2-(6-Methoxy-7-methyl-1,2,3,4-tetrahydro-1-naphthyl)ethyl 4,7,7-trimethyl-3-oxo-2-oxabicyclo[2.2.1]heptane-1-carboxylate
Noltemeyer, M.; Raschke, T.; Tietze, L. F.; Acta Crystallographica Section C 52 (1996) 2256–2258; doi:10.1107/S0108270196004167

data_2005375
_publ_section_title
;
 2-(6-Methoxy-7-methyl-1,2,3,4-tetrahydro-1-naphthyl)ethyl
 4,7,7-trimethyl-3-oxo-2-oxabicyclo[2.2.1]heptane-1-carboxylate
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2256
_journal_page_last               2258
_journal_paper_doi               10.1107/S0108270196004167
_journal_volume                  52
_journal_year                    1996
_chemical_formula_iupac          'C24 H32 O5'
_chemical_formula_sum            'C24 H32 O5'
_chemical_formula_weight         400.50
_chemical_melting_point          124
_chemical_name_systematic
;
2-(6-Methoxy-7-methyl-1,2,3,4-tetrahydro-naphthalene-1-yl)ethyl
4,7,7-trimethyl-3-oxo-2-oxa-bicyclo[2.2.1]heptane-1-carboxylate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   6.4190(10)
_cell_length_b                   13.340(2)
_cell_length_c                   24.701(2)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      10
_cell_volume                     2115.1(5)
_computing_cell_refinement       DIF4
_computing_data_collection       'DIF4 (Stoe & Cie, 1991a)'
_computing_data_reduction        'REDU4 (Stoe & Cie, 1991b)'
_computing_molecular_graphics    'SHELXTL-Plus (Sheldrick, 1990b)'
_computing_publication_material  SHELXTL-Plus
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990a)'
_diffrn_ambient_temperature      153(2)
_diffrn_measurement_device       'Stoe AED2 four-circle'
_diffrn_measurement_method       'profile fitted 2\q-\w'
_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  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0353
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4299
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         3.52
_diffrn_standards_decay_%        none
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.258
_exptl_crystal_description       block
_exptl_crystal_F_000             864
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.80
_exptl_crystal_size_min          0.70
_refine_diff_density_max         0.213
_refine_diff_density_min         -0.153
_refine_ls_abs_structure_details
;
Flack (1983) parameter = -1.2(13); consequently
the absolute structure was assigned according to
that of the camphane group
;
_refine_ls_abs_structure_Flack   -1.2(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.066
_refine_ls_goodness_of_fit_obs   1.066
_refine_ls_hydrogen_treatment    'H atoms refined as riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     267
_refine_ls_number_reflns         2150
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.066
_refine_ls_R_factor_all          0.0356
_refine_ls_R_factor_obs          0.0320
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
;
calc w = 1/[\s^2^(F~o~^2^) + (0.036P)^2^ + 0.47P]
where P = (F~o~^2^ + 2F~c~^2^)/3
;
_refine_ls_wR_factor_all         0.0818
_refine_ls_wR_factor_obs         0.0776
_reflns_number_observed          2003
_reflns_number_total             2151
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ka1161.cif
_cod_data_source_block           tie73
_cod_database_code               2005375