Crystal structure of (2-(2-chlorophenyl)-5-methyl-1,3-dioxan-5-yl)methanol, C12H15ClO3
Li, Zhong-Yan; Yuan, Lin; Zhang, Min; Yuan, Xian-You; Zeitschrift für Kristallographie - New Crystal Structures 231 (2016) 957–958; doi:10.1515/ncrs-2016-0020

data_8107061
_publ_section_title
;
 Crystal structure of
 (2-(2-chlorophenyl)-5-methyl-1,3-dioxan-5-yl)methanol, C12H15ClO3
;
_journal_issue                   3
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              957
_journal_page_last               958
_journal_paper_doi               10.1515/ncrs-2016-0020
_journal_volume                  231
_journal_year                    2016
_chemical_formula_moiety         'C12 H15 Cl O3'
_chemical_formula_sum            'C12 H15 Cl O3'
_chemical_formula_weight         242.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 106.637(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.0231(14)
_cell_length_b                   10.7318(16)
_cell_length_c                   11.2419(17)
_cell_measurement_reflns_used    8199
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.56
_cell_measurement_theta_min      2.68
_cell_volume                     1158.6(3)
_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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0696
_diffrn_reflns_av_unetI/netI     0.1004
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14420
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.12
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.319
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.7156
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0407 before and 0.0300 after correction.
The Ratio of minimum to maximum transmission is 0.9598.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             512
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.36
_refine_diff_density_max         0.979
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.121
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         2025
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.156
_refine_ls_R_factor_all          0.1548
_refine_ls_R_factor_gt           0.0493
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1218P)^2^+0.0614P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1607
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                1430
_reflns_number_total             2025
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            suppl_ncrs-2016-0020_suppl.cif
_cod_data_source_block           1
_cod_database_code               8107061
_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. Rigid bond restraints
 C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 O1, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O1, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.005
 O1, C12
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.01
 O1, C12
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
3. Uiso/Uaniso restraints and constraints
O1 \\sim C12: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
4.a Ternary CH refined with riding coordinates:
 C1(H1)
4.b Secondary CH2 refined with riding coordinates:
 C8(H8A,H8B), C9(H9A,H9B)
4.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C4(H4), C7(H7), C6(H6)
4.d Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C)
4.e Idealised tetrahedral OH refined as rotating group:
 O1(H1A)
;
_olex2_submission_special_instructions 'No special instructions were received'