Information (SI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_ak-251
_database_code_depnum_ccdc_archive 'CCDC 2330476'
loop_
_audit_author_name
_audit_author_address
'R Murugavel'
;IIT Bombay
India
;
_audit_update_record             
;
2024-02-02 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
_audit_creation_date             2024-01-29
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H16 Li O6 P, H2 O'
_chemical_formula_sum            'C4 H18 Li O7 P'
_chemical_formula_weight         216.09
_chemical_melting_point          ?
_chemical_oxdiff_formula         'Li1 O5 P4'
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   6.2774(3)
_cell_length_b                   6.5742(4)
_cell_length_c                   15.5423(8)
_cell_angle_alpha                79.599(4)
_cell_angle_beta                 88.942(4)
_cell_angle_gamma                63.141(5)
_cell_volume                     561.36(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5115
_cell_measurement_temperature    150
_cell_measurement_theta_max      28.5600
_cell_measurement_theta_min      2.6500
_shelx_estimated_absorpt_T_max   0.976
_shelx_estimated_absorpt_T_min   0.929
_exptl_absorpt_coefficient_mu    0.248
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.54706
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.278
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             232
_exptl_crystal_preparation       .
_exptl_crystal_recrystallization_method .
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0924
_diffrn_reflns_av_unetI/netI     0.0460
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            12680
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         2.672
_diffrn_ambient_temperature      150.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -53.00  94.00   1.00    4.00    --    5.00  19.00 -90.00  147
  2  ω   -104.00  24.00   1.00    4.00    --  -14.30 -72.00  60.00  128
  3  ω   -104.00  24.00   1.00    4.00    --  -14.30 -72.00-180.00  128
  4  ω   -104.00  19.00   1.00    4.00    --  -14.30 -38.00 -90.00  123
  5  ω    -53.00  75.00   1.00    4.00    --  -14.30  72.00-120.00  128
  6  ω    -50.00  75.00   1.00    4.00    --  -14.30  57.00   0.00  125
  7  ω    -50.00  75.00   1.00    4.00    --  -14.30  57.00-150.00  125
  8  ω    -53.00 -15.00   1.00    4.00    --  -14.30  72.00  30.00   38
  9  ω    -53.00  75.00   1.00    4.00    --  -14.30  72.00  90.00  128
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0864606000
_diffrn_orient_matrix_UB_12      -0.0212878000
_diffrn_orient_matrix_UB_13      0.0336497000
_diffrn_orient_matrix_UB_21      0.0679488000
_diffrn_orient_matrix_UB_22      0.0315930000
_diffrn_orient_matrix_UB_23      -0.0316959000
_diffrn_orient_matrix_UB_31      -0.0635023000
_diffrn_orient_matrix_UB_32      0.1172212000
_diffrn_orient_matrix_UB_33      0.0052100000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          .
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1700
_reflns_number_total             1969
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.872
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1969
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0705
_refine_ls_R_factor_gt           0.0632
_refine_ls_restrained_S_all      1.066
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1038P)²+0.2998P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1661
_refine_ls_wR_factor_ref         0.1742
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2.a Free rotating group:
 O7(H7A)
2.b Rotating group:
 O4(H4A,H4B), O5(H5A), O6(H6A,H6B)
2.c Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4C,H4D,H4E)
2.d Idealised tetrahedral OH refined as rotating group:
 O3(H3)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.67938(12) 0.26694(12) 0.73106(4) 0.0272(3) Uani 1 1 d . . . . .
O1 O 0.4811(3) 0.5034(3) 0.69348(12) 0.0295(5) Uani 1 1 d . . . . .
O2 O 0.6947(4) 0.0733(3) 0.68791(14) 0.0383(6) Uani 1 1 d . . . . .
O3 O 0.9321(3) 0.2666(3) 0.72068(13) 0.0321(5) Uani 1 1 d . . . . .
H3 H 0.915016 0.401877 0.718190 0.048 Uiso 1 1 calc GR . . . .
O4 O 0.2220(4) 0.7572(4) 0.49765(14) 0.0413(6) Uani 1 1 d . . . . .
H4A H 0.261301 0.621022 0.488872 0.062 Uiso 1 1 d GR . . . .
H4B H 0.247674 0.827111 0.450073 0.062 Uiso 1 1 d GR . . . .
O5 O 0.7381(4) 0.6697(4) 0.53885(14) 0.0342(5) Uani 1 1 d . . . . .
H5A H 0.713811 0.763168 0.489889 0.051 Uiso 1 1 d GR . . . .
H5B H 0.835(7) 0.661(6) 0.574(2) 0.039(10) Uiso 1 1 d . . . . .
O6 O 0.3197(3) 1.0441(3) 0.62234(12) 0.0304(5) Uani 1 1 d . . . . .
H6A H 0.430453 1.045307 0.652999 0.046 Uiso 1 1 d GR . . . .
H6B H 0.206078 1.068246 0.656399 0.046 Uiso 1 1 d GR . . . .
C1 C 0.6605(5) 0.1958(6) 0.84845(19) 0.0387(8) Uani 1 1 d . . . . .
C2 C 0.6695(8) 0.3832(7) 0.8917(2) 0.0631(11) Uani 1 1 d . . . . .
H2A H 0.823922 0.384564 0.883071 0.095 Uiso 1 1 calc GR . . . .
H2B H 0.650409 0.349973 0.954576 0.095 Uiso 1 1 calc GR . . . .
H2C H 0.539890 0.535252 0.865054 0.095 Uiso 1 1 calc GR . . . .
C3 C 0.8723(6) -0.0426(7) 0.8861(2) 0.0508(9) Uani 1 1 d . . . . .
H3A H 0.862368 -0.162512 0.859403 0.076 Uiso 1 1 calc GR . . . .
H3B H 0.865725 -0.079227 0.949748 0.076 Uiso 1 1 calc GR . . . .
H3C H 1.023329 -0.037536 0.872975 0.076 Uiso 1 1 calc GR . . . .
C4 C 0.4243(7) 0.1819(9) 0.8642(3) 0.0727(14) Uani 1 1 d . . . . .
H4C H 0.289626 0.329830 0.837020 0.109 Uiso 1 1 calc GR . . . .
H4D H 0.407714 0.150592 0.927355 0.109 Uiso 1 1 calc GR . . . .
H4E H 0.425096 0.056497 0.838126 0.109 Uiso 1 1 calc GR . . . .
Li1 Li 0.4314(8) 0.7368(8) 0.5924(3) 0.0330(11) Uani 1 1 d . . . . .
O7 O 1.0024(4) 0.6305(4) 0.68928(15) 0.0358(5) Uani 1 1 d . . . . .
H7A H 1.147984 0.603313 0.693918 0.054 Uiso 1 1 d G . . . .
H7B H 0.928(9) 0.763(8) 0.699(3) 0.078(15) Uiso 1 1 d . . . . .


