Crystal structure of (5-ethyl-2-(4-methoxyphenyl)-1,3-dioxan-5-yl)methanol, C14H20O4
Yuan, Xian-You; Yuan, Lin; Zhang, Min; Li, Zhong-Yan; Zeitschrift für Kristallographie - New Crystal Structures 233 (2018) 937–938; doi:10.1515/ncrs-2018-0114

data_8106353
_publ_section_title
;
 Crystal structure of
 (5-ethyl-2-(4-methoxyphenyl)-1,3-dioxan-5-yl)methanol, C14H20O4
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              937
_journal_page_last               938
_journal_paper_doi               10.1515/ncrs-2018-0114
_journal_volume                  233
_journal_year                    2018
_chemical_formula_moiety         'C14 H20 O4'
_chemical_formula_sum            'C14 H20 O4'
_chemical_formula_weight         252.30
_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   mixed
_atom_sites_solution_primary     direct
_cell_angle_alpha                100.673(2)
_cell_angle_beta                 92.465(2)
_cell_angle_gamma                98.973(2)
_cell_formula_units_Z            4
_cell_length_a                   6.1028(13)
_cell_length_b                   10.885(2)
_cell_length_c                   20.737(4)
_cell_measurement_reflns_used    3868
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.06
_cell_measurement_theta_min      2.34
_cell_volume                     1333.5(5)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0236
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            12893
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.009
_diffrn_reflns_theta_max         25.009
_diffrn_reflns_theta_min         1.002
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.091
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6819
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0470 before and 0.0368 after correction.
The Ratio of minimum to maximum transmission is 0.9144.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_refine_diff_density_max         0.170
_refine_diff_density_min         -0.151
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4683
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0431
_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^)+(0.0640P)^2^+0.1362P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1116
_refine_ls_wR_factor_ref         0.1225
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3531
_reflns_number_total             4683
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_ncrs-2018-0114_suppl.cif
_cod_data_source_block           1
_cod_database_code               8106353
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups
2.a Riding coordinates:
 O4(H4), O8(H8A)
2.b Ternary CH refined with riding coordinates:
 C8(H8), C22(H22)
2.c Secondary CH2 refined with riding coordinates:
 C9(H9A,H9B), C12(H12A,H12B), C11(H11A,H11B), C14(H14A,H14B), C23(H23A,H23B),
 C25(H25A,H25B), C28(H28A,H28B), C26(H26A,H26B)
2.d Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4A), C6(H6), C7(H7), C20(H20), C18(H18), C21(H21), C17(H17)
2.e Idealised Me refined as rotating group:
 C13(H13A,H13B,H13C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              36914
_shelx_hkl_checksum              34117
_olex2_submission_special_instructions 'No special instructions were received'