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_4116665
_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            'C16 H24'
_chemical_formula_weight         216.35
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 115.24(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.619(3)
_cell_length_b                   8.230(2)
_cell_length_c                   12.452(3)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      33.22
_cell_measurement_theta_min      2.98
_cell_volume                     1262.4(6)
_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 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  0.0201
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13610
_diffrn_reflns_theta_max         33.22
_diffrn_reflns_theta_min         2.98
_exptl_absorpt_coefficient_mu    0.063
_exptl_absorpt_correction_T_max  0.9722
_exptl_absorpt_correction_T_min  0.9632
_exptl_absorpt_correction_type   semiempirical
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.138
_exptl_crystal_description       blocks
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.50
_exptl_crystal_size_min          0.45
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.185
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     122
_refine_ls_number_reflns         2401
_refine_ls_number_restraints     27
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0443
_refine_ls_R_factor_gt           0.0393
_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^)+(0.0581P)^2^+0.4277P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1064
_reflns_number_gt                2160
_reflns_number_total             2401
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja973118x_2.cif
_cod_data_source_block           6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.4277P] 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^)+(0.0581P)^2^+0.4277P] 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        1262.4(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4116665