_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 O1 1.5027(19) . ?
P1 O2 1.508(2) . ?
P1 O3 1.5904(19) . ?
P1 C1 1.815(3) . ?
O1 Li1 1.906(5) . ?
O3 H3 0.8400 . ?
O4 H4A 0.8508 . ?
O4 H4B 0.8509 . ?
O4 Li1 1.938(5) . ?
O5 H5A 0.8549 . ?
O5 H5B 0.80(4) . ?
O5 Li1 1.975(5) . ?
O6 H6A 0.8536 . ?
O6 H6B 0.8535 . ?
O6 Li1 1.959(5) . ?
C1 C2 1.528(5) . ?
C1 C3 1.543(5) . ?
C1 C4 1.539(4) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4C 0.9800 . ?
C4 H4D 0.9800 . ?
C4 H4E 0.9800 . ?
O7 H7A 0.8502 . ?
O7 H7B 0.82(5) . ?

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 P1 O2 115.15(11) . . ?
O1 P1 O3 110.25(10) . . ?
O1 P1 C1 110.25(13) . . ?
O2 P1 O3 105.27(12) . . ?
O2 P1 C1 110.30(15) . . ?
O3 P1 C1 105.05(12) . . ?
P1 O1 Li1 135.56(19) . . ?
P1 O3 H3 109.5 . . ?
H4A O4 H4B 104.4 . . ?
Li1 O4 H4A 108.9 . . ?
Li1 O4 H4B 109.4 . . ?
H5A O5 H5B 117.1 . . ?
Li1 O5 H5A 110.0 . . ?
Li1 O5 H5B 110(3) . . ?
H6A O6 H6B 104.3 . . ?
Li1 O6 H6A 109.4 . . ?
Li1 O6 H6B 109.5 . . ?
C2 C1 P1 109.2(2) . . ?
C2 C1 C3 110.0(3) . . ?
C2 C1 C4 110.8(3) . . ?
C3 C1 P1 109.2(2) . . ?
C4 C1 P1 108.4(2) . . ?
C4 C1 C3 109.2(3) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4C 109.5 . . ?
C1 C4 H4D 109.5 . . ?
C1 C4 H4E 109.5 . . ?
H4C C4 H4D 109.5 . . ?
H4C C4 H4E 109.5 . . ?
H4D C4 H4E 109.5 . . ?
O1 Li1 O4 115.6(3) . . ?
O1 Li1 O5 109.7(2) . . ?
O1 Li1 O6 111.9(2) . . ?
O4 Li1 O5 103.9(2) . . ?
O4 Li1 O6 109.3(2) . . ?
O6 Li1 O5 105.7(2) . . ?
H7A O7 H7B 103.8 . . ?

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
_geom_hbond_publ_flag
O3 H3 O7 0.84 1.80 2.585(3) 153.9 . yes
O4 H4A O5 0.85 2.03 2.862(3) 165.1 2_666 yes
O5 H5A O6 0.85 1.91 2.768(3) 175.9 2_676 yes
O5 H5B O7 0.80(4) 2.03(4) 2.797(3) 161(3) . yes
O6 H6A O2 0.85 1.85 2.680(3) 163.5 1_565 yes
O6 H6B O3 0.85 2.01 2.802(3) 154.1 1_465 yes
O7 H7A O1 0.85 1.89 2.730(3) 170.4 1_655 yes
O7 H7B O2 0.82(5) 1.88(5) 2.665(3) 161(4) 1_565 yes

