Synthesis, Structure, and Photochemical Behavior of [5]Heli-viologen Isomers.
Zhang, Xiaoping; Clennan, Edward L.; Arulsamy, Navamoney; Weber, Rachael; Weber, Jacob; The Journal of organic chemistry 81 (2016) 5474–5486; doi:10.1021/acs.joc.6b00835

data_4032011
_publ_section_title
;
 Synthesis, Structure, and Photochemical Behavior of [5]Heli-viologen
 Isomers.
;
_journal_issue                   13
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              5474
_journal_page_last               5486
_journal_paper_doi               10.1021/acs.joc.6b00835
_journal_volume                  81
_journal_year                    2016
_chemical_formula_moiety         'C24 H18 N2, 2(B F4), C2 H3 N'
_chemical_formula_sum            'C24 H21 B2 F8 N3'
_chemical_formula_weight         525.06
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 115.335(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.7449(6)
_cell_length_b                   19.7482(6)
_cell_length_c                   11.4956(3)
_cell_measurement_reflns_used    8726
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      34.77
_cell_measurement_theta_min      2.75
_cell_volume                     4666.9(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0333
_diffrn_reflns_av_unetI/netI     0.0296
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39271
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.727
_diffrn_reflns_theta_min         2.055
_exptl_absorpt_coefficient_mu    0.133
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.7058
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SAINT'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          0.471
_exptl_crystal_size_mid          0.232
_exptl_crystal_size_min          0.210
_refine_diff_density_max         0.952
_refine_diff_density_min         -0.503
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         9306
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0989
_refine_ls_R_factor_gt           0.0745
_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^)+(0.1517P)^2^+2.6571P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2156
_refine_ls_wR_factor_ref         0.2443
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6598
_reflns_number_total             9306
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo6b00835_si_002.cif
_cod_data_source_block           xz03a
_cod_database_code               4032011
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.935
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              71660
_shelx_hkl_checksum              24397