#------------------------------------------------------------------------------
#$Date: 2024-02-05 14:09:55 +0200 (Mon, 05 Feb 2024) $
#$Revision: 289697 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/04/1570437.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_1570437
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                90.249(12)
_cell_angle_beta                 93.92(2)
_cell_angle_gamma                90.14(3)
_cell_formula_units_Z            8
_cell_length_a                   4.2888(17)
_cell_length_b                   8.3045(18)
_cell_length_c                   12.7912(13)
_cell_measurement_reflns_used    1388
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.6310
_cell_measurement_theta_min      4.9210
_cell_volume                     454.5(2)
_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         5600000
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.330
_diffrn_measured_fraction_theta_max 0.303
_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  0.0306
_diffrn_reflns_av_unetI/netI     0.0272
_diffrn_reflns_Laue_measured_fraction_full 0.330
_diffrn_reflns_Laue_measured_fraction_max 0.303
_diffrn_reflns_limit_h_max       2
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            2631
_diffrn_reflns_point_group_measured_fraction_full 0.330
_diffrn_reflns_point_group_measured_fraction_max 0.303
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.255
_diffrn_reflns_theta_min         4.792
_exptl_absorpt_coefficient_mu    0.104
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78843
_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    1.346
_exptl_crystal_description       disc
_exptl_crystal_F_000             208
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.21
_refine_diff_density_max         0.231
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.057
_refine_ls_extinction_coef       0.12(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.135
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         559
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.1296
_refine_ls_R_factor_gt           0.1173
_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)+(0.0699P)²+2.7136P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2518
_refine_ls_wR_factor_ref         0.2604
_reflns_Friedel_coverage         0.000
_reflns_number_gt                486
_reflns_number_total             559
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            lq5055.cif
_cod_data_source_block           dimethyl_ether_phase_gamma_5_60GPa
_cod_depositor_comments
'Adding full bibliography for 1570433--1570452.cif.'
_cod_database_code               1570437
_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 5.60(2) GPa
(5600000 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 0.242(3) 0.8248(9) -0.0022(4) 0.0355(18) Uiso 1 1 d . . . . .
C1 C -0.044(6) 0.7338(16) -0.0090(7) 0.044(3) Uiso 1 1 d . . . . .
H13 H -0.090194 0.698647 -0.079991 0.066 Uiso 1 1 calc R U . . .
H11 H -0.211365 0.800321 0.012419 0.066 Uiso 1 1 calc R U . . .
H12 H -0.022179 0.641798 0.036022 0.066 Uiso 1 1 calc R U . . .
C2 C 0.253(5) 0.9101(16) 0.0956(7) 0.035(2) Uiso 1 1 d . . . . .
H23 H 0.401532 0.996640 0.094303 0.053 Uiso 1 1 calc R U . . .
H21 H 0.315057 0.837755 0.151533 0.053 Uiso 1 1 calc R U . . .
H22 H 0.050127 0.952873 0.106470 0.053 Uiso 1 1 calc R U . . .
O2 O 0.839(4) 0.5131(9) 0.1969(4) 0.0355(19) Uiso 1 1 d . . . . .
C3 C 0.583(6) 0.4931(16) 0.1409(8) 0.044(3) Uiso 1 1 d . . . . .
H33 H 0.597037 0.397973 0.098645 0.066 Uiso 1 1 calc R U . . .
H31 H 0.545875 0.584812 0.096426 0.066 Uiso 1 1 calc R U . . .
H32 H 0.413976 0.481568 0.185831 0.066 Uiso 1 1 calc R U . . .
C4 C 0.826(5) 0.6641(14) 0.2545(7) 0.033(2) Uiso 1 1 d . . . . .
H42 H 0.736833 0.746038 0.208976 0.050 Uiso 1 1 calc R U . . .
H43 H 1.033412 0.695640 0.279589 0.050 Uiso 1 1 calc R U . . .
H41 H 0.699224 0.650412 0.312783 0.050 Uiso 1 1 calc R U . . .
O3 O 0.711(4) 0.0119(9) 0.2914(4) 0.039(2) Uiso 1 1 d . . . . .
C5 C 0.423(6) -0.0119(17) 0.3472(8) 0.048(3) Uiso 1 1 d . . . . .
H51 H 0.261497 0.056876 0.317384 0.072 Uiso 1 1 calc R U . . .
H52 H 0.464730 0.014100 0.419992 0.072 Uiso 1 1 calc R U . . .
H53 H 0.357516 -0.122233 0.340226 0.072 Uiso 1 1 calc R U . . .
C6 C 0.678(6) 0.1662(14) 0.2479(7) 0.038(2) Uiso 1 1 d . . . . .
H62 H 0.509187 0.165541 0.194479 0.057 Uiso 1 1 calc R U . . .
H63 H 0.867947 0.196660 0.217750 0.057 Uiso 1 1 calc R U . . .
H61 H 0.632919 0.242027 0.301708 0.057 Uiso 1 1 calc R U . . .
O4 O 0.274(4) 0.3116(10) 0.4989(4) 0.0381(19) Uiso 1 1 d . . . . .
C7 C -0.032(6) 0.2154(16) 0.5048(7) 0.038(3) Uiso 1 1 d . . . . .
H73 H -0.012530 0.143250 0.563344 0.058 Uiso 1 1 calc R U . . .
H71 H -0.072304 0.154542 0.441314 0.058 Uiso 1 1 calc R U . . .
H72 H -0.201529 0.288377 0.513443 0.058 Uiso 1 1 calc R U . . .
C8 C 0.222(6) 0.4120(15) 0.4061(6) 0.033(2) Uiso 1 1 d . . . . .
H81 H 0.111214 0.507395 0.423767 0.050 Uiso 1 1 calc R U . . .
H82 H 0.101913 0.353007 0.352648 0.050 Uiso 1 1 calc R U . . .
H83 H 0.420049 0.441628 0.380646 0.050 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
C2 O1 C1 106.6(11) . . ?
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 109.2(16) . . ?
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 . . ?
C6 O3 C5 104.3(15) . . ?
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 . . ?
C8 O4 C7 104.7(11) . . ?
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 1.44(2) . ?
O1 C2 1.433(11) . ?
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 1.28(3) . ?
O2 C4 1.455(13) . ?
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 1.48(3) . ?
O3 C6 1.403(15) . ?
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 1.543(19) . ?
O4 C8 1.459(13) . ?
C7 H73 0.9600 . ?
C7 H71 0.9600 . ?
C7 H72 0.9600 . ?
C8 H81 0.9600 . ?
C8 H82 0.9600 . ?
C8 H83 0.9600 . ?
