Steric control of the in/out sense of bridgehead substituents in macrobicyclic compounds: isolation of new 'crossed chain' variants of in/out isomers
Michael Stollenz; Deeb Taher; Nattamai Bhuvanesh; Joseph H. Reibenspies; Zuzana Baranova; John A. Gladysz; Chem.Commun. 51 (2015) 16053–; doi:10.1039/C5cc05620A

data_7118012
_publ_section_title
;
 Steric control of the in/out sense of bridgehead substituents in
 macrobicyclic compounds: isolation of new 'crossed chain' variants of
 in/out isomers
;
_journal_name_full               Chem.Commun.
_journal_page_first              16053
_journal_paper_doi               10.1039/C5cc05620A
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C54 H64 Au P'
_chemical_formula_weight         940.99
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-07-03 deposited with the CCDC.
2015-08-28 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.438(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.8975(10)
_cell_length_b                   12.5051(9)
_cell_length_c                   28.706(3)
_cell_measurement_reflns_used    4333
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      31.31
_cell_measurement_theta_min      3.43
_cell_volume                     4629.7(7)
_computing_cell_refinement       'Bruker FRAMBO'
_computing_data_collection       'Bruker FRAMBO'
_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      110(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'MWPC area detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1607
_diffrn_reflns_av_sigmaI/netI    0.0825
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            94166
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.43
_exptl_absorpt_coefficient_mu    6.538
_exptl_absorpt_correction_T_max  0.9375
_exptl_absorpt_correction_T_min  0.5609
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            'colorless '
_exptl_crystal_density_diffrn    1.350
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'plate     '
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.523
_refine_diff_density_min         -1.226
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     639
_refine_ls_number_reflns         6802
_refine_ls_number_restraints     483
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0742
_refine_ls_R_factor_gt           0.0470
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0520P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1096
_reflns_number_gt                4582
_reflns_number_total             6802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c5cc05620a2.cif
_cod_data_source_block           jga
_cod_original_cell_volume        4629.6(6)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_database_code               7118012