Conformation-aggregation interplay in the simplest aliphatic ethers probed under high pressure.
Sacharczuk, Natalia; Olejniczak, Anna; Bujak, Maciej; Dziubek, Kamil Filip; Katrusiak, Andrzej; Podsiadło, Marcin; IUCrJ 11 (2024) 57–61; doi:10.1107/S2052252523009995

data_1570452
_publ_section_title
;
 Conformation-aggregation interplay in the simplest aliphatic ethers
 probed under high pressure.
;
_journal_issue                   'Pt 1'
_journal_name_full               IUCrJ
_journal_page_first              57
_journal_page_last               61
_journal_paper_doi               10.1107/S2052252523009995
_journal_volume                  11
_journal_year                    2024
_chemical_formula_moiety         'C6 H14 O'
_chemical_formula_sum            'C6 H14 O'
_chemical_formula_weight         102.17
_chemical_name_systematic        'dipropyl ether'
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.32(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.099(12)
_cell_length_b                   3.9465(3)
_cell_length_c                   14.649(8)
_cell_measurement_reflns_used    1024
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.1230
_cell_measurement_theta_min      5.3170
_cell_volume                     520.5(8)
_computing_cell_refinement       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.49 (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         5300000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.317
_diffrn_measured_fraction_theta_max 0.296
_diffrn_measurement_device_type  'KUMA KM4-CCD, Eos'
_diffrn_measurement_method       '\f- and \w-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.317
_diffrn_reflns_Laue_measured_fraction_max 0.296
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       4
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            2594
_diffrn_reflns_point_group_measured_fraction_full 0.317
_diffrn_reflns_point_group_measured_fraction_max 0.296
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.273
_diffrn_reflns_theta_min         5.355
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.72522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.42.49 (Rigaku Oxford Diffraction, 2022)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_description       disc
_exptl_crystal_F_000             232
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.096
_refine_diff_density_min         -0.077
_refine_diff_density_rms         0.022
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     66
_refine_ls_number_reflns         310
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0666
_refine_ls_R_factor_gt           0.0469
_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^)+(0.0445P)^2^+0.3422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1081
_refine_ls_wR_factor_ref         0.1229
_reflns_Friedel_coverage         0.000
_reflns_number_gt                232
_reflns_number_total             310
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            lq5055.cif
_cod_data_source_block           dipropyl_ether_phase_alpha_5_30GPa
_cod_depositor_comments
'Adding full bibliography for 1570433--1570452.cif.'
_cod_original_cell_volume        520.5(7)
_cod_database_code               1570452
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
Data were collected at room temperature (295(2) K) and pressure of 5.50(2) GPa
(5300000 kPa).
;
_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. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.05 and sigma for terminal atoms of 0.02
3.a Secondary CH2 refined with riding coordinates:
 C1(H12,H11), C2(H22,H21), C4(H41,H42), C5(H51,H52)
3.b Idealised Me refined as rotating group:
 C3(H33,H31,H32), C6(H63,H61,H62)
;
_shelx_res_checksum              24215
_shelx_hkl_checksum              63913
_olex2_submission_special_instructions 'No special instructions were received'