High and Low Rotational Barriers in Metal Tricarbonyl Complexes of 2- and 3-Indenyl Anthracenes and Triptycenes: Rational Design of Molecular Brakes
Nikitin, Kirill; Bothe, Cornelia; Müller-Bunz, Helge; Ortin, Yannick; McGlinchey, Michael J.; Organometallics 31 (2012) 6183–; doi:10.1021/om300512z

data_4079122
_publ_section_title
;
 High and Low Rotational Barriers in Metal Tricarbonyl Complexes of 2- and
 3-Indenyl Anthracenes and Triptycenes: Rational Design of Molecular
 Brakes
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6183
_journal_paper_doi               10.1021/om300512z
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C18 H11 O3 Re'
_chemical_formula_sum            'C18 H11 O3 Re'
_chemical_formula_weight         461.47
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            12
_cell_length_a                   8.3815(4)
_cell_length_b                   10.1729(4)
_cell_length_c                   52.705(2)
_cell_measurement_reflns_used    8046
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      30.60
_cell_measurement_theta_min      2.31
_cell_volume                     4493.8(3)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0375
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       73
_diffrn_reflns_limit_l_min       -74
_diffrn_reflns_number            51259
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.57
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    8.121
_exptl_absorpt_correction_T_max  0.6415
_exptl_absorpt_correction_T_min  0.3394
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 SADABS v.2.10 (Bruker,2003) was used for absorption correction. 
 R(int) for selected reflections was 0.133 before and 0.035 after 
 correction. The Ratio of minimum to maximum transmission is 0.529089. 
 The \l/2 correction factor is 0.0015 
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2616
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.06
_refine_diff_density_max         3.145
_refine_diff_density_min         -3.365
_refine_diff_density_rms         0.257
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.491(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         13490
_refine_ls_number_restraints     291
_refine_ls_restrained_S_all      1.272
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0035P)^2^+60.2519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0950
_refine_ls_wR_factor_ref         0.0955
_reflns_number_gt                13239
_reflns_number_total             13490
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            om300512z_si_002.cif
_cod_data_source_block           mjm237(16)
_cod_database_code               4079122