Crystal structure of 2-(4-Bromophenyl)-5-ethyl-1,3-dioxane-5-carboxylic acid, C13H15BrO4
Jia, Guo-Kai; Yuan, Lin; Zhang, Min; Yuan, Xian-You; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 959–960; doi:10.1515/ncrs-2016-0021

data_8107062
_publ_section_title
;
 Crystal structure of 2-(4-Bromophenyl)-5-ethyl-1,3-dioxane-5-carboxylic
 acid, C13H15BrO4
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              959
_journal_page_last               960
_journal_paper_doi               10.1515/ncrs-2016-0021
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C13 H15 Br O4'
_chemical_formula_sum            'C13 H15 Br O4'
_chemical_formula_weight         315.17
_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                 92.556(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   12.872(4)
_cell_length_b                   8.311(2)
_cell_length_c                   24.598(7)
_cell_measurement_reflns_used    9646
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.65
_cell_measurement_theta_min      2.45
_cell_volume                     2628.9(13)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_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    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.9978
_diffrn_measured_fraction_theta_max 0.9978
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            27785
_diffrn_reflns_theta_full        25.0065
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.01
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.131
_exptl_absorpt_correction_T_max  0.4340
_exptl_absorpt_correction_T_min  0.3462
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.5924
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1278.4709
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.4714
_refine_diff_density_min         -0.9354
_refine_diff_density_rms         0.1121
_refine_ls_d_res_high            0.8407
_refine_ls_d_res_low             6.7577
_refine_ls_goodness_of_fit_ref   1.0454
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    50
_refine_ls_number_parameters     328
_refine_ls_number_reflns         4613
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0454
_refine_ls_R_factor_all          0.0454
_refine_ls_R_factor_gt           0.0357
_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^)+(0.0506P)^2^+1.3557P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0874
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              13
_reflns_limit_h_min              -15
_reflns_limit_k_max              9
_reflns_limit_k_min              0
_reflns_limit_l_max              29
_reflns_limit_l_min              -12
_reflns_number_gt                3860
_reflns_number_total             4613
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            suppl_ncrs-2016-0021_suppl.cif
_cod_data_source_block           1
_cod_original_cell_volume        2629.0(13)
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_database_code               8107062
_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 Ternary CH refined with riding coordinates:
 C7(H7), C20(H20)
2.b Secondary CH2 refined with riding coordinates:
 C22(H22a,H22b), C21(H21a,H21b), C8(H8a,H8b), C9(H9a,H9b), C11(H11a,H11b),
 C24(H24a,H24b)
2.c Aromatic/amide H refined with riding coordinates:
 C4(H4), C15(H15), C16(H16), C6(H6), C3(H3), C2(H2), C18(H18), C19(H19)
2.d Idealised Me refined as rotating group:
 C25(H25a,H25b,H25c), C12(H12a,H12b,H12c)
2.e Idealised tetrahedral OH refined as rotating group:
 O4(H4a), O8(H8)
;
_olex2_submission_special_instructions 'No special instructions were received'