#------------------------------------------------------------------------------
#$Date: 2024-02-05 14:09:55 +0200 (Mon, 05 Feb 2024) $
#$Revision: 289697 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/04/1570436.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1570436
loop_
_publ_author_name
'Sacharczuk, Natalia'
'Olejniczak, Anna'
'Bujak, Maciej'
'Dziubek, Kamil Filip'
'Katrusiak, Andrzej'
'Podsiadło, Marcin'
_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         'C2 H6 O'
_chemical_formula_sum            'C2 H6 O'
_chemical_formula_weight         46.07
_chemical_name_systematic        'dimethyl ether'
_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     direct
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_cell_angle_alpha                90.55(4)
_cell_angle_beta                 93.89(6)
_cell_angle_gamma                90.83(2)
_cell_formula_units_Z            8
_cell_length_a                   4.3394(12)
_cell_length_b                   8.414(2)
_cell_length_c                   12.821(6)
_cell_measurement_reflns_used    1331
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.6930
_cell_measurement_theta_min      4.7360
_cell_volume                     467.0(3)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_environment      'diamond-anvil cell'
_diffrn_ambient_pressure         4500000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.320
_diffrn_measured_fraction_theta_max 0.297
_diffrn_measurement_device_type  'KUMA KM4-CCD, Eos'
_diffrn_measurement_method       'φ- and ω-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.320
_diffrn_reflns_Laue_measured_fraction_max 0.297
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            2659
_diffrn_reflns_point_group_measured_fraction_full 0.320
_diffrn_reflns_point_group_measured_fraction_max 0.297
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.154
_diffrn_reflns_theta_min         4.868
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.50805
_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    1.311
_exptl_crystal_description       disc
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.150
_refine_diff_density_min         -0.140
_refine_diff_density_rms         0.034
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         556
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0628
_refine_ls_R_factor_gt           0.0554
_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/[σ²(Fo²)+(0.0885P)²+0.3224P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1474
_refine_ls_wR_factor_ref         0.1553
_reflns_Friedel_coverage         0.000
_reflns_number_gt                481
_reflns_number_total             556
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lq5055.cif
_cod_data_source_block           dimethyl_ether_phase_gamma_4_50GPa
_cod_depositor_comments
'Adding full bibliography for 1570433--1570452.cif.'
_cod_database_code               1570436
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_exptl_absorpt_special_details
;
Data were collected at room temperature (295(2) K) and pressure of 4.50(2) GPa
(4500000 kPa).
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C1(H13,H11,H12), C2(H23,H21,H22), C3(H33,H31,H32), C4(H42,H43,H41), C5(H51,
 H52,H53), C6(H62,H63,H61), C7(H73,H71,H72), C8(H81,H82,H83)
;
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
O1 O 0.2353(9) 0.8266(5) -0.0051(11) 0.062(9) Uani 1 1 d . . . . .
C1 C -0.0287(9) 0.7298(5) -0.0134(10) 0.044(8) Uani 1 1 d . . . . .
H13 H -0.043845 0.676938 -0.080241 0.065 Uiso 1 1 calc R U . . .
H11 H -0.207859 0.793660 -0.006548 0.065 Uiso 1 1 calc R U . . .
H12 H -0.016169 0.652057 0.041042 0.065 Uiso 1 1 calc R U . . .
C2 C 0.2688(14) 0.9025(8) 0.0925(17) 0.065(14) Uani 1 1 d . . . . .
H23 H 0.450244 0.969563 0.095980 0.098 Uiso 1 1 calc R U . . .
H21 H 0.288592 0.824268 0.146477 0.098 Uiso 1 1 calc R U . . .
H22 H 0.090664 0.965959 0.102216 0.098 Uiso 1 1 calc R U . . .
O2 O 0.8338(5) 0.5159(3) 0.1951(6) 0.053(7) Uani 1 1 d . . . . .
C3 C 0.5369(8) 0.4961(6) 0.1440(10) 0.050(9) Uani 1 1 d . . . . .
H33 H 0.538992 0.409885 0.094456 0.075 Uiso 1 1 calc R U . . .
H31 H 0.480134 0.592040 0.108156 0.075 Uiso 1 1 calc R U . . .
H32 H 0.389909 0.472796 0.194624 0.075 Uiso 1 1 calc R U . . .
C4 C 0.8463(10) 0.6574(5) 0.2578(12) 0.061(11) Uani 1 1 d . . . . .
H42 H 0.788825 0.746478 0.214836 0.092 Uiso 1 1 calc R U . . .
H43 H 1.052462 0.673782 0.288411 0.092 Uiso 1 1 calc R U . . .
H41 H 0.705954 0.647051 0.312144 0.092 Uiso 1 1 calc R U . . .
O3 O 0.7072(5) 0.0121(3) 0.2903(6) 0.043(6) Uani 1 1 d . . . . .
C5 C 0.4487(9) -0.0198(6) 0.3482(11) 0.068(11) Uani 1 1 d . . . . .
H51 H 0.262856 -0.006975 0.304254 0.103 Uiso 1 1 calc R U . . .