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
O1 P1 C1 C2 -57.1(2) . . . . ?
O1 P1 C1 C3 -177.5(2) . . . . ?
O1 P1 C1 C4 63.7(3) . . . . ?
O2 P1 O1 Li1 -78.5(3) . . . . ?
O2 P1 C1 C2 174.6(2) . . . . ?
O2 P1 C1 C3 54.2(3) . . . . ?
O2 P1 C1 C4 -64.6(3) . . . . ?
O3 P1 O1 Li1 40.4(3) . . . . ?
O3 P1 C1 C2 61.6(2) . . . . ?
O3 P1 C1 C3 -58.7(2) . . . . ?
O3 P1 C1 C4 -177.5(3) . . . . ?
C1 P1 O1 Li1 156.0(3) . . . . ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 2.814
_oxdiff_exptl_absorpt_empirical_full_min 0.338
####################################################################### 
# 
# 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_ak-252
_database_code_depnum_ccdc_archive 'CCDC 2330478'
loop_
_audit_author_name
_audit_author_address
'R Murugavel'
;IIT Bombay
India
;
_audit_update_record             
;
2024-02-02 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;
# start Validation Reply Form
_vrf_PLAT043_ak-252              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       2.02 Check 
RESPONSE: H-atoms on the triply coordinated water oxygen atom were 
not identified or meaningfully fixed, which account for the 
difference of two H-atoms.

;

# end Validation Reply Form

_audit_creation_date             2024-01-31
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H10 K O4 P'
_chemical_formula_sum            'C4 H12 K O4 P'
_chemical_formula_weight         194.21
_chemical_melting_point          ?
_chemical_oxdiff_formula         'K1 C10 P2 O5'
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'
K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   13.6615(6)
_cell_length_b                   9.2070(4)
_cell_length_c                   7.0197(3)
_cell_angle_alpha                90
_cell_angle_beta                 101.967(4)
_cell_angle_gamma                90
_cell_volume                     863.76(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5392
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.9120
_cell_measurement_theta_min      2.6670
_shelx_estimated_absorpt_T_max   0.888
_shelx_estimated_absorpt_T_min   0.869
_exptl_absorpt_coefficient_mu    0.761
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.85550
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             408
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            14934
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.992
_diffrn_reflns_theta_max         24.992
_diffrn_reflns_theta_min         2.686
_diffrn_ambient_temperature      100.0
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -48.00  75.00   1.00    8.00    --  -14.30  38.00 -30.00  123
  2  ω   -104.00  19.00   1.00    8.00    --  -14.30 -38.00 120.00  123
  3  ω    -48.00  75.00   1.00    8.00    --  -14.30  38.00-120.00  123
  4  ω   -104.00  24.00   1.00    8.00    --  -14.30 -72.00 -60.00  128
  5  ω    -53.00  75.00   1.00    8.00    --  -14.30  72.00   0.00  128
  6  ω   -104.00   0.00   1.00    8.00    --  -14.30 -57.00  60.00  104
  7  ω    -48.00  75.00   1.00    8.00    --  -14.30  38.00 120.00  123
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0291129000
_diffrn_orient_matrix_UB_12      -0.0628257000
_diffrn_orient_matrix_UB_13      0.0302977000
_diffrn_orient_matrix_UB_21      -0.0438330000
_diffrn_orient_matrix_UB_22      -0.0381141000
_diffrn_orient_matrix_UB_23      0.0096496000
_diffrn_orient_matrix_UB_31      -0.0068965000
_diffrn_orient_matrix_UB_32      -0.0230920000
_diffrn_orient_matrix_UB_33      -0.0982913000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1435
_reflns_number_total             1520
_reflns_odcompleteness_completeness 99.95
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         1.374
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.145
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     95
_refine_ls_number_reflns         1520
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0841
_refine_ls_R_factor_gt           0.0815
_refine_ls_restrained_S_all      1.119
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1377P)²+3.4259P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2322
_refine_ls_wR_factor_ref         0.2350
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2. Restrained distances
 P1-O2
 1.508 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
3.b Idealised tetrahedral OH refined as rotating group:
 O2(H2)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K1 K 0.44722(9) 0.59475(14) 0.72305(17) 0.0351(5) Uani 1 1 d . . . . .
P1 P 0.70236(10) 0.43655(14) 0.7181(2) 0.0264(5) Uani 1 1 d D . . . .
O1 O 0.6285(3) 0.5520(4) 0.6320(6) 0.0347(10) Uani 1 1 d . . . . .
O2 O 0.7108(3) 0.4373(4) 0.9455(5) 0.0314(9) Uani 1 1 d D . . . .
H2 H 0.702921 0.352515 0.983889 0.047 Uiso 1 1 calc GR . . . .
O3 O 0.6750(3) 0.2865(4) 0.6384(5) 0.0324(9) Uani 1 1 d . . . . .
O4 O 0.5896(3) 0.8417(5) 0.5723(6) 0.0402(10) Uani 1 1 d . . . . .
C2 C 0.8204(5) 0.4958(7) 0.4603(10) 0.0436(15) Uani 1 1 d . . . . .
H2A H 0.808644 0.398449 0.403583 0.065 Uiso 1 1 calc GR . . . .
H2B H 0.883580 0.534017 0.435655 0.065 Uiso 1 1 calc GR . . . .
H2C H 0.765388 0.560143 0.400800 0.065 Uiso 1 1 calc GR . . . .
C3 C 0.9039(5) 0.3740(8) 0.7706(11) 0.0484(16) Uani 1 1 d . . . . .
H3A H 0.905858 0.366662 0.910655 0.073 Uiso 1 1 calc GR . . . .
H3B H 0.969916 0.403137 0.749927 0.073 Uiso 1 1 calc GR . . . .
H3C H 0.885829 0.279500 0.709052 0.073 Uiso 1 1 calc GR . . . .
C4 C 0.8556(5) 0.6356(7) 0.7705(10) 0.0464(16) Uani 1 1 d . . . . .
H4A H 0.805391 0.707775 0.712795 0.070 Uiso 1 1 calc GR . . . .
H4B H 0.920963 0.663575 0.745357 0.070 Uiso 1 1 calc GR . . . .
H4C H 0.859418 0.630946 0.911343 0.070 Uiso 1 1 calc GR . . . .
C5 C 0.8261(4) 0.4875(6) 0.6805(8) 0.0325(12) Uani 1 1 d . . . . .


