Direct <i>in situ</i> measurement of polymorphic transition temperatures under thermo-mechanochemical conditions.
Alić, Jasna; Lončarić, Ivor; Etter, Martin; Rubčić, Mirta; Štefanić, Zoran; Šekutor, Marina; Užarević, Krunoslav; Stolar, Tomislav; Physical chemistry chemical physics : PCCP 26 (2024) 4840–4844; doi:10.1039/d3cp04364a

data_7248039
_publ_section_title
;
 Direct <i>in situ</i> measurement of polymorphic transition temperatures
 under thermo-mechanochemical conditions.
;
_journal_issue                   6
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              4840
_journal_page_last               4844
_journal_paper_doi               10.1039/d3cp04364a
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C24 H34 O'
_chemical_formula_sum            'C24 H34 O'
_chemical_formula_weight         338.51
_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
_audit_creation_date             2023-06-15
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2023-06-15 deposited with the CCDC.	2024-01-03 downloaded from the CCDC.
;
_cell_angle_alpha                76.757(4)
_cell_angle_beta                 84.981(4)
_cell_angle_gamma                78.050(5)
_cell_formula_units_Z            2
_cell_length_a                   7.7886(5)
_cell_length_b                   10.8558(5)
_cell_length_c                   11.3845(4)
_cell_measurement_reflns_used    6542
_cell_measurement_temperature    296.69(13)
_cell_measurement_theta_max      78.7960
_cell_measurement_theta_min      5.0110
_cell_volume                     915.86(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.54a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      296.69(13)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.940
_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    -65.00 -38.00   0.50    1.20    --  -48.47 -30.00  21.00   54
  2  \w   -122.00 -71.00   0.50    1.20    --  -48.47 -30.00  21.00  102
  3  \w    -25.00  25.00   0.50    1.20    --  -48.47  30.00-177.00  100
  4  \w    -24.00  28.00   0.50    1.20    --   48.47 -30.00  21.00  104
  5  \w   -117.00 -91.00   0.50    4.81    --  -90.00 -30.00  21.00   52
  6  \w   -163.00-124.00   0.50    4.81    --  -90.00 -30.00  21.00   78
  7  \w    -42.00 -16.00   0.50    1.20    --  -48.47 125.00 150.00   52
  8  \w    -25.00  20.00   0.50    1.20    --  -48.47  19.00 -30.00   90
  9  \w    -25.00  19.00   0.50    1.20    --  -48.47  19.00 -90.00   88
 10  \w    -82.00 -49.00   0.50    1.20    --  -48.47 125.00 150.00   66
 11  \w   -115.00 -90.00   0.50    1.20    --  -48.47-125.00-180.00   50
 12  \w     52.00  96.00   0.50    1.20    --   48.47  30.00-177.00   88
 13  \w    -52.00 -21.00   0.50    4.81    --  -90.00 125.00-180.00   62
 14  \w    -62.00 -19.00   0.50    4.81    --  -90.00 125.00-120.00   86
 15  \w    -52.00 -18.00   0.50    4.81    --  -90.00 125.00  30.00   68
 16  \w   -161.00-122.00   0.50    4.81    --  -90.00 -45.00   0.00   78
 17  \w    -85.00 -34.00   0.50    4.81    --  -90.00 125.00  60.00  102
 18  \w    -82.00 -55.00   0.50    4.81    --  -90.00 125.00-180.00   54
 19  \w    -52.00 -26.00   0.50    4.81    --  -90.00  77.00   0.00   52
 20  \w   -161.00 -79.00   0.50    4.81    --  -90.00 -45.00 -30.00  164
 21  \w    -86.00 -60.00   0.50    4.81    --  -90.00  77.00   0.00   52
 22  \w   -105.00 -80.00   0.50    4.81    --  -90.00 -45.00   0.00   50
 23  \w     47.00  73.00   0.50    4.81    --  111.50-125.00-120.00   52
 24  \w     72.00  98.00   0.50    4.81    --  111.50-125.00   0.00   52
 25  \w     72.00  97.00   0.50    4.81    --  111.50 -95.00 -90.00   50
 26  \w     40.00  70.00   0.50    4.81    --  111.50-125.00   0.00   60
 27  \w     40.00  66.00   0.50    4.81    --  111.50 -95.00 -90.00   52
 28  \w    100.00 134.00   0.50    4.81    --  111.50 125.00   0.00   68
 29  \w     42.00 101.00   0.50    4.81    --  111.50-125.00  90.00  118
 30  \w     43.00  68.00   0.50    4.81    --  111.50 -61.00-180.00   50
 31  \w     93.00 128.00   0.50    4.81    --  111.50  77.00  60.00   70
 32  \w    148.00 177.00   0.50    4.81    --  111.50  77.00  60.00   58
 33  \w     50.00 111.00   0.50    4.81    --  111.50-125.00 150.00  122
 34  \w    134.00 169.00   0.50    4.81    --  111.50  61.00 -90.00   70
 35  \w     45.00  70.00   0.50    4.81    --  111.50 -61.00 150.00   50
 36  \w     97.00 125.00   0.50    4.81    --  111.50  61.00 -90.00   56
