Methyl 5-<i>cis</i>-bromo-2,2,6-trimethyl-6-<i>trans</i>-phenyltetrahydropyran-3-carboxylate
Hartung, Jens; Greb, Marco; Svoboda, Ingrid; Fuess, Hartmut; Acta Crystallographica Section E 62 (2006) o4975–o4976; doi:10.1107/S1600536806039055

data_2211001
_publ_section_title
;Methyl
 5-<i>cis</i>-bromo-2,2,6-trimethyl-6-<i>trans</i>-phenyltetrahydropyran-3-carboxylate
;
_journal_coeditor_code           GA2006
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o4975
_journal_page_last               o4976
_journal_paper_doi               10.1107/S1600536806039055
_journal_volume                  62
_journal_year                    2006
_chemical_formula_iupac          'C16 H21 Br O3'
_chemical_formula_moiety         'C16 H21 Br O3'
_chemical_formula_sum            'C16 H21 Br O3'
_chemical_formula_weight         341.24
_chemical_name_systematic
;Methyl
 5-cis-bromo-2,2,6-trimethyl-6-trans-phenyltetrahydropyran-3-carboxylate
;
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.26(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.547(2)
_cell_length_b                   19.805(3)
_cell_length_c                   7.5980(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    304(2)
_cell_measurement_theta_max      11.96
_cell_measurement_theta_min      3.66
_cell_volume                     1556.5(4)
_computing_cell_refinement
;
CAD-4 Diffractometer Control Software
;
_computing_data_collection
;
CAD-4 Diffractometer Control Software (Nonius, 1993)
;
_computing_data_reduction
;
CAD-4 Diffractometer Control Software
;
_computing_molecular_graphics
;
PLATON2002 (Spek, 2003) and ORTEP-3 (Farrugia, 1997,
2005)
;
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      304(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Enraf--Nonius CAD-4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0549
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       2
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            3907
_diffrn_reflns_theta_full        25.98
_diffrn_reflns_theta_max         25.98
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        4.20
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.645
_exptl_absorpt_correction_T_max  0.711
_exptl_absorpt_correction_T_min  0.466
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North <i>et al.</i>,  1968)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Prism
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.752
_refine_diff_density_min         -0.769
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         3052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0955
_refine_ls_R_factor_gt           0.0454
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0826P)^2^+0.1955P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1190
_refine_ls_wR_factor_ref         0.1363
_reflns_number_gt                1966
_reflns_number_total             3052
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ga2006.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2211001
_cod_database_fobs_code          2211001