_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 K1 4.099(2) 3_666 ?
K1 K1 4.233(2) 3_667 ?
K1 P1 3.8210(18) 2_656 ?
K1 P1 3.3501(18) 3_666 ?
K1 P1 3.7846(18) . ?
K1 O1 2.835(4) 3_666 ?
K1 O1 2.712(4) . ?
K1 O3 2.742(4) 2_656 ?
K1 O3 2.944(4) 3_666 ?
K1 O4 2.836(4) 2_646 ?
K1 O4 3.306(4) . ?
K1 O4 2.857(4) 4_576 ?
P1 O1 1.503(4) . ?
P1 O2 1.577(4) . ?
P1 O3 1.508(4) . ?
P1 C5 1.825(5) . ?
O2 H2 0.8400 . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C2 C5 1.534(8) . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C3 C5 1.531(8) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C4 C5 1.522(8) . ?

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
K1 K1 K1 114.80(6) 3_666 3_667 ?
P1 K1 K1 73.19(4) . 3_667 ?
P1 K1 K1 109.15(5) 2_656 3_667 ?
P1 K1 K1 135.56(5) 2_656 3_666 ?
P1 K1 K1 60.07(4) 3_666 3_666 ?
P1 K1 K1 50.10(3) . 3_666 ?
P1 K1 K1 147.14(6) 3_666 3_667 ?
P1 K1 P1 146.33(5) . 2_656 ?
P1 K1 P1 110.17(4) 3_666 . ?
P1 K1 P1 86.18(4) 3_666 2_656 ?
O1 K1 K1 127.15(9) 3_666 3_667 ?
O1 K1 K1 90.15(9) . 3_667 ?
O1 K1 K1 41.20(8) 3_666 3_666 ?
O1 K1 K1 43.53(9) . 3_666 ?
O1 K1 P1 112.44(9) 3_666 2_656 ?
O1 K1 P1 132.85(10) . 2_656 ?
O1 K1 P1 26.49(8) 3_666 3_666 ?
O1 K1 P1 18.92(9) . . ?
O1 K1 P1 88.70(8) 3_666 . ?
O1 K1 P1 100.46(9) . 3_666 ?
O1 K1 O1 84.74(12) . 3_666 ?
O1 K1 O3 146.08(13) . 2_656 ?
O1 K1 O3 51.75(11) 3_666 3_666 ?
O1 K1 O3 103.49(12) . 3_666 ?
O1 K1 O4 100.25(11) 3_666 . ?
O1 K1 O4 105.46(12) . 2_646 ?
O1 K1 O4 89.03(12) 3_666 2_646 ?
O1 K1 O4 155.72(12) 3_666 4_576 ?
O1 K1 O4 52.96(11) . . ?
O1 K1 O4 74.89(12) . 4_576 ?
O3 K1 K1 93.22(9) 2_656 3_667 ?
O3 K1 K1 151.79(9) 2_656 3_666 ?
O3 K1 K1 74.10(8) 3_666 3_666 ?
O3 K1 K1 165.77(9) 3_666 3_667 ?
O3 K1 P1 151.70(9) 2_656 . ?
O3 K1 P1 119.59(8) 3_666 . ?
O3 K1 P1 26.75(7) 3_666 3_666 ?
O3 K1 P1 94.80(9) 2_656 3_666 ?
O3 K1 P1 18.75(8) 2_656 2_656 ?
O3 K1 P1 64.33(8) 3_666 2_656 ?
O3 K1 O1 118.72(12) 2_656 3_666 ?
O3 K1 O3 77.79(8) 2_656 3_666 ?
O3 K1 O4 85.41(12) 2_656 4_576 ?
O3 K1 O4 74.61(11) 3_666 . ?
O3 K1 O4 96.46(11) 2_656 . ?
O3 K1 O4 99.46(12) 2_656 2_646 ?
O4 K1 K1 99.48(9) 2_646 3_666 ?
O4 K1 K1 41.78(9) 4_576 3_667 ?
O4 K1 K1 117.26(9) 4_576 3_666 ?
O4 K1 K1 42.15(8) 2_646 3_667 ?
O4 K1 K1 117.81(8) . 3_667 ?
O4 K1 K1 74.02(8) . 3_666 ?
O4 K1 P1 67.80(9) 4_576 . ?
O4 K1 P1 69.97(8) . . ?
O4 K1 P1 170.85(10) 4_576 3_666 ?
O4 K1 P1 91.30(9) 4_576 2_656 ?
O4 K1 P1 80.30(8) . 2_656 ?
O4 K1 P1 92.86(8) . 3_666 ?
O4 K1 P1 105.02(9) 2_646 3_666 ?
O4 K1 P1 117.83(9) 2_646 2_656 ?
O4 K1 P1 87.07(9) 2_646 . ?
O4 K1 O3 127.84(12) 2_646 3_666 ?
O4 K1 O3 145.83(12) 4_576 3_666 ?
O4 K1 O4 78.04(9) 4_576 . ?
O4 K1 O4 83.93(13) 2_646 4_576 ?
O4 K1 O4 154.83(7) 2_646 . ?
K1 P1 K1 69.83(4) 3_666 . ?
K1 P1 K1 77.98(4) 3_666 2_646 ?
K1 P1 K1 78.57(3) . 2_646 ?
O1 P1 K1 107.24(16) . 2_646 ?
O1 P1 K1 57.28(16) . 3_666 ?
O1 P1 K1 35.79(16) . . ?
O1 P1 O2 107.8(2) . . ?
O1 P1 O3 113.9(2) . . ?
O1 P1 C5 109.0(2) . . ?
O2 P1 K1 147.00(16) . 3_666 ?
