Pressure-freezing of dodecane: exploring the crystal structures, formation kinetics and phase diagrams for colossal barocaloric effects in n-alkanes
Poręba, Tomasz; Kicior, Inga; RSC Advances 13 (2023) 33305–33317; doi:10.1039/D3RA06957E

data_7247707
_publ_section_title
;
 Pressure-freezing of dodecane: exploring the crystal structures,
 formation kinetics and phase diagrams for colossal barocaloric effects in
 n-alkanes
;
_journal_issue                   47
_journal_name_full               'RSC Advances'
_journal_page_first              33305
_journal_page_last               33317
_journal_paper_doi               10.1039/D3RA06957E
_journal_volume                  13
_journal_year                    2023
_chemical_formula_moiety         'C11 H24'
_chemical_formula_sum            'C11 H24'
_chemical_formula_weight         156.30
_chemical_name_common            undecane
_chemical_name_systematic        n-undecane
_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     dual
_audit_creation_date             2023-07-12
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2023-07-12 deposited with the CCDC.	2023-11-03 downloaded from the CCDC.
;
_cell_angle_alpha                93.609(19)
_cell_angle_beta                 90.41(2)
_cell_angle_gamma                107.274(9)
_cell_formula_units_Z            2
_cell_length_a                   4.1808(5)
_cell_length_b                   4.7113(3)
_cell_length_c                   29.53(2)
_cell_measurement_pressure       170000
_cell_measurement_reflns_used    147
_cell_measurement_temperature    295
_cell_measurement_theta_max      16.1090
_cell_measurement_theta_min      2.6160
_cell_volume                     554.1(4)
_computing_cell_refinement       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.67a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.67a (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 2017/1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      Helium
_diffrn_ambient_pressure         170000
_diffrn_ambient_temperature      295
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 13.3333
_diffrn_detector_type            'Eiger 9M CdTe'
_diffrn_measured_fraction_theta_full 0.268
_diffrn_measured_fraction_theta_max 0.261
_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    -32.00  32.00   0.50    1.00    --    0.00   0.00   0.00  128
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       '\w scans'
_diffrn_measurement_specimen_support 'diamond anvil cell'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0134237000
_diffrn_orient_matrix_UB_12      0.0048137000
_diffrn_orient_matrix_UB_13      0.0137352000
_diffrn_orient_matrix_UB_21      -0.0273326000
_diffrn_orient_matrix_UB_22      -0.0911428000
_diffrn_orient_matrix_UB_23      -0.0001327000
_diffrn_orient_matrix_UB_31      0.0981195000
_diffrn_orient_matrix_UB_32      0.0037707000
_diffrn_orient_matrix_UB_33      0.0022379000
_diffrn_radiation_monochromator  synchrotron
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_reflns_av_R_equivalents  0.0054
_diffrn_reflns_av_unetI/netI     0.0122
_diffrn_reflns_Laue_measured_fraction_full 0.268
_diffrn_reflns_Laue_measured_fraction_max 0.261
_diffrn_reflns_limit_h_max       4
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       5
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            867
_diffrn_reflns_point_group_measured_fraction_full 0.268
_diffrn_reflns_point_group_measured_fraction_max 0.261
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         14.802
_diffrn_reflns_theta_min         2.618
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.025
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58199
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.67a (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    0.937
_exptl_crystal_description       plate
_exptl_crystal_F_000             180
_exptl_crystal_recrystallization_method
'in-situ recrystallization from melt at high pressure in diamond anvil cell'
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.072
_refine_diff_density_min         -0.070
_refine_diff_density_rms         0.023
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.995
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     102
_refine_ls_number_reflns         586
_refine_ls_number_restraints     80
_refine_ls_restrained_S_all      0.972
_refine_ls_R_factor_all          0.1045
_refine_ls_R_factor_gt           0.0539
_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^)+(0.1112P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1564
_refine_ls_wR_factor_ref         0.1951
_reflns_Friedel_coverage         0.000
_reflns_number_gt                253
_reflns_number_total             586
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra06957e3.cif
_cod_data_source_block           undecane
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_diffrn_measurement_specimen_suport' was replaced with
'_diffrn_measurement_specimen_support' as specified in the
replacement file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_database_code               7247707
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.994
_diffrn_orient_matrix_axis[1]    matrixX
_diffrn_orient_matrix_axis[2]    matrixY
_diffrn_orient_matrix_axis[3]    matrixZ
_reflns_odcompleteness_completeness 15.49
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     21.01
_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. Restrained distances
 C11-C10 = C9-C10 = C9-C8 = C8-C7 = C7-C6 = C6-C5 = C5-C4 = C4-C3 = C3-C2 = C2-
 C1
 1.52 with sigma of 0.005
 C1-C2 \\sim C2-C3
 with sigma of 0.02
 C9-C10 \\sim C10-C11
 with sigma of 0.02
 C3-C4 \\sim C4-C5
 with sigma of 0.02
 C5-C6 \\sim C6-C7
 with sigma of 0.02
 C7-C8 \\sim C8-C9
 with sigma of 0.02
 C9-C8 \\sim C8-C7
 with sigma of 0.02
 C7-C6 \\sim C7-C8
 with sigma of 0.02
 C10-C9 \\sim C9-C8
 with sigma of 0.02
 C5-C6 \\sim C5-C4
 with sigma of 0.02
 C3-C4 \\sim C2-C3
 with sigma of 0.02
3. Rigid bond restraints
 C1, C2, C3, C4, C5, C6, C7, C8, C9, C10, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Uanis(C11) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C4(H4A,H4B), C8(H8A,H8B), C3(H3A,H3B), C9(H9A,H9B), C10(H10A,
 H10B), C7(H7A,H7B), C5(H5A,H5B), C2(H2A,H2B)
5.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              27023
_olex2_exptl_crystal_mounting_method DAC
_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 1.425
_oxdiff_exptl_absorpt_empirical_full_min 0.756