Novel Oxidative Rearrangement Product of the First <i>trans</i>,<i>cis</i>,<i>cis</i>,<i>cis</i>-[5.5.5.5]Fenestrane Derivative
Wender, Paul A.; deLong, Mitch A.; Wireko, Fred C.; Acta Crystallographica Section C 53 (1997) 954–956; doi:10.1107/S0108270197002278

data_2006311
_publ_section_title
;
 Novel Oxidative Rearrangement Product of the First
 <i>trans</i>,<i>cis</i>,<i>cis</i>,<i>cis</i>-[5.5.5.5]Fenestrane
 Derivative
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              954
_journal_page_last               956
_journal_paper_doi               10.1107/S0108270197002278
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C16 H22 O2'
_chemical_formula_sum            'C16 H22 O2'
_chemical_formula_weight         246.34
_chemical_name_common
;
trans,cis,cis,cis-[5,5,5,5]fenestrane
;
_chemical_name_systematic
;
 rel-(4S,6R,9S,11S)-1-hydroxy-16-methyl-14-oxapentacyclo-
[7.4.3.0^4,15^.0^11,15^.0^6,16^]hexadeca-7-ene
;
_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'
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 98.05(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.567(2)
_cell_length_b                   12.189(2)
_cell_length_c                   12.557(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30
_cell_measurement_theta_min      18
_cell_volume                     1298.3(5)
_computing_cell_refinement
'TEXSAN (Molcular Structure Corporation, 1992b)'
_computing_data_collection
;
 MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1992a)
;
_computing_data_reduction        TEXSAN
_computing_molecular_graphics    SHELXTL
_computing_structure_refinement  'SHELXTL (Sheldrick, 1994)'
_computing_structure_solution    'SHELXTL-Plus (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Rigaku AFC5R RU200'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         xray_tube
_diffrn_radiation_type           'Copper K\a'
_diffrn_radiation_wavelength     1.54059
_diffrn_reflns_av_R_equivalents  0.0206
_diffrn_reflns_av_sigmaI/netI    0.0323
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2183
_diffrn_reflns_theta_max         61.86
_diffrn_reflns_theta_min         5.08
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.635
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.260
_exptl_crystal_density_meas      ?
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.253
_refine_diff_density_min         -0.187
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.104
_refine_ls_hydrogen_treatment
'H-atom positions refined, U values fixed in final cycle'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         2035
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.104
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_obs          .0469
_refine_ls_shift/esd_max         -0.048
_refine_ls_shift/esd_mean        0.009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.4621P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1257
_refine_ls_wR_factor_obs         .1226
_reflns_number_observed          1871
_reflns_number_total             2035
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fr1026.cif
_cod_data_source_block           del
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.4621P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to 'w =
1/[\s^2^(Fo^2^)+(0.0573P)^2^+0.4621P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2006311