1D polymeric and 2D layered zinc monoalkyl phosphates bearing long alkyl chains: synthesis, structural transformations and thermal behaviour.
Arya, Harsha; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 54 (2025) 11232–11245; doi:10.1039/d5dt00783f

data_7718958
_publ_section_title
;
 1D polymeric and 2D layered zinc monoalkyl phosphates bearing long alkyl
 chains: synthesis, structural transformations and thermal behaviour.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11232
_journal_page_last               11245
_journal_paper_doi               10.1039/d5dt00783f
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C11 H24 N O5 P Zn'
_chemical_formula_sum            'C11 H24 N O5 P Zn'
_chemical_formula_weight         346.65
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                85.187(2)
_cell_angle_beta                 82.270(2)
_cell_angle_gamma                82.405(3)
_cell_formula_units_Z            2
_cell_length_a                   5.4254(2)
_cell_length_b                   9.4114(3)
_cell_length_c                   15.2643(4)
_cell_measurement_reflns_used    12172
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.9180
_cell_measurement_theta_min      2.1900
_cell_volume                     763.81(4)
_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 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (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      150.00(10)
_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   -339.92  20.08   1.00    5.00  15.81  -9.84 -59.25    --   360
  2  \w    -60.89   0.11   1.00    5.00    --  -14.77  94.56 -34.84   61
  3  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56 145.16   65
  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  20.08  116
  6  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56   1.16   65
  7  \w    -65.46  -0.46   1.00    5.00    --  -19.34  94.56  73.16   65
  8  \f   -349.73  10.27   1.00    5.00   6.61  -9.84 -31.50    --   360
  9  \w   -100.81  15.19   1.00    5.00    --   -9.84 -59.25 -51.92  116
;
_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      0.0209654000
_diffrn_orient_matrix_UB_12      0.0221645000
_diffrn_orient_matrix_UB_13      -0.0456770000
_diffrn_orient_matrix_UB_21      0.1193514000
_diffrn_orient_matrix_UB_22      -0.0416806000
_diffrn_orient_matrix_UB_23      -0.0033518000
_diffrn_orient_matrix_UB_31      -0.0546575000
_diffrn_orient_matrix_UB_32      -0.0598235000
_diffrn_orient_matrix_UB_33      -0.0105570000
_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  0.0531
_diffrn_reflns_av_unetI/netI     0.0234
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            28102
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.188
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.726
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.45702
_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_density_diffrn    1.507
_exptl_crystal_description       plate
_exptl_crystal_F_000             364
_exptl_crystal_size_max          0.62
_exptl_crystal_size_mid          0.154
_exptl_crystal_size_min          0.026
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     175
_refine_ls_number_reflns         2700
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0292
_refine_ls_R_factor_gt           0.0272
_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^)+(0.0304P)^2^+0.9525P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0670
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2558
_reflns_number_total             2700
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00783f2.cif
_cod_data_source_block           rm_ha_62
_cod_depositor_comments
'Adding full bibliography for 7718958--7718959.cif.'
_cod_database_code               7718958
_shelx_shelxl_version_number     2018/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C1(H1A,H1B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C5(H5A,H5B),
 C7(H7A,H7B)
2.b Aromatic/amide H refined with riding coordinates:
 C9(H9)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C10(H10A,H10B,H10C), C8(H8A,H8B,H8C)
;
_shelx_res_checksum              36667
_shelx_hkl_checksum              65748
_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 2.214
_oxdiff_exptl_absorpt_empirical_full_min 0.462