 37  \w     78.00 104.00   0.50    4.81    --  111.50 -77.00 120.00   52
 38  \w     82.00 110.00   0.50    4.81    --  111.50-125.00-120.00   56
 39  \w     48.00 111.00   0.50    4.81    --  111.50-125.00  60.00  126
 40  \w     40.00 109.00   0.50    4.81    --  111.50-125.00-180.00  138
 41  \w     69.00  95.00   0.50    4.81    --  111.50 -77.00  60.00   52
 42  \w     44.00 105.00   0.50    4.81    --  111.50 -95.00-120.00  122
 43  \w     51.00 111.00   0.50    4.81    --  111.50-125.00  30.00  120
 44  \w    102.00 178.00   0.50    4.81    --  111.50  30.00-177.00  152
 45  \w   -124.00 -98.00   0.50    4.81    --  -90.00 -32.00  22.00   52
 46  \w    -23.00   9.00   0.50    1.20    --   48.47 -19.00 -90.00   64
 47  \w      2.00  28.00   0.50    1.20    --   48.47 -99.00-180.00   52
 48  \w     40.00  81.00   0.50    1.20    --   48.47 -99.00-180.00   82
 49  \w    -51.00 -26.00   0.50    4.81    --  -90.00  45.00 150.00   50
 50  \w     86.00 111.00   0.50    4.81    --  111.50-125.00-150.00   50
 51  \w    147.00 174.00   0.50    4.81    --  111.50 125.00  30.00   54
 52  \w     46.00  72.00   0.50    4.81    --  111.50-125.00-150.00   52
 53  \w    109.00 147.00   0.50    4.81    --  111.50  30.00 -30.00   76
 54  \w     80.00 105.00   0.50    4.81    --  111.50 -95.00  60.00   50
 55  \w     68.00  94.00   0.50    4.81    --  111.50 -95.00  90.00   52
 56  \w    150.00 177.00   0.50    4.81    --  111.50  45.00-150.00   54
 57  \w    102.00 128.00   0.50    4.81    --  111.50-150.00  24.46   52
 58  \w     97.00 127.00   0.50    4.81    --  111.50 125.00  30.00   60
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0183607000
_diffrn_orient_matrix_UB_12      -0.1404950000
_diffrn_orient_matrix_UB_13      -0.0125811000
_diffrn_orient_matrix_UB_21      -0.1870796000
_diffrn_orient_matrix_UB_22      -0.0021304000
_diffrn_orient_matrix_UB_23      0.0558764000
_diffrn_orient_matrix_UB_31      -0.0749180000
_diffrn_orient_matrix_UB_32      0.0482905000
_diffrn_orient_matrix_UB_33      -0.1268061000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0672
_diffrn_reflns_av_unetI/netI     0.0627
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.940
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11118
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.940
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         79.364
_diffrn_reflns_theta_min         4.264
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.542
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.54a (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_description       prism
_exptl_crystal_F_000             372
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.634
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.428
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         3740
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.428
_refine_ls_R_factor_all          0.1164
_refine_ls_R_factor_gt           0.0914
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2734
_refine_ls_wR_factor_ref         0.3245
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3029
_reflns_number_total             3740
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cp04364a2.cif
_cod_data_source_block           tm-4(polimorfja-49)thf_auto
_cod_depositor_comments          'Adding full bibliography for 7248039.cif.'
_cod_database_code               7248039
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_usercomment
'Ponovljeno snimanje, nije bio dobar completnes'
_shelx_estimated_absorpt_t_max   0.899
_shelx_estimated_absorpt_t_min   0.812
_diffrn_oxdiff_digest_frames
;
01a7f32baa12f82a35d555a2d8aeddb57a0343872fb
;
_diffrn_oxdiff_digest_hkl
;
010275d4f165e34ac84a814e84c540f9354032
;
_reflns_odcompleteness_completeness 98.27
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Ternary CH refined with riding coordinates:
 C6(H6), C10(H10), C1(H1), C11(H11), C12(H12), C18(H18), C8(H8), C23(H23),
 C16(H16), C3(H3)
2.b Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C2(H2A,H2B), C4(H4A,H4B), C9(H9A,H9B), C13(H13A,H13B), C7(H7A,
 H7B), C17(H17A,H17B), C21(H21A,H21B), C14(H14A,H14B), C22(H22A,H22B), C24(H24A,
 H24B), C25(H25A,H25B)
;
_shelx_res_checksum              26503
_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 4.816
_oxdiff_exptl_absorpt_empirical_full_min 0.373