Thermally labile mono-alkyl phosphates and their alkali metal derivatives: synthesis and solid-state supramolecular aggregation.
Kumar, Anuj; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 54 (2025) 10691–10709; doi:10.1039/d5dt00255a

data_7718735
_publ_section_title
;
 Thermally labile mono-alkyl phosphates and their alkali metal
 derivatives: synthesis and solid-state supramolecular aggregation.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10691
_journal_page_last               10709
_journal_paper_doi               10.1039/d5dt00255a
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C6 H9 F9 Li3 O12 P3'
_chemical_formula_sum            'C6 H9 F9 Li3 O12 P3'
_chemical_formula_weight         557.86
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
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;
Olex2 1.5-ac6-016
(compiled 2024.01.13 svn.r2f8d729c for Rigaku Oxford Diffraction, GUI svn.r6897)
;
_audit_update_record
;
2024-10-08 deposited with the CCDC.	2025-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                103.790(8)
_cell_angle_beta                 90.794(6)
_cell_angle_gamma                115.729(8)
_cell_formula_units_Z            2
_cell_length_a                   8.0883(5)
_cell_length_b                   8.7705(8)
_cell_length_c                   14.5790(13)
_cell_measurement_reflns_used    2722
_cell_measurement_temperature    150
_cell_measurement_theta_max      22.4310
_cell_measurement_theta_min      3.7530
_cell_volume                     896.65(15)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
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_computing_structure_solution
'olex2.solve 1.5-ac6-016 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_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  t~exp~   \w     \q     \k     \f   Frames
  1  \f   -349.73  10.27   1.00    5.00   6.61  -9.84 -31.50    --   360
  2  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56 145.16   65
  3  \w    -60.88   0.12   1.00    5.00    --  -14.77  94.56 -34.84   61
  4  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25  20.08  116
  5  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 164.08  116
  6  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56  73.16   65
  7  \f   -339.92  20.08   1.00    5.00  15.81  -9.84 -59.25    --   360
  8  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56   1.16   65
  9  \w    -97.81  15.19   1.00    5.00    --   -9.84 -59.25-123.92  113
;
_diffrn_measurement_device       'abstract diffractometer'
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'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0569766000
_diffrn_orient_matrix_UB_12      -0.0097558000
_diffrn_orient_matrix_UB_13      0.0332919000
_diffrn_orient_matrix_UB_21      0.0293374000
_diffrn_orient_matrix_UB_22      -0.0455032000
_diffrn_orient_matrix_UB_23      -0.0380111000
_diffrn_orient_matrix_UB_31      0.0744490000
_diffrn_orient_matrix_UB_32      0.0808322000
_diffrn_orient_matrix_UB_33      -0.0015536000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1300
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            32220
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.678
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.483
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58471
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.066
_exptl_crystal_description       block
_exptl_crystal_F_000             552
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.144
_refine_diff_density_max         0.511
_refine_diff_density_min         -0.577
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
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_refine_ls_number_reflns         3166
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0969
_refine_ls_R_factor_gt           0.0580
_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/[\s^2^(Fo^2^)+(0.0781P)^2^+0.3360P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1605
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2136
_reflns_number_total             3166
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00255a2.cif
_cod_data_source_block           rm_ak_491_autored
_cod_depositor_comments
'Adding full bibliography for 7718729--7718735.cif.'
_cod_original_cell_volume        896.65(14)
_cod_database_code               7718735
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.934
_shelx_estimated_absorpt_t_min   0.858
_reflns_odcompleteness_completeness 80.37
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.64
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H14-O14
 0.84 with sigma of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C11(H11A,H11B), C21(H21A,H21B)
3.b Idealised tetrahedral OH refined as rotating group:
 O4(H4), O24(H24)
;
_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 1.557
_oxdiff_exptl_absorpt_empirical_full_min 0.599