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_4116664
_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            'C25 H36 O2'
_chemical_formula_weight         368.54
_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
_cell_angle_alpha                87.96(10)
_cell_angle_beta                 89.90(10)
_cell_angle_gamma                60.54(10)
_cell_formula_units_Z            2
_cell_length_a                   8.395(10)
_cell_length_b                   8.475(15)
_cell_length_c                   16.053(30)
_cell_measurement_reflns_used    40
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12
_cell_measurement_theta_min      10
_cell_volume                     994(3)
_computing_cell_refinement       'STOE DIF4'
_computing_data_collection       'STOE DIF4'
_computing_data_reduction        'STOE REDU4'
_computing_molecular_graphics    'Siemens SHELXTL (V. 5.06)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Stoe-Siemens-AED four circle diffractometer'
_diffrn_measurement_method       'Profile data from 2theta/omega'
_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  0.1570
_diffrn_reflns_av_sigmaI/netI    0.0562
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       6
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2568
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         3.68
_diffrn_standards_interval_time  90
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.075
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.232
_exptl_crystal_description       blocks
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.70
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.50
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.248
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.043
_refine_ls_goodness_of_fit_obs   1.116
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.087
_refine_ls_restrained_S_obs      1.116
_refine_ls_R_factor_all          0.1314
_refine_ls_R_factor_obs          0.0930
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+2.3730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2896
_refine_ls_wR_factor_obs         0.2386
_reflns_number_observed          1687
_reflns_number_total             2545
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja973118x_1.cif
_cod_data_source_block           25'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1270P)^2^+2.3730P] 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^)+(0.1270P)^2^+2.3730P] 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        993.7(22)
_cod_database_code               4116664