O2 P1 K1 82.11(16) . . ?
O2 P1 K1 79.77(14) . 2_646 ?
O2 P1 C5 105.7(2) . . ?
O3 P1 K1 101.41(16) . . ?
O3 P1 K1 35.75(14) . 2_646 ?
O3 P1 K1 61.43(15) . 3_666 ?
O3 P1 O2 109.9(2) . . ?
O3 P1 C5 110.4(2) . . ?
C5 P1 K1 141.70(19) . . ?
C5 P1 K1 107.11(19) . 3_666 ?
C5 P1 K1 139.40(19) . 2_646 ?
K1 O1 K1 95.27(12) . 3_666 ?
P1 O1 K1 125.3(2) . . ?
P1 O1 K1 96.22(19) . 3_666 ?
P1 O2 H2 109.5 . . ?
K1 O3 K1 105.47(13) 2_646 3_666 ?
P1 O3 K1 125.5(2) . 2_646 ?
P1 O3 K1 91.82(17) . 3_666 ?
K1 O4 K1 96.07(13) 2_656 4_575 ?
K1 O4 K1 103.01(12) 2_656 . ?
K1 O4 K1 94.27(12) 4_575 . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C5 C2 H2A 109.5 . . ?
C5 C2 H2B 109.5 . . ?
C5 C2 H2C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C5 C3 H3A 109.5 . . ?
C5 C3 H3B 109.5 . . ?
C5 C3 H3C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C5 C4 H4A 109.5 . . ?
C5 C4 H4B 109.5 . . ?
C5 C4 H4C 109.5 . . ?
C2 C5 P1 107.7(4) . . ?
C3 C5 P1 110.5(4) . . ?
C3 C5 C2 109.6(5) . . ?
C4 C5 P1 110.1(4) . . ?
C4 C5 C2 109.1(5) . . ?
C4 C5 C3 109.8(5) . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O2 H2 O3 0.84 1.77 2.568(5) 157.9 4_566 yes

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
K1 P1 O1 K1 101.0(3) 3_666 . . . ?
K1 P1 O1 K1 38.3(3) 2_646 . . . ?
K1 P1 O1 K1 -101.0(3) . . . 3_666 ?
K1 P1 O1 K1 -62.71(13) 2_646 . . 3_666 ?
K1 P1 O3 K1 110.5(2) 2_646 . . 3_666 ?
K1 P1 O3 K1 59.31(10) . . . 3_666 ?
K1 P1 O3 K1 -51.2(2) . . . 2_646 ?
K1 P1 O3 K1 -110.5(2) 3_666 . . 2_646 ?
K1 P1 C5 C2 -80.0(5) . . . . ?
K1 P1 C5 C2 -1.1(4) 3_666 . . . ?
K1 P1 C5 C2 90.3(4) 2_646 . . . ?
K1 P1 C5 C3 -29.4(6) 2_646 . . . ?
K1 P1 C5 C3 160.3(3) . . . . ?
K1 P1 C5 C3 -120.8(4) 3_666 . . . ?
K1 P1 C5 C4 -150.9(3) 2_646 . . . ?
K1 P1 C5 C4 38.8(6) . . . . ?
K1 P1 C5 C4 117.8(4) 3_666 . . . ?
O1 P1 O3 K1 24.0(2) . . . 3_666 ?
O1 P1 O3 K1 -86.6(3) . . . 2_646 ?
O1 P1 C5 C2 -61.6(4) . . . . ?
O1 P1 C5 C3 178.7(4) . . . . ?
O1 P1 C5 C4 57.2(5) . . . . ?
O2 P1 O1 K1 -46.3(3) . . . . ?
O2 P1 O1 K1 -147.22(17) . . . 3_666 ?
O2 P1 O3 K1 144.95(18) . . . 3_666 ?
O2 P1 O3 K1 34.4(3) . . . 2_646 ?
O2 P1 C5 C2 -177.2(4) . . . . ?
O2 P1 C5 C3 63.1(5) . . . . ?
O2 P1 C5 C4 -58.3(5) . . . . ?
O3 P1 O1 K1 75.9(3) . . . . ?
O3 P1 O1 K1 -25.1(2) . . . 3_666 ?
O3 P1 C5 C2 64.1(4) . . . . ?
O3 P1 C5 C3 -55.6(5) . . . . ?
O3 P1 C5 C4 -177.1(4) . . . . ?
C5 P1 O1 K1 98.6(2) . . . 3_666 ?
C5 P1 O1 K1 -160.5(3) . . . . ?
C5 P1 O3 K1 150.5(3) . . . 2_646 ?
C5 P1 O3 K1 -98.9(2) . . . 3_666 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.796
_oxdiff_exptl_absorpt_empirical_full_min 0.618
####################################################################### 
# 
# 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_ak-242
_database_code_depnum_ccdc_archive 'CCDC 2330477'
loop_
_audit_author_name
_audit_author_address
'R Murugavel'
;IIT Bombay
India
;
_audit_update_record             
;
2024-02-02 deposited with the CCDC.	2024-07-30 downloaded from the CCDC.
;

