Determining the Conformational Landscape of σ and π Coupling Using para-Phenylene and "Aviram-Ratner" Bridges.
Stasiw, Daniel E.; Zhang, Jinyuan; Wang, Guangbin; Dangi, Ranjana; Stein, Benjamin W.; Shultz, David A.; Kirk, Martin L.; Wojtas, Lukasz; Sommer, Roger D.; Journal of the American Chemical Society 137 (2015) 9222–9225; doi:10.1021/jacs.5b04629

data_4124138
_publ_section_title
;
 Determining the Conformational Landscape of \s and \p Coupling Using
 para-Phenylene and &quot;Aviram-Ratner&quot; Bridges.
;
_journal_issue                   29
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9222
_journal_page_last               9225
_journal_paper_doi               10.1021/jacs.5b04629
_journal_volume                  137
_journal_year                    2015
_chemical_formula_moiety         'C66 H81 B N8 O4 Zn, C6 H6'
_chemical_formula_sum            'C72 H87 B N8 O4 Zn'
_chemical_formula_weight         1204.67
_chemical_name_common            DES8-81-3
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                90
_cell_angle_beta                 108.948(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9485(5)
_cell_length_b                   34.5936(13)
_cell_length_c                   14.2895(6)
_cell_measurement_reflns_used    9506
_cell_measurement_temperature    110.(2)
_cell_measurement_theta_max      27.9457
_cell_measurement_theta_min      2.3217
_cell_volume                     6521.5(4)
_computing_cell_refinement       'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_data_collection       'Bruker Instrument Service v2013.12.0.0'
_computing_data_reduction        'SAINT V8.34A (Bruker AXS Inc., 2013)'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      110.(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker-Nonius X8 Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0528
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -49
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            138066
_diffrn_reflns_theta_full        30.54
_diffrn_reflns_theta_max         30.54
_diffrn_reflns_theta_min         1.77
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    0.432
_exptl_absorpt_correction_T_max  0.94
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2012/1 (Bruker AXS Inc.)'
_exptl_crystal_colour            grey-purple
_exptl_crystal_density_diffrn    1.227
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.383
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.154
_refine_diff_density_max         0.574
_refine_diff_density_min         -0.549
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     813
_refine_ls_number_reflns         19942
_refine_ls_number_restraints     44
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0766
_refine_ls_R_factor_gt           0.0536
_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^)+(0.0538P)^2^+6.0187P]
where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1254
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                15256
_reflns_number_total             19942
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja5b04629_si_002.cif
_cod_data_source_block           I
_cod_depositor_comments
'Adding full bibliography for 4124134--4124138.cif.'
_cod_database_code               4124138
_shelx_res_checksum              51796
_shelx_hkl_checksum              15092