Crystal structure of 5-ethyl-2-(p-tolyl)-1,3-dioxane-5-carboxylic acid, C14H18O4
Jia, Guo-Kai; Yuan, Lin; Yuan, Xian-You; Li, Zhong-Yan; Zeitschrift für Kristallographie - New Crystal Structures 232 (2017) 819–820; doi:10.1515/ncrs-2017-0061

data_8106689
_publ_section_title
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 Crystal structure of 5-ethyl-2-(p-tolyl)-1,3-dioxane-5-carboxylic acid,
 C14H18O4
;
_journal_issue                   5
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              819
_journal_page_last               820
_journal_paper_doi               10.1515/ncrs-2017-0061
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C14 H18 O4'
_chemical_formula_sum            'C14 H18 O4'
_chemical_formula_weight         250.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_cell_angle_alpha                90
_cell_angle_beta                 92.238(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.763(6)
_cell_length_b                   5.941(4)
_cell_length_c                   20.310(12)
_cell_measurement_reflns_used    6778
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.43
_cell_measurement_theta_min      2.81
_cell_volume                     1297.7(14)
_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  'olex2.refine (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9974
_diffrn_measured_fraction_theta_max 0.9974
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0173
_diffrn_reflns_av_unetI/netI     0.0113
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            13878
_diffrn_reflns_theta_full        25.0086
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         2.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.093
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0435 before and 0.0278 after correction.
The Ratio of minimum to maximum transmission is 0.9406.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    1.2810
_exptl_crystal_description       block
_exptl_crystal_F_000             536.3217
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.2360
_refine_diff_density_min         -0.2237
_refine_diff_density_rms         0.0529
_refine_ls_d_res_high            0.8406
_refine_ls_d_res_low             10.1473
_refine_ls_goodness_of_fit_ref   1.0778
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    27
_refine_ls_number_parameters     168
_refine_ls_number_reflns         2273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0778
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          0.0000
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0730P)^2^+0.4018P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1351
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              24
_reflns_limit_l_min              -10
_reflns_number_gt                2041
_reflns_number_total             2273
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2017-0061_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        1297.7(13)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               8106689
_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
2.a Ternary CH refined with riding coordinates:
 C8(H8)
2.b Secondary CH2 refined with riding coordinates:
 C10(H10a,H10b), C9(H9a,H9b), C13(H13a,H13b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4a), C6(H6), C3(H3), C7(H7)
2.d Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C14(H14a,H14b,H14c)
;
_olex2_submission_special_instructions 'No special instructions were received'