# start Validation Reply Form
_vrf_PLAT043_ak-242              
;
PROBLEM: Calculated and Reported Mol. Weight Differ by ..       6.04 Check 
RESPONSE: 
H-atoms on the doubly coordinated water oxygen atoms (3 of them) were 
not identified or meaningfully fixed, which account for the 
difference of six H-atoms.

;
_audit_creation_date             2024-01-31
_audit_creation_method           
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C4 H11 Na2 O7 P'
_chemical_formula_sum            'C4 H17 Na2 O7 P'
_chemical_formula_weight         254.12
_chemical_melting_point          ?
_chemical_oxdiff_formula         C12H12O4PNa
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'
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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   14.5571(5)
_cell_length_b                   6.79238(16)
_cell_length_c                   13.4207(3)
_cell_angle_alpha                90
_cell_angle_beta                 104.188(3)
_cell_angle_gamma                90
_cell_volume                     1286.53(7)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    4288
_cell_measurement_temperature    100
_cell_measurement_theta_max      25.0480
_cell_measurement_theta_min      2.8650
_shelx_estimated_absorpt_T_max   0.958
_shelx_estimated_absorpt_T_min   0.802
_exptl_absorpt_coefficient_mu    0.288
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.40217
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.32a (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            colourless
_exptl_crystal_colour_lustre     .
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.312
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_preparation       0
_exptl_crystal_recrystallization_method ?
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0771
_diffrn_reflns_av_unetI/netI     0.0370
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            22368
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.887
_diffrn_ambient_temperature      100
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -104.00  21.00   1.00   10.00    --  -14.30 -57.00-180.00  125
  2  ω    -48.00  75.00   1.00   10.00    --  -14.30  38.00  90.00  123
  3  ω   -104.00  21.00   1.00   10.00    --  -14.30 -57.00 -90.00  125
  4  ω    -50.00  75.00   1.00   10.00    --  -14.30  57.00-150.00  125
  5  ω   -104.00  21.00   1.00   10.00    --  -14.30 -57.00  60.00  125
  6  ω    -53.00  73.00   1.00   10.00    --  -14.30  72.00   0.00  126
  7  ω    -50.00  75.00   1.00   10.00    --  -14.30  57.00 -90.00  125
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RCD3): Kappa single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0401327000
_diffrn_orient_matrix_UB_12      -0.0625222000
_diffrn_orient_matrix_UB_13      -0.0141136000
_diffrn_orient_matrix_UB_21      -0.0298987000
_diffrn_orient_matrix_UB_22      0.0801350000
_diffrn_orient_matrix_UB_23      0.0046633000
_diffrn_orient_matrix_UB_31      -0.0046684000
_diffrn_orient_matrix_UB_32      0.0239619000
_diffrn_orient_matrix_UB_33      -0.0524446000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          100
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2039
_reflns_number_total             2250
_reflns_odcompleteness_completeness 99.93
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.32a (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_refine_diff_density_max         0.765
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.123
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.110
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         2250
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.1029
_refine_ls_R_factor_gt           0.0953
_refine_ls_restrained_S_all      1.110
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.1414P)²+3.5181P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2483
_refine_ls_wR_factor_ref         0.2563
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2. Restrained distances
 O5-H5A
 0.88 with sigma of 0.02
3.a Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.25047(9) 0.75088(17) 0.42387(9) 0.0266(5) Uani 1 1 d . . . . .
Na1 Na 0.49724(13) 0.5562(3) 0.25468(13) 0.0315(6) Uani 1 1 d . . . . .
Na2 Na 0.3721(3) 0.2336(5) 0.4693(3) 0.0842(11) Uani 1 1 d . . . . .
O1 O 0.2565(3) 0.5423(5) 0.3712(3) 0.0341(9) Uani 1 1 d . . . . .
O2 O 0.2881(2) 0.7247(5) 0.5377(3) 0.0319(9) Uani 1 1 d . . . . .
O3 O 0.3019(2) 0.9006(5) 0.3738(2) 0.0314(8) Uani 1 1 d . . . . .
O4 O 0.5196(2) 0.3023(5) 0.3741(3) 0.0328(9) Uani 1 1 d . . . . .
O5 O 0.3205(3) 0.5012(6) 0.2021(3) 0.0346(9) Uani 1 1 d D . . . .
H5A H 0.317(4) 0.373(4) 0.187(5) 0.052 Uiso 1 1 d DR . . . .
H5B H 0.307(5) 0.565(10) 0.162(5) 0.052 Uiso 1 1 d R . . . .
O6 O 0.4834(2) 0.8143(5) 0.3611(2) 0.0314(8) Uani 1 1 d . . . . .
O7 O 0.6780(2) 0.5814(5) 0.3088(3) 0.0345(9) Uani 1 1 d . . . . .
C1 C 0.1256(4) 0.8116(8) 0.3944(4) 0.0336(12) Uani 1 1 d . . . . .
C2 C 0.0864(4) 0.8129(10) 0.2775(4) 0.0501(16) Uani 1 1 d . . . . .
H2A H 0.019202 0.849027 0.260985 0.075 Uiso 1 1 calc GR . . . .
H2B H 0.093472 0.681650 0.250019 0.075 Uiso 1 1 calc GR . . . .
H2C H 0.121560 0.908937 0.246800 0.075 Uiso 1 1 calc GR . . . .
C3 C 0.0724(4) 0.6578(10) 0.4423(5) 0.0513(15) Uani 1 1 d . . . . .
H3A H 0.004750 0.690092 0.425561 0.077 Uiso 1 1 calc GR . . . .
H3B H 0.097253 0.657520 0.517123 0.077 Uiso 1 1 calc GR . . . .
H3C H 0.081243 0.527279 0.414935 0.077 Uiso 1 1 calc GR . . . .
C4 C 0.1134(4) 1.0140(9) 0.4384(5) 0.0478(15) Uani 1 1 d . . . . .
H4A H 0.140354 1.013066 0.512822 0.072 Uiso 1 1 calc GR . . . .
H4B H 0.045819 1.046421 0.424039 0.072 Uiso 1 1 calc GR . . . .
H4C H 0.146175 1.112695 0.406485 0.072 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
P1 O1 1.596(3) . ?
P1 O2 1.502(4) . ?
P1 O3 1.514(3) . ?
P1 C1 1.811(5) . ?
Na1 Na1 3.40021(19) 2_655 ?
Na1 Na1 3.40016(19) 2_645 ?
Na1 Na2 3.990(4) 3_666 ?
Na1 Na2 4.112(4) 2_655 ?
Na1 O4 2.374(4) 2_655 ?
Na1 O4 2.323(4) . ?
Na1 O5 2.523(4) . ?
Na1 O6 2.325(4) 2_645 ?
Na1 O6 2.301(4) . ?
Na1 O7 2.558(4) . ?
Na2 O1 2.807(5) . ?
Na2 O3 2.676(5) 1_545 ?
Na2 O4 2.794(5) . ?
Na2 O6 2.713(5) 3_666 ?
O5 H5A 0.89(2) . ?
O5 H5B 0.68(7) . ?
C1 C2 1.533(7) . ?
C1 C3 1.532(8) . ?
C1 C4 1.523(7) . ?
C2 H2A 0.9800 . ?
C2 H2B 0.9800 . ?
C2 H2C 0.9800 . ?
C3 H3A 0.9800 . ?
C3 H3B 0.9800 . ?
C3 H3C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?

