A Benzannulated [5.3.1] Propellanone Related to the <i>ABC</i> Ring System of Taxol^TM^
Mackay, Maureen F.; Banwell, Martin G.; Phyland, James R.; Acta Crystallographica Section C 53 (1997) 1497–1499; doi:10.1107/S0108270197007531

data_2006628
_publ_section_title
;
 A Benzannulated [5.3.1] Propellanone Related to the <i>ABC</i> Ring
 System of Taxol^TM^
;
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1497
_journal_page_last               1499
_journal_paper_doi               10.1107/S0108270197007531
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C16 H16 Br2 O2'
_chemical_formula_structural     'C16 H16 Br2 O2'
_chemical_formula_sum            'C16 H16 Br2 O2'
_chemical_formula_weight         400.2
_chemical_melting_point          464.0(10)
_chemical_name_systematic
;(3a\a,10a\a)11,11 Dibromo-6-methoxy-2,3,9,10-tetrahydro-1H,4H-3a,10a-
methano[f]azulene'
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_audit_creation_method           'SHELXL-93 (Sheldrick,1993)'
_cell_angle_alpha                104.990(10)
_cell_angle_beta                 103.740(10)
_cell_angle_gamma                92.720(10)
_cell_formula_units_Z            2
_cell_length_a                   9.4110(10)
_cell_length_b                   10.427(2)
_cell_length_c                   7.930(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      32
_cell_measurement_theta_min      18
_cell_volume                     725.2(2)
_computing_cell_refinement       'Rigaku-AFC software'
_computing_data_collection       'Rigaku-AFC software'
_computing_data_reduction        'Rigaku-AFC software'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick,1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick,1985)'
_diffrn_ambient_temperature      292(2)
_diffrn_measurement_device       'Rigaku-AFC diffractometer'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.034
_diffrn_reflns_av_sigmaI/netI    0.0145
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2422
_diffrn_reflns_theta_max         65.0
_diffrn_reflns_theta_min         4.4
_diffrn_standards_decay_%        <2.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.08
_exptl_absorpt_correction_T_max  0.465
_exptl_absorpt_correction_T_min  0.202
_exptl_absorpt_correction_type   'Gaussian (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.832
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.256
_exptl_crystal_size_mid          0.256
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.970
_refine_diff_density_min         -0.672
_refine_ls_extinction_coef       0.0050(8)
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     185
_refine_ls_number_reflns         2252
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.081
_refine_ls_restrained_S_obs      1.086
_refine_ls_R_factor_all          0.0458
_refine_ls_R_factor_obs          .044
_refine_ls_shift/esd_max         0.030
_refine_ls_shift/esd_mean        0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.1065P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.137
_refine_ls_wR_factor_obs         .1327
_reflns_number_observed          2089
_reflns_number_total             2252
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1166.cif
_cod_data_source_block           Compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '463-465' was changed to '464.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_chemical_melting_point' value '463-465' was changed to '464.0(10)'
- the average value was taken and precision was estimated.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w =
1/[\s^2^(Fo^2^)+(0.1065P)^2^+0.3562P] 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^)+(0.1065P)^2^+0.3562P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               2006628