A New Rotane Family: Synthesis, Structure, Conformation, and Dynamics of [3.4]-, [4.4]-, [5.4]-, and [6.4]Rotane1
Lutz Fitjer; Christoph Steeneck; Said Gaini-Rahimi; Ulrike Schröder; Karl Justus; Peter Puder; Martin Dittmer; Carla Hassler; Jörg Weiser; Mathias Noltemeyer; Markus Teichert; Journal of the American Chemical Society 120 (1998) 317–328; doi:10.1021/ja973118x

data_4116667
_publ_section_title
;
 A New Rotane Family: Synthesis, Structure, Conformation, and Dynamics of
 [3.4]-, [4.4]-, [5.4]-, and [6.4]Rotane1
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              317
_journal_page_last               328
_journal_paper_doi               10.1021/ja973118x
_journal_volume                  120
_journal_year                    1998
_chemical_formula_sum            'C24 H36'
_chemical_formula_weight         324.53
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.08(1)
_cell_angle_beta                 74.08(1)
_cell_angle_gamma                76.60(1)
_cell_formula_units_Z            1
_cell_length_a                   7.666(2)
_cell_length_b                   7.983(1)
_cell_length_c                   8.208(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.81
_cell_measurement_theta_min      2.72
_cell_volume                     446.17(17)
_computing_cell_refinement       'Siemens SAINT (V. 4.050, Siemens 1996)'
_computing_data_collection       'Siemens SMART (V. 4.050, Siemens 1996)'
_computing_data_reduction        'Siemens SAINT (V. 4.050, Siemens 1996)'
_computing_molecular_graphics    'Siemens SHELXTL (V. 5.06)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean '8.192 pixels/mm'
_diffrn_measurement_device_type
;
 Stoe-Siemens-Huber four circle diffractometer
;
_diffrn_measurement_method       'phi and omega scan'
_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  0.0231
_diffrn_reflns_av_sigmaI/netI    0.0250
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5947
_diffrn_reflns_theta_max         29.81
_diffrn_reflns_theta_min         2.72
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_T_max  0.9867
_exptl_absorpt_correction_T_min  0.9610
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.208
_exptl_crystal_description       plates
_exptl_crystal_F_000             180
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.073(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2320
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0476
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.1330P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1098
_refine_ls_wR_factor_ref         0.1149
_reflns_number_gt                2006
_reflns_number_total             2320
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja973118x_4.cif
_cod_data_source_block           8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0617P)^2^+0.1330P] 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^)+(0.0617P)^2^+0.1330P] 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               4116667