Synthesis, supramolecular organization and thermotropic phase behaviour of N-acyltris(hydroxymethyl)aminomethane
Megarajan, Sengan; Subramaniyan, Siva Bala; Muthuswamy, Sureshan; Anthony, Savarimuthu Philip; Arunachalam, Jothi; Moon, Dohyun; Veerappan, Anbazhagan; RSC Advances 8 (2018) 32823–; doi:10.1039/C8RA06479B

data_7231549
_publ_section_title
;
 Synthesis, supramolecular organization and thermotropic phase behaviour
 of N-acyltris(hydroxymethyl)aminomethane
;
_journal_issue                   57
_journal_name_full               'RSC Advances'
_journal_page_first              32823
_journal_paper_doi               10.1039/C8RA06479B
_journal_volume                  8
_journal_year                    2018
_chemical_formula_moiety         'C16 H33 N O4'
_chemical_formula_sum            'C16 H33 N O4'
_chemical_formula_weight         303.43
_chemical_name_systematic        N12TM
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2018-03-23 deposited with the CCDC.
2018-09-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.41(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.076(5)
_cell_length_b                   8.6760(17)
_cell_length_c                   9.0510(18)
_cell_measurement_reflns_used    39791
_cell_measurement_temperature    284(2)
_cell_measurement_theta_max      33.679
_cell_measurement_theta_min      0.350
_cell_volume                     1811.5(6)
_computing_cell_refinement       '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_data_collection
'<i>PAL BL2D-SMDC Program</i>(Shin et. al, 2016)'
_computing_data_reduction        '<i>HKL3000sm</i>(Otwinowski & Minor, 1997)'
_computing_molecular_graphics    '<i>DIAMOND 4</i>(Putz & Brandenburg, 2014)'
_computing_publication_material  '<i>enCifer 1.6</i>'
_computing_structure_refinement  '<i>SHELXL-2017</i> (Sheldrick, 2015)'
_computing_structure_solution    '<i>SHELXT-2014</i> (Sheldrick, 2015)'
_diffrn_ambient_temperature      284(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.953
_diffrn_measurement_device_type  'ADSC Q210 CCD area detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.610
_diffrn_reflns_av_R_equivalents  0.0453
_diffrn_reflns_av_unetI/netI     0.0417
_diffrn_reflns_Laue_measured_fraction_full 0.963
_diffrn_reflns_Laue_measured_fraction_max 0.953
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            16669
_diffrn_reflns_point_group_measured_fraction_full 0.963
_diffrn_reflns_point_group_measured_fraction_max 0.953
_diffrn_reflns_theta_full        21.469
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.792
_diffrn_source                   'PLSII 2D bending magnet'
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.948
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
'<i>HKL3000sm Scalepack(Otwinowski & Minor, 1997)</i>'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.113
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.125
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.010
_refine_diff_density_max         0.345
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.136(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     195
_refine_ls_number_reflns         4799
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0688
_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^)+(0.1155P)^2^+0.6033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2175
_refine_ls_wR_factor_ref         0.2292
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3346
_reflns_number_total             4799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8ra06479b2.cif
_cod_data_source_block           SPA245
_cod_database_code               7231549
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_min   0.993
_shelx_estimated_absorpt_t_max   0.999
_shelx_res_checksum              85640