A Diastereomeric Pair of Cyclophane Derivatives: Planar–Chiral and <i>meso</i>-Dimethylbis([2.2]paracyclophan-4-yl)silane
Jones, Peter G.; Ernst, Ludger; Dix, Ina; Wittkowski, Lars; Acta Crystallographica Section C 53 (1997) 612–615; doi:10.1107/S0108270197000085

data_2006105
_publ_section_title
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 A Diastereomeric Pair of Cyclophane Derivatives: Planar--Chiral and
 <i>meso</i>-Dimethylbis([2.2]paracyclophan-4-yl)silane
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_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              612
_journal_page_last               615
_journal_paper_doi               10.1107/S0108270197000085
_journal_volume                  53
_journal_year                    1997
_chemical_formula_sum            'C34 H36 Si'
_chemical_formula_weight         472.72
_chemical_name_systematic
meso-dimethyl-bis([2.2]paracyclophan-4-yl)silane
_chemical_temperature_decomposition 254
_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
_cell_angle_alpha                65.191(12)
_cell_angle_beta                 87.299(10)
_cell_angle_gamma                79.709(12)
_cell_formula_units_Z            4
_cell_length_a                   11.115(2)
_cell_length_b                   15.077(3)
_cell_length_c                   17.182(3)
_cell_measurement_reflns_used    64
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      11.5
_cell_measurement_theta_min      3.1
_cell_volume                     2570.3(9)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1991)'
_computing_data_reduction        XSCANS
_computing_molecular_graphics    'XP (Siemens, 1994)'
_computing_publication_material  SHELXL93
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_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  0.0272
_diffrn_reflns_av_sigmaI/netI    0.1774
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9147
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        2
_diffrn_standards_interval_count 247
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.113
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.222
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       tablet
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.76
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.651
_refine_diff_density_min         -0.224
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.788
_refine_ls_goodness_of_fit_obs   1.007
_refine_ls_hydrogen_treatment    'H atoms: methyl H atoms rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     635
_refine_ls_number_reflns         8777
_refine_ls_number_restraints     628
_refine_ls_restrained_S_all      0.768
_refine_ls_restrained_S_obs      0.926
_refine_ls_R_factor_all          0.1511
_refine_ls_R_factor_obs          .0531
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0323P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1106
_refine_ls_wR_factor_obs         .0876
_reflns_number_observed          3765
_reflns_number_total             8779
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1229.cif
_cod_data_source_block           parasil
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '254
(dec.)'. The value '254 (dec.)' was changed to '254'.

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

The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '254
(dec.)'. The value '254 (dec.)' was changed to '254'.

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^)+(0.0323P)^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^)+(0.0323P)^2^]
where P = (Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
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_cod_original_cell_volume        2570.5(8)
_cod_database_code               2006105