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_7718731
_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_absolute_configuration unk
_chemical_formula_moiety         'C2 H4 F3 O4 P'
_chemical_formula_sum            'C2 H4 F3 O4 P'
_chemical_formula_weight         180.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-07
_audit_creation_method
;
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                90
_cell_angle_beta                 97.992(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   4.5644(7)
_cell_length_b                   5.0754(9)
_cell_length_c                   13.312(2)
_cell_measurement_reflns_used    2418
_cell_measurement_temperature    107(5)
_cell_measurement_theta_max      28.3470
_cell_measurement_theta_min      3.0680
_cell_volume                     305.39(9)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-ac6-016 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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   -339.92  20.08   1.00    5.00  15.81  -9.84 -59.25    --   360
  2  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56 145.16   65
  3  \w    -60.89   0.11   1.00    5.00    --  -14.77  94.56 -34.84   61
  4  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 164.08  116
  5  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 -51.92  116
  6  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56   1.16   65
  7  \f   -349.73  10.27   1.00    5.00   6.61  -9.84 -31.50    --   360
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'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      0.0493502000
_diffrn_orient_matrix_UB_12      0.0507182000
_diffrn_orient_matrix_UB_13      -0.0443625000
_diffrn_orient_matrix_UB_21      -0.1037326000
_diffrn_orient_matrix_UB_22      0.1044106000
_diffrn_orient_matrix_UB_23      -0.0010483000
_diffrn_orient_matrix_UB_31      0.1070308000
_diffrn_orient_matrix_UB_32      0.0777601000
_diffrn_orient_matrix_UB_33      0.0304046000
_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  0.0994
_diffrn_reflns_av_unetI/netI     0.0478
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9819
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.995
_diffrn_reflns_theta_max         24.995
_diffrn_reflns_theta_min         1.545
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.472
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80883
_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    1.958
_exptl_crystal_description       plate
_exptl_crystal_F_000             180
_exptl_crystal_size_max          0.389
_exptl_crystal_size_mid          0.111
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.753
_refine_diff_density_min         -0.401
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details
;
 Flack x determined using 388 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.14(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.170
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         1069
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0551
_refine_ls_R_factor_gt           0.0505
_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^)+(0.0696P)^2^+0.2466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1295
_refine_ls_wR_factor_ref         0.1329
_reflns_Friedel_coverage         0.776
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                999
_reflns_number_total             1069
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00255a2.cif
_cod_data_source_block           rm_ak_629_autored
_cod_depositor_comments
'Adding full bibliography for 7718729--7718735.cif.'
_cod_original_cell_volume        305.38(9)
_cod_database_code               7718731
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.838
_reflns_odcompleteness_completeness 83.32
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     36.82
_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.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B)
2.b Idealised tetrahedral OH refined as rotating group:
 O4(H4)
;
_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 1.611
_oxdiff_exptl_absorpt_empirical_full_min 0.711