Resolution of (<i>S</i>,<i>S</i>)-4-(2,2,4-trimethylchroman-4-yl)phenyl camphanate and its 4-chromanyl epimer by crystallization
Esterhuysen, Catharine; Bredenkamp, Martin W.; Lloyd, Gareth O.; Acta Crystallographica Section C 61 (2005) o32–o34; doi:10.1107/S0108270104029671

data_2014700
_publ_section_title
;
 Resolution of
 (<i>S</i>,<i>S</i>)-4-(2,2,4-trimethylchroman-4-yl)phenyl camphanate
 and its 4-chromanyl epimer by crystallization
;
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o32
_journal_page_last               o34
_journal_paper_doi               10.1107/S0108270104029671
_journal_volume                  61
_journal_year                    2005
_chemical_formula_iupac          'C28 H32 O5'
_chemical_formula_moiety         'C28 H32 O5'
_chemical_formula_sum            'C28 H32 O5'
_chemical_formula_weight         448.54
_chemical_name_common
;
(R,S)-4-(2,2,4-trimethylchroman-4-yl)phenyl camphanate
;
_chemical_name_systematic
;
(R,S)-4-(2,2,4-trimethylchroman-4-yl)phenyl
4,7,7-trimethyl-3-oxo-2-oxobicyclo[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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.0710(5)
_cell_length_b                   6.8500(4)
_cell_length_c                   48.717(4)
_cell_measurement_reflns_used    5449
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     2359.7(3)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'XSEED (Barbour, 2001)'
_computing_publication_material  XSEED
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       \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  0.0641
_diffrn_reflns_av_sigmaI/netI    0.0794
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -56
_diffrn_reflns_number            13513
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.67
_exptl_absorpt_coefficient_mu    0.086
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2002)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.263
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.195
_refine_diff_density_min         -0.153
_refine_ls_abs_structure_details 'Flack (1983), with how many Friedel pairs'
_refine_ls_abs_structure_Flack   0(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.191
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         2734
_refine_ls_number_restraints     324
_refine_ls_restrained_S_all      1.135
_refine_ls_R_factor_all          0.0839
_refine_ls_R_factor_gt           0.0670
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0295P)^2^+0.4167P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1236
_refine_ls_wR_factor_ref         0.1306
_reflns_number_gt                2282
_reflns_number_total             2734
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hj1032.cif
_cod_data_source_block           Ia
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               2014700
_cod_database_fobs_code          2014700