Packing polymorphism, odd–even alternation and thermotropic phase transitions in N-,O-diacylethanolamines with varying N-acyl chains. A combined experimental and computational study
Reddy, Soudherpally Thirupathi; Sivaramakrishna, Dokku; Mamatha, Keerthi; Sharma, Manju; Swamy, Musti J.; Physical Chemistry Chemical Physics  (2021) –; doi:10.1039/D1CP03704H

data_7243848
_publ_section_title
;
 Packing polymorphism, odd--even alternation and thermotropic phase
 transitions in N-,O-diacylethanolamines with varying N-acyl chains. A
 combined experimental and computational study
;
_journal_name_full               'Physical Chemistry Chemical Physics'
_journal_paper_doi               10.1039/D1CP03704H
_journal_year                    2021
_chemical_formula_moiety         'C30 H59 N O3'
_chemical_formula_sum            'C30 H59 N O3'
_chemical_formula_weight         481.81
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2020-05-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-10-27 deposited with the CCDC.	2021-10-20 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 92.787(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   68.97(4)
_cell_length_b                   4.852(3)
_cell_length_c                   8.906(5)
_cell_measurement_reflns_used    6874
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.35
_cell_measurement_theta_min      2.66
_cell_volume                     2977(3)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.970
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0958
_diffrn_reflns_av_unetI/netI     0.0691
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.970
_diffrn_reflns_limit_h_max       81
_diffrn_reflns_limit_h_min       -81
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            23859
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.970
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         1.182
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.075
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.311
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5094
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.1929
_refine_ls_R_factor_gt           0.1433
_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^)+(0.0722P)^2^+12.1404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2996
_refine_ls_wR_factor_ref         0.3252
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3256
_reflns_number_total             5094
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1cp03704h2.cif
_cod_data_source_block           nlopb
_cod_depositor_comments
;

2025-01-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         32.12
_cod_original_formula_moiety         '0.07(C30 H59 N O3)'
_cod_original_formula_units_Z            60
_cod_original_formula_sum        'C2 H3.93 N0.07 O0.20'
_cod_database_code               7243848
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.993
_shelx_estimated_absorpt_t_min   0.980
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C11(H11A,H11B), C26(H26A,H26B), C24(H24A,H24B), C19(H19A,
 H19B), C23(H23A,H23B), C18(H18A,H18B), C25(H25A,H25B), C20(H20A,H20B), C5(H5A,
 H5B), C6(H6A,H6B), C22(H22A,H22B), C9(H9A,H9B), C8(H8A,H8B), C7(H7A,H7B),
 C17(H17A,H17B), C3(H3A,H3B), C16(H16A,H16B), C10(H10A,H10B), C4(H4A,H4B),
 C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C2(H2A,H2B), C13(H13A,H13B),
 C14(H14A,H14B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              14126
_olex2_submission_special_instructions 'No special instructions were received'