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 P1 C1 105.5(2) . . ?
O2 P1 O1 107.43(19) . . ?
O2 P1 O3 115.7(2) . . ?
O2 P1 C1 110.2(2) . . ?
O3 P1 O1 108.24(18) . . ?
O3 P1 C1 109.2(2) . . ?
Na1 Na1 Na1 174.44(12) 2_645 2_655 ?
Na1 Na1 Na2 112.42(9) 2_645 3_666 ?
Na1 Na1 Na2 70.19(7) 2_655 2_655 ?
Na1 Na1 Na2 70.53(7) 2_655 3_666 ?
Na1 Na1 Na2 104.26(9) 2_645 2_655 ?
Na2 Na1 Na2 111.92(8) 3_666 2_655 ?
O4 Na1 Na1 132.51(12) 2_655 2_645 ?
O4 Na1 Na1 43.02(9) 2_655 2_655 ?
O4 Na1 Na1 140.05(12) . 2_655 ?
O4 Na1 Na1 44.21(9) . 2_645 ?
O4 Na1 Na2 135.27(12) . 2_655 ?
O4 Na1 Na2 40.97(10) 2_655 2_655 ?
O4 Na1 Na2 70.77(10) . 3_666 ?
O4 Na1 Na2 111.39(11) 2_655 3_666 ?
O4 Na1 O4 175.96(12) . 2_655 ?
O4 Na1 O5 89.11(13) 2_655 . ?
O4 Na1 O5 92.51(13) . . ?
O4 Na1 O6 85.23(13) . 2_645 ?
O4 Na1 O7 94.32(13) 2_655 . ?
O4 Na1 O7 83.86(13) . . ?
O5 Na1 Na1 82.72(11) . 2_645 ?
O5 Na1 Na1 99.75(12) . 2_655 ?
O5 Na1 Na2 117.48(11) . 2_655 ?
O5 Na1 Na2 122.26(11) . 3_666 ?
O5 Na1 O7 175.30(14) . . ?
O6 Na1 Na1 132.32(12) 2_645 2_655 ?
O6 Na1 Na1 42.41(9) 2_645 2_645 ?
O6 Na1 Na1 142.22(12) . 2_645 ?
O6 Na1 Na1 42.97(9) . 2_655 ?
O6 Na1 Na2 64.22(10) 2_645 2_655 ?
O6 Na1 Na2 110.92(11) . 2_655 ?
O6 Na1 Na2 41.02(10) . 3_666 ?
O6 Na1 Na2 139.89(12) 2_645 3_666 ?
O6 Na1 O4 98.99(13) . . ?
O6 Na1 O4 84.62(12) . 2_655 ?
O6 Na1 O4 91.09(13) 2_645 2_655 ?
O6 Na1 O5 89.46(13) 2_645 . ?
O6 Na1 O5 92.76(13) . . ?
O6 Na1 O6 175.13(14) . 2_645 ?
O6 Na1 O7 87.27(13) 2_645 . ?
O6 Na1 O7 90.76(13) . . ?
O7 Na1 Na1 84.95(10) . 2_655 ?
O7 Na1 Na1 92.59(11) . 2_645 ?
O7 Na1 Na2 63.92(10) . 2_655 ?
O7 Na1 Na2 59.30(10) . 3_666 ?
Na1 Na2 Na1 125.66(10) 3_666 2_645 ?
O1 Na2 Na1 105.25(12) . 3_666 ?
O1 Na2 Na1 101.96(12) . 2_645 ?
O3 Na2 Na1 65.99(10) 1_545 2_645 ?
O3 Na2 Na1 141.83(14) 1_545 3_666 ?
O3 Na2 O1 106.96(15) 1_545 . ?
O3 Na2 O4 99.70(15) 1_545 . ?
O3 Na2 O6 115.28(16) 1_545 3_666 ?
O4 Na2 Na1 33.86(8) . 2_645 ?
O4 Na2 Na1 96.90(12) . 3_666 ?
O4 Na2 O1 95.74(15) . . ?
O6 Na2 Na1 100.14(12) 3_666 2_645 ?
O6 Na2 Na1 33.82(8) 3_666 3_666 ?
O6 Na2 O1 137.37(16) 3_666 . ?
O6 Na2 O4 83.08(14) 3_666 . ?
P1 O1 Na2 123.18(19) . . ?
P1 O3 Na2 121.86(19) . 1_565 ?
Na1 O4 Na1 92.77(12) . 2_645 ?
Na1 O4 Na2 105.17(15) 2_645 . ?
Na1 O4 Na2 116.51(16) . . ?
Na1 O5 H5A 102(4) . . ?
Na1 O5 H5B 102(6) . . ?
H5A O5 H5B 117(7) . . ?
Na1 O6 Na1 94.61(12) . 2_655 ?
Na1 O6 Na2 105.16(15) . 3_666 ?
Na1 O6 Na2 116.70(16) 2_655 3_666 ?
C2 C1 P1 109.0(4) . . ?
C3 C1 P1 109.7(4) . . ?
C3 C1 C2 109.5(5) . . ?
C4 C1 P1 109.1(4) . . ?
C4 C1 C2 110.0(5) . . ?
C4 C1 C3 109.6(5) . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
C1 C3 H3A 109.5 . . ?
C1 C3 H3B 109.5 . . ?
C1 C3 H3C 109.5 . . ?
H3A C3 H3B 109.5 . . ?
H3A C3 H3C 109.5 . . ?
H3B C3 H3C 109.5 . . ?
C1 C4 H4A 109.5 . . ?
C1 C4 H4B 109.5 . . ?
C1 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?

loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O5 H5A O7 0.89(2) 1.98(3) 2.856(5) 166(6) 2_645 yes
O5 H5B O2 0.68(7) 2.16(7) 2.837(5) 171(8) 4_575 yes

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
O1 P1 O3 Na2 -156.8(2) . . . 1_565 ?
O1 P1 C1 C2 -57.6(4) . . . . ?
O1 P1 C1 C3 62.3(4) . . . . ?
O1 P1 C1 C4 -177.7(4) . . . . ?
O2 P1 O1 Na2 -18.5(3) . . . . ?
O2 P1 O3 Na2 -36.2(3) . . . 1_565 ?
O2 P1 C1 C2 -173.2(4) . . . . ?
O2 P1 C1 C3 -53.3(4) . . . . ?
O2 P1 C1 C4 66.6(4) . . . . ?
O3 P1 O1 Na2 107.1(2) . . . . ?
O3 P1 C1 C2 58.6(4) . . . . ?
O3 P1 C1 C3 178.5(4) . . . . ?
O3 P1 C1 C4 -61.5(4) . . . . ?
C1 P1 O1 Na2 -136.1(2) . . . . ?
C1 P1 O3 Na2 88.8(3) . . . 1_565 ?

_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.919
_oxdiff_exptl_absorpt_empirical_full_min 0.562
