An axial <i>tert</i>-butyl group in strained cyclohexene: X-ray analysis and theoretical calculations of 2-(2-<i>tert</i>-butylcyclohex-3-enyl)propan-2-ol
Kakou-Yao, Rita; Sessouma, Bintou; Aycard, Jean Pierre; Acta Crystallographica Section C 64 (2008) o61–o63; doi:10.1107/S0108270107065468

data_2016455
_publ_section_title
;
 An axial <i>tert</i>-butyl group in strained cyclohexene: X-ray
 analysis and theoretical calculations of
 2-(2-<i>tert</i>-butylcyclohex-3-enyl)propan-2-ol
;
_journal_coeditor_code           SK3183
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o61
_journal_page_last               o63
_journal_paper_doi               10.1107/S0108270107065468
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          'C13 H24 O'
_chemical_formula_moiety         'C13 H24 O'
_chemical_formula_sum            'C13 H24 O'
_chemical_formula_weight         196.33
_chemical_name_common            dom1
_chemical_name_systematic
;
2-(2-tert-butylcyclohex-3-enyl)propan-2-ol
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           CRYSTALS_ver_12.84
_cell_angle_alpha                90
_cell_angle_beta                 103.915(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.0192(4)
_cell_length_b                   6.0581(2)
_cell_length_c                   16.3514(4)
_cell_measurement_reflns_used    15244
_cell_measurement_temperature    294
_cell_measurement_theta_max      30.055
_cell_measurement_theta_min      1.611
_cell_volume                     1251.81(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics
;
ORTEP-3 for Windows (Farrugia, 1997) and PLATON (Spek, 2003)
;
_computing_publication_material  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge <i>et al.</i>,  2003)'
_computing_structure_solution    'SIR92 (Altomare <i>et al.</i>,  1994)'
_diffrn_ambient_temperature      294
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.040
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            15244
_diffrn_reflns_theta_full        28.252
_diffrn_reflns_theta_max         30.055
_diffrn_reflns_theta_min         1.611
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.042
_exptl_crystal_description       needle
_exptl_crystal_F_000             440
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.19
_refine_diff_density_min         -0.17
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9125
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    93
_refine_ls_number_parameters     130
_refine_ls_number_reflns         2533
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0872
_refine_ls_R_factor_gt           0.0567
_refine_ls_shift/su_max          0.000254
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial (Watkin, 1994, Prince, 1982),
[weight] = 1.0/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)],
where A~i~ are the Chebychev coefficients listed below and x = Fcalc/Fmax.
Method = Robust Weighting (Prince, 1982),
W = [weight] * [1-(\dF/6*\sF)^2^]^2^
A~i~ are: 430, 475, 362, 83.5.
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1246
_refine_ls_wR_factor_gt          0.1047
_refine_ls_wR_factor_ref         0.1047
_reflns_number_gt                2533
_reflns_number_total             3625
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            sk3183.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2016455
_cod_database_fobs_code          2016455