Ansa [1]Trochrocenophanes and Their Related Unstrained 1,1'-Disubstituted Counterparts: Synthesis and Electronic Structure
Holger Braunschweig; Thomas Kupfer; Matthias Lutz; Krzysztof Radacki; Journal of the American Chemical Society 129 (2007) 8893–8906; doi:10.1021/ja0724947

data_4109668
_publ_contact_author_address
; Institut fuer Anorganische Chemie
Universitaet Wuerzburg
Am Hubland
97074 Wuerzburg, Germany
;
_publ_contact_author_email       H.Braunschweig@mail.uni-wuerzburg.de
_publ_contact_author_fax         +49-931-8884623
_publ_contact_author_name        'Prof. Dr. Holger Braunschweig'
_publ_contact_author_phone       +49-931-8885260
_publ_section_title
;
 Ansa [1]Trochrocenophanes and Their Related Unstrained 1,1'-Disubstituted
 Counterparts: Synthesis and Electronic Structure
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              8893
_journal_page_last               8906
_journal_paper_doi               10.1021/ja0724947
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C48 H68 Cr2 Li4 O6, 2(C4 H8 O)'
_chemical_formula_sum            'C56 H84 Cr2 Li4 O8'
_chemical_formula_weight         1016.99
_chemical_name_common
;
?
;
_chemical_name_systematic
; 
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 94.224(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.2885(3)
_cell_length_b                   28.3264(9)
_cell_length_c                   18.4643(6)
_cell_measurement_reflns_used    8634
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.86
_cell_measurement_theta_min      2.21
_cell_volume                     5366.5(3)
_computing_cell_refinement       'Saint+ ver. 7.12A (Bruker AXS)'
_computing_data_collection       'APEX2 ver. 1.0-27 (Bruker AXS)'
_computing_data_reduction        'Saint+ ver. 7.12A (Bruker AXS)'
_computing_molecular_graphics    'XP ver. 5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'multi-layer mirror'
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0644
_diffrn_reflns_av_sigmaI/netI    0.0376
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            44428
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.54
_diffrn_reflns_theta_min         1.32
_exptl_absorpt_coefficient_mu    0.457
_exptl_absorpt_correction_T_max  0.973
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs 2004/1 (Brucker Nonius 2004)'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.259
_exptl_crystal_description       block
_exptl_crystal_F_000             2176
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.541
_refine_diff_density_min         -0.428
_refine_diff_density_rms         0.080
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     782
_refine_ls_number_reflns         11106
_refine_ls_number_restraints     936
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0765
_refine_ls_R_factor_gt           0.0675
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1366P)^2^+1.1110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2253
_reflns_number_gt                10432
_reflns_number_total             11106
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0724947si20070410_071649.cif
_cod_data_source_block           kr095
_cod_original_sg_symbol_Hall     '-P 2yn '
_cod_database_code               4109668