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_7718959
_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         'C9 H20 N O5 P Zn'
_chemical_formula_sum            'C9 H20 N O5 P Zn'
_chemical_formula_weight         318.60
_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     iterative
_audit_creation_date             2023-09-09
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2024-04-23 deposited with the CCDC.	2025-06-23 downloaded from the CCDC.
;
_cell_angle_alpha                83.203(3)
_cell_angle_beta                 88.754(3)
_cell_angle_gamma                82.318(3)
_cell_formula_units_Z            2
_cell_length_a                   5.4197(2)
_cell_length_b                   9.3778(4)
_cell_length_c                   13.3722(5)
_cell_measurement_reflns_used    12123
_cell_measurement_temperature    107(4)
_cell_measurement_theta_max      32.2460
_cell_measurement_theta_min      2.1950
_cell_volume                     668.79(5)
_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    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      107(4)
_diffrn_detector                 'CCD plate'
_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    -10.27 349.73   1.50    8.00  77.88 -12.98  31.50    --   240
  2  \w    -65.46  -0.96   1.50    8.00    --  -15.96  94.56-142.84   43
  3  \w    -65.46  -0.96   1.50    8.00    --  -15.96  94.56   1.16   43
  4  \w    -65.46  -0.96   1.50    8.00    --  -15.96  94.56  73.16   43
  5  \w   -108.63  15.87   1.50    8.00    --  -12.98 -59.25  71.08   83
  6  \f   -349.73  10.27   1.50    8.00   9.41 -12.98 -31.50    --   240
  7  \w   -108.63  15.87   1.50    8.00    --  -12.98 -59.25 -84.92   83
  8  \f   -339.52  20.33   1.50    8.00  16.12 -12.98 -59.25    --   240
;
_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      0.0237023000
_diffrn_orient_matrix_UB_12      -0.0705682000
_diffrn_orient_matrix_UB_13      -0.0151159000
_diffrn_orient_matrix_UB_21      -0.0791130000
_diffrn_orient_matrix_UB_22      0.0224845000
_diffrn_orient_matrix_UB_23      -0.0420753000
_diffrn_orient_matrix_UB_31      0.1030529000
_diffrn_orient_matrix_UB_32      0.0204868000
_diffrn_orient_matrix_UB_33      -0.0292368000
_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  0.0465
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_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       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            25008
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.206
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.964
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.36075
_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 whiteish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   whiteish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.582
_exptl_crystal_description       plate
_exptl_crystal_F_000             332
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.103
_exptl_crystal_size_min          0.095
_refine_diff_density_max         0.337
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     157
_refine_ls_number_reflns         2358
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0235
_refine_ls_R_factor_gt           0.0225
_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/[\s^2^(Fo^2^)+(0.0186P)^2^+0.6526P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0516
_refine_ls_wR_factor_ref         0.0520
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2273
_reflns_number_total             2358
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00783f2.cif
_cod_data_source_block           rm_ha_61_autored
_cod_depositor_comments
'Adding full bibliography for 7718958--7718959.cif.'
_cod_database_code               7718959
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.835
_shelx_estimated_absorpt_t_min   0.388
_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:
 C3(H3A,H3B), C1(H1A,H1B), C2(H2A,H2B), C4(H4A,H4B), C5(H5A,H5B)
2.b Aromatic/amide H refined with riding coordinates:
 C7(H7)
2.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C)
;
_shelx_res_checksum              76665
_shelx_hkl_checksum              9401
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.816
_oxdiff_exptl_absorpt_empirical_full_min 0.591