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_2006106
_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
;
_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
;
 chiral dimethyl-bis([2.2]paracyclophan-4-yl)silane
;
_chemical_temperature_decomposition 180
_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           SHELXL
_cell_angle_alpha                90
_cell_angle_beta                 93.089(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.941(2)
_cell_length_b                   17.694(2)
_cell_length_c                   10.4379(14)
_cell_measurement_reflns_used    63
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      12.5
_cell_measurement_theta_min      4.7
_cell_volume                     2571.0(6)
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0641
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4837
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_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    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1016
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.48
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.206
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.920
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    'H atoms: methyl H atoms rigid, others riding'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         4527
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0780
_refine_ls_R_factor_obs          .0457
_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^)+(0.0599P)^2^] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1144
_refine_ls_wR_factor_obs         .1034
_reflns_number_observed          2972
_reflns_number_total             4530
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            fg1229.cif
_cod_data_source_block           deneb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_temperature_decomposition' since the value had been '180
(dec.)'. The value '180 (dec.)' was changed to '180'.

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 '180
(dec.)'. The value '180 (dec.)' was changed to '180'.

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^)+(0.0599P)^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^)+(0.0599P)^2^]
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               2006106