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_7247706
_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         'C12 H26'
_chemical_formula_sum            'C12 H26'
_chemical_formula_weight         170.33
_chemical_name_common            dodecane
_chemical_name_systematic        n-dodecane
_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                88.90(3)
_cell_angle_beta                 84.67(2)
_cell_angle_gamma                73.309(19)
_cell_formula_units_Z            1
_cell_length_a                   4.2522(9)
_cell_length_b                   4.7701(11)
_cell_length_c                   15.904(6)
_cell_measurement_pressure       150000
_cell_measurement_reflns_used    1339
_cell_measurement_temperature    295
_cell_measurement_theta_max      18.375
_cell_measurement_theta_min      2.226
_cell_volume                     307.65(15)
_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         150000
_diffrn_ambient_temperature      295(1)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_type            'Eiger 9M CdTe'
_diffrn_measured_fraction_theta_full 0.436
_diffrn_measured_fraction_theta_max 0.354
_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    0.20    --    0.00   0.00   0.00  128
Two of these runs were performed for two crystals in two different orientations.
Then, the two datasets were merged in SORTAV
;
_diffrn_measurement_device_type
'esperanto-CrysAlisPro-abstract goniometer imported esperanto images'
_diffrn_measurement_method       'omega scan'
_diffrn_measurement_specimen_support 'diamond anvil cell'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.410
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_Laue_measured_fraction_full 0.436
_diffrn_reflns_Laue_measured_fraction_max 0.354
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -6
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            1339
_diffrn_reflns_point_group_measured_fraction_full 0.436
_diffrn_reflns_point_group_measured_fraction_max 0.354
_diffrn_reflns_theta_full        14.241
_diffrn_reflns_theta_max         18.375
_diffrn_reflns_theta_min         2.226
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.025
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             98
_exptl_crystal_recrystallization_method
'isochoric recrystallization at high pressure in diamond anvil cell'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.075
_refine_diff_density_min         -0.074
_refine_diff_density_rms         0.022
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     56
_refine_ls_number_reflns         834
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0953
_refine_ls_R_factor_gt           0.0662
_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^)+(0.1497P)^2^+0.0002P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2262
_refine_ls_wR_factor_ref         0.2574
_reflns_Friedel_coverage         0.000
_reflns_number_gt                439
_reflns_number_total             834
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3ra06957e3.cif
_cod_data_source_block           n-dodecane
_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_original_cell_volume        307.64(16)
_cod_database_code               7247706
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.999
_shelx_estimated_absorpt_t_min   0.994
_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:
 C5(H5A,H5B), C6(H6A,H6B), C4(H4A,H4B), C3(H3A,H3B), C2(H2A,H2B)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C)
;
_shelx_res_checksum              51288
_olex2_exptl_crystal_mounting_method DAC
_olex2_submission_special_instructions 'No special instructions were received'