Plastic phase transitions in tris(hydroxymethyl)aminomethane perchlorate.
Zhou, Feng; Weng, Yan-Ran; Shi, Yu; Yu, Yun-Hui; Lu, Dan; Yu, Yong; She, Jia-Zi; Ai, Yong; Dalton transactions (Cambridge, England : 2003) 53 (2024) 7965–7970; doi:10.1039/d4dt00791c

data_7715784
_publ_section_title
;
 Plastic phase transitions in tris(hydroxymethyl)aminomethane perchlorate.
;
_journal_issue                   18
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7965
_journal_page_last               7970
_journal_paper_doi               10.1039/d4dt00791c
_journal_volume                  53
_journal_year                    2024
_chemical_formula_moiety         'Cl1 O4, C4 H12 N1 O3'
_chemical_formula_sum            'C4 H12 Cl N O7'
_chemical_formula_weight         221.60
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2023-12-11
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-12-26 deposited with the CCDC.	2024-04-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   8.0483(2)
_cell_length_b                   8.0483(2)
_cell_length_c                   23.8037(5)
_cell_measurement_reflns_used    1214
_cell_measurement_temperature    299.98(10)
_cell_measurement_theta_max      74.1390
_cell_measurement_theta_min      5.5570
_cell_volume                     1335.31(5)
_computing_cell_refinement       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.79a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      299.98(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     86.00 114.00   0.50    0.50    --  108.36 125.00 120.00   56
  2  \w    131.00 178.00   0.50    0.50    --  108.36 125.00 120.00   94
  3  \w     35.00  92.00   0.50    0.50    --  108.36 -77.00 -90.00  114
  4  \w     47.00  72.00   0.50    0.50    --  108.36 -61.00 -60.00   50
  5  \w    -32.00  12.00   0.50    1.00    --   45.20 -19.00-180.00   88
  6  \w    -23.00  28.00   0.50    1.00    --   45.20 -18.00  48.00  102
  7  \w    -18.00   7.00   0.50    1.00    --  -45.20  18.00-143.00   50
  8  \w    -67.00 -28.00   0.50    0.50    -- -102.00  61.00 138.00   78
  9  \w   -174.00 -96.00   0.50    0.50    -- -102.00 -37.00   4.00  156
 10  \w   -167.00-107.00   0.50    0.50    -- -102.00-107.00 -82.00  120
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0786183000
_diffrn_orient_matrix_UB_12      -0.0522211000
_diffrn_orient_matrix_UB_13      0.0519744000
_diffrn_orient_matrix_UB_21      0.0217157000
_diffrn_orient_matrix_UB_22      -0.1490111000
_diffrn_orient_matrix_UB_23      -0.0350115000
_diffrn_orient_matrix_UB_31      0.2054552000
_diffrn_orient_matrix_UB_32      0.1546306000
_diffrn_orient_matrix_UB_33      -0.0161773000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0105
_diffrn_reflns_av_unetI/netI     0.0085
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            1186
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.330
_diffrn_reflns_theta_min         5.576
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.003
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38407
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.79a (Rigaku Oxford Diffraction, 2022)
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    1.653
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.478
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.083
_refine_ls_extinction_coef       0.023(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     43
_refine_ls_number_reflns         584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0547
_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^)+(0.0826P)^2^+5.7118P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1439
_refine_ls_wR_factor_ref         0.1439
_reflns_Friedel_coverage         0.000
_reflns_number_gt                582
_reflns_number_total             584
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt00791c2.cif
_cod_data_source_block           zf231125-1-300k_auto
_cod_depositor_comments          'Adding full bibliography for 7715784.cif.'
_cod_original_cell_volume        1335.31(7)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               7715784
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C H N O Cl'
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.380
_reflns_odcompleteness_completeness 98.87
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups, All N(H,H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Others
 Fixed Sof: H1C(0.33333) H1B(0.33333) H1A(0.33333)
3.a Secondary CH2 refined with riding coordinates:
 C005(H00A,H00B)
3.b Idealised Me refined as rotating group:
 N1(H1C,H1B,H1A)
3.c Idealised tetrahedral OH refined as rotating group:
 O002(H002)
;
_shelx_res_checksum              78193
_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 1.509
_oxdiff_exptl_absorpt_empirical_full_min 0.626