A <i>gem</i>-Dichloro[4.3.1]propellane and a <i>gem</i>-Dichloro[5.3.1]propellenone
Mackay, Maureen F.; Banwell, Martin G.; Pallich, Susanne; Phyland, James R.; Acta Crystallographica Section C 54 (1998) 378–380; doi:10.1107/S0108270197014893

data_2007082
_publ_section_title
;
 A <i>gem</i>-Dichloro[4.3.1]propellane and a
 <i>gem</i>-Dichloro[5.3.1]propellenone
;
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              378
_journal_page_last               380
_journal_paper_doi               10.1107/S0108270197014893
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         'C12 H13 Cl3 O'
_chemical_formula_structural     'C12 H13 Cl3 O'
_chemical_formula_sum            'C12 H13 Cl3 O'
_chemical_formula_weight         279.6
_chemical_melting_point          346.5(5)
_chemical_name_systematic
;
(3a\a,7a\a)-Chloromethyl-8,8-dichloro-2,3-dihydro-5-methoxy-3a,7a-methano-
1H-indene
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           ' SHELXL-93 (Sheldrick, 1993)'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.11(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.831(3)
_cell_length_b                   9.817(2)
_cell_length_c                   13.488(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    292(2)
_cell_measurement_theta_max      28.1
_cell_measurement_theta_min      16.5
_cell_volume                     1244.1(6)
_computing_cell_refinement       'Rigaku AFC Software'
_computing_data_collection
'Rigaku AFC Software (Rigaku Corporation, 1974)'
_computing_data_reduction        'Rigaku AFC Software'
_computing_molecular_graphics    'ORTEPII (Johnson,1976)'
_computing_publication_material  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELX76 (Sheldrick, 1976)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_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  0.049
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2236
_diffrn_reflns_theta_max         65.1
_diffrn_reflns_theta_min         4.9
_diffrn_standards_decay_%        <12
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.47
_exptl_absorpt_correction_T_max  '0.342 (0.305)'
_exptl_absorpt_correction_T_min  '0.189 (0.104)'
_exptl_absorpt_correction_type   'gaussian (SHELX76; Sheldrick, 1976)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.493
_exptl_crystal_density_meas      1.480(10)
_exptl_crystal_density_method    flotation
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             576.0
_exptl_crystal_size_max          '0.145 (0.195)'
_exptl_crystal_size_mid          '0.140 (0.192)'
_exptl_crystal_size_min          '0.042 (0.128)'
_refine_diff_density_max         0.284
_refine_diff_density_min         -0.378
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.152
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     158
_refine_ls_number_reflns         2053
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.152
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.062
_refine_ls_R_factor_obs          .050
_refine_ls_shift/esd_max         0.008
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.5971P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.145
_refine_ls_wR_factor_obs         .119
_reflns_number_observed          1688
_reflns_number_total             2053
_reflns_observed_criterion       I>2sigma(I)
_cod_data_source_file            ha1196.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value '346-347' was changed to '346.5(5)' -
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 '346-347' was changed to '346.5(5)' -
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^)+(0.0622P)^2^+0.5971P] 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^)+(0.0622P)^2^+0.5971P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1244.1(5)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2007082