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_7718734
_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         'C5 H11 O4 P, H2 O, C H4 O, 2(C6 H14 N)'
_chemical_formula_sum            'C18 H45 N2 O6 P'
_chemical_formula_weight         416.54
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2022-05-09
_audit_creation_method
;
Olex2 1.3-ac4
(compiled 2019.04.23 svn.r3594 for Rigaku Oxford Diffraction, GUI svn.r5739)
;
_audit_update_record
;
2024-10-08 deposited with the CCDC.	2025-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.490(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4547(10)
_cell_length_b                   6.4842(3)
_cell_length_c                   25.2056(17)
_cell_measurement_reflns_used    1525
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      20.5310
_cell_measurement_theta_min      2.7150
_cell_volume                     2445.5(3)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_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     -9.73 182.27   1.20   10.00  13.56  -2.89 -31.50    --   160
  2  \w    -38.66  22.54   1.20   10.00    --   -2.89 -59.25  92.08   51
;
_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      0.0048250000
_diffrn_orient_matrix_UB_12      -0.0079656000
_diffrn_orient_matrix_UB_13      -0.0271977000
_diffrn_orient_matrix_UB_21      0.0460257000
_diffrn_orient_matrix_UB_22      -0.0225476000
_diffrn_orient_matrix_UB_23      0.0102801000
_diffrn_orient_matrix_UB_31      -0.0101311000
_diffrn_orient_matrix_UB_32      -0.1067410000
_diffrn_orient_matrix_UB_33      -0.0001347000
_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  0.0978
_diffrn_reflns_av_unetI/netI     0.1246
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            23318
_diffrn_reflns_theta_full        24.9995
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.144
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91191
_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            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.1313
_exptl_crystal_description       plate
_exptl_crystal_F_000             920.8709
_exptl_crystal_size_max          0.188
_exptl_crystal_size_mid          0.159
_exptl_crystal_size_min          0.098
_refine_diff_density_max         0.9069
_refine_diff_density_min         -0.8718
_refine_diff_density_rms         0.0999
_refine_ls_d_res_high            0.8409
_refine_ls_d_res_low             11.5348
_refine_ls_goodness_of_fit_ref   1.0398
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    66
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4297
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0398
_refine_ls_R_factor_all          0.1067
_refine_ls_R_factor_gt           0.0729
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0700P)^2^+4.3823P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1695
_refine_ls_wR_factor_ref         0.1941
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -18
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -12
_reflns_number_gt                3027
_reflns_number_total             4297
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt00255a2.cif
_cod_data_source_block           RM_AK_NEOPENTYL_PHOSPHATE_autored
_cod_depositor_comments
'Adding full bibliography for 7718729--7718735.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               7718734
_reflns_odcompleteness_completeness 80.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.48
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H,H,H) groups
 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:
 O5(H5d,H5e)
2.b Ternary CH refined with riding coordinates:
 C12(H12), C6(H6)
2.c Secondary CH2 refined with riding coordinates:
 C1(H1a,H1b), C13(H13a,H13b), C14(H14a,H14b), C15(H15a,H15b), C16(H16a,H16b),
 C17(H17a,H17b), C7(H7a,H7b), C8(H8a,H8b), C9(H9a,H9b), C10(H10a,H10b),
 C11(H11a,H11b)
2.d Idealised Me refined as rotating group:
 C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C5(H5a,H5b,H5c), C18(H18a,H18b,H18c),
 N1(H1c,H1d,H1e), N2(H2a,H2b,H2c)
2.e Idealised tetrahedral OH refined as rotating group:
 O6(H6a)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.145
_oxdiff_exptl_absorpt_empirical_full_min 0.846