Novel Products from the Rearrangement of Some [<i>n</i>.3.1]Propellanes
Mackay, Maureen F.; Banwell, Martin G.; Pallich, Susanne; Phyland, James R.; Acta Crystallographica Section C 53 (1997) 2000–2002; doi:10.1107/S0108270197010044

data_2006888
_publ_section_title
;
 Novel Products from the Rearrangement of Some
 [<i>n</i>.3.1]Propellanes
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              2000
_journal_page_last               2002
_journal_paper_doi               10.1107/S0108270197010044
_journal_volume                  53
_journal_year                    1997
_chemical_formula_moiety         'C12 H13 Cl3 O'
_chemical_formula_structural     'C12 H13 C13 O'
_chemical_formula_sum            'C12 H13 Cl3 O'
_chemical_formula_weight         279.59
_chemical_melting_point          411.0(10)
_chemical_name_systematic
;
7-Methoxy-4,4,6-trichloro-2,4,5,6-tetrahydro-3H-3a,5-meth-anoazulene
;
_space_group_IT_number           33
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_audit_creation_method           'SHELXL-93 (Sheldrick, 1993)'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.8050(10)
_cell_length_b                   13.2250(10)
_cell_length_c                   13.9020(10)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      37
_cell_measurement_theta_min      19
_cell_volume                     1251.1(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'
_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  0.0
_diffrn_reflns_av_sigmaI/netI    0.0
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1069
_diffrn_reflns_theta_max         65
_diffrn_reflns_theta_min         4.6
_diffrn_standards_decay_%        <1.5
_diffrn_standards_interval_count 50
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.43
_exptl_absorpt_correction_T_max  0.479
_exptl_absorpt_correction_T_min  0.283
_exptl_absorpt_correction_type   'Gaussian (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_meas      1.470(10)
_exptl_crystal_density_method    'flotation in K~2~[HgI~4~]'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             576.0
_exptl_crystal_size_max          0.173
_exptl_crystal_size_mid          0.109
_exptl_crystal_size_min          0.071
_refine_diff_density_max         0.401
_refine_diff_density_min         -0.336
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.05(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.031
_refine_ls_goodness_of_fit_obs   1.074
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     145
_refine_ls_number_reflns         1069
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.031
_refine_ls_restrained_S_obs      1.074
_refine_ls_R_factor_all          0.057
_refine_ls_R_factor_obs          .052
_refine_ls_shift/esd_max         0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0758P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.125
_refine_ls_wR_factor_obs         .121
_reflns_number_observed          942
_reflns_number_total             1069
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ta1168.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '410-412' was changed to '411.0(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 '410-412' was changed to '411.0(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^)+(0.0758P)^2^] 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^)+(0.0758P)^2^]
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               2006888