H52 H 0.449390 0.052624 0.406528 0.103 Uiso 1 1 calc R U . . .
H53 H 0.457795 -0.126945 0.373262 0.103 Uiso 1 1 calc R U . . .
C6 C 0.6947(12) 0.1668(6) 0.2465(11) 0.056(11) Uani 1 1 d . . . . .
H62 H 0.513907 0.174374 0.199385 0.083 Uiso 1 1 calc R U . . .
H63 H 0.875650 0.185774 0.208993 0.083 Uiso 1 1 calc R U . . .
H61 H 0.686102 0.244659 0.301374 0.083 Uiso 1 1 calc R U . . .
O4 O 0.2707(5) 0.3082(3) 0.4954(7) 0.042(7) Uani 1 1 d . . . . .
C7 C 0.0047(8) 0.2104(5) 0.5040(10) 0.040(8) Uani 1 1 d . . . . .
H73 H 0.034023 0.144502 0.564476 0.060 Uiso 1 1 calc R U . . .
H71 H -0.027707 0.144552 0.442571 0.060 Uiso 1 1 calc R U . . .
H72 H -0.172111 0.276006 0.510812 0.060 Uiso 1 1 calc R U . . .
C8 C 0.2335(9) 0.4051(5) 0.4043(10) 0.050(10) Uani 1 1 d . . . . .
H81 H 0.047544 0.465073 0.406699 0.076 Uiso 1 1 calc R U . . .
H82 H 0.220763 0.338591 0.342861 0.076 Uiso 1 1 calc R U . . .
H83 H 0.407307 0.476676 0.402276 0.076 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 O1 C2 111.0(13) . . ?
O1 C1 H13 109.5 . . ?
O1 C1 H11 109.5 . . ?
O1 C1 H12 109.5 . . ?
H13 C1 H11 109.5 . . ?
H13 C1 H12 109.5 . . ?
H11 C1 H12 109.5 . . ?
O1 C2 H23 109.5 . . ?
O1 C2 H21 109.5 . . ?
O1 C2 H22 109.5 . . ?
H23 C2 H21 109.5 . . ?
H23 C2 H22 109.5 . . ?
H21 C2 H22 109.5 . . ?
C3 O2 C4 110.1(4) . . ?
O2 C3 H33 109.5 . . ?
O2 C3 H31 109.5 . . ?
O2 C3 H32 109.5 . . ?
H33 C3 H31 109.5 . . ?
H33 C3 H32 109.5 . . ?
H31 C3 H32 109.5 . . ?
O2 C4 H42 109.5 . . ?
O2 C4 H43 109.5 . . ?
O2 C4 H41 109.5 . . ?
H42 C4 H43 109.5 . . ?
H42 C4 H41 109.5 . . ?
H43 C4 H41 109.5 . . ?
C5 O3 C6 111.5(5) . . ?
O3 C5 H51 109.5 . . ?
O3 C5 H52 109.5 . . ?
O3 C5 H53 109.5 . . ?
H51 C5 H52 109.5 . . ?
H51 C5 H53 109.5 . . ?
H52 C5 H53 109.5 . . ?
O3 C6 H62 109.5 . . ?
O3 C6 H63 109.5 . . ?
O3 C6 H61 109.5 . . ?
H62 C6 H63 109.5 . . ?
H62 C6 H61 109.5 . . ?
H63 C6 H61 109.5 . . ?
C7 O4 C8 110.2(5) . . ?
O4 C7 H73 109.5 . . ?
O4 C7 H71 109.5 . . ?
O4 C7 H72 109.5 . . ?
H73 C7 H71 109.5 . . ?
H73 C7 H72 109.5 . . ?
H71 C7 H72 109.5 . . ?
O4 C8 H81 109.5 . . ?
O4 C8 H82 109.5 . . ?
O4 C8 H83 109.5 . . ?
H81 C8 H82 109.5 . . ?
H81 C8 H83 109.5 . . ?
H82 C8 H83 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
O1 C1 1.393(5) . ?
O1 C2 1.40(3) . ?
C1 H13 0.9600 . ?
C1 H11 0.9600 . ?
C1 H12 0.9600 . ?
C2 H23 0.9600 . ?
C2 H21 0.9600 . ?
C2 H22 0.9600 . ?
O2 C3 1.412(7) . ?
O2 C4 1.428(12) . ?
C3 H33 0.9600 . ?
C3 H31 0.9600 . ?
C3 H32 0.9600 . ?
C4 H42 0.9600 . ?
C4 H43 0.9600 . ?
C4 H41 0.9600 . ?
O3 C5 1.411(10) . ?
O3 C6 1.423(6) . ?
C5 H51 0.9600 . ?
C5 H52 0.9600 . ?
C5 H53 0.9600 . ?
C6 H62 0.9600 . ?
C6 H63 0.9600 . ?
C6 H61 0.9600 . ?
O4 C7 1.419(4) . ?
O4 C8 1.432(11) . ?
C7 H73 0.9600 . ?
C7 H71 0.9600 . ?
C7 H72 0.9600 . ?
C8 H81 0.9600 . ?
C8 H82 0.9600 . ?
C8 H83 0.9600 . ?
