Phosphorescent Bismoviologens for Electrophosphorochromism and Visible Light-Induced Cross-Dehydrogenative Coupling.
Ma, Wenqiang; Xu, Letian; Zhang, Sikun; Li, Guoping; Ma, Tianyu; Rao, Bin; Zhang, Mingming; He, Gang; Journal of the American Chemical Society 143 (2021) 1590–1597; doi:10.1021/jacs.0c12015

data_4135504
_publ_section_title
;
 Phosphorescent Bismoviologens for Electrophosphorochromism and Visible
 Light-Induced Cross-Dehydrogenative Coupling.
;
_journal_issue                   3
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1590
_journal_page_last               1597
_journal_paper_doi               10.1021/jacs.0c12015
_journal_volume                  143
_journal_year                    2021
_chemical_formula_moiety         'C24 H17 Bi N2 S2, 2(C F3 O3 S), C2 H3 N'
_chemical_formula_sum            'C28 H20 Bi F6 N3 O6 S4'
_chemical_formula_weight         945.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-11-10
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 99.641(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.9686(15)
_cell_length_b                   17.018(2)
_cell_length_c                   14.8907(17)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.747
_cell_measurement_theta_min      2.270
_cell_volume                     3240.0(7)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  Stoe
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            34706
_diffrn_reflns_theta_full        26.78
_diffrn_reflns_theta_max         26.78
_diffrn_reflns_theta_min         1.83
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    5.781
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.5749
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.939
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1832
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.613
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     453
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0310
_refine_ls_R_factor_gt           0.0235
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0214P)^2^+9.2204P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0557
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                5977
_reflns_number_total             6877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0c12015_si_004.cif
_cod_data_source_block           1_pl
_cod_depositor_comments
'Adding full bibliography for 4135504--4135506.cif.'
_cod_original_cell_volume        3240.0(6)
_cod_database_code               4135504
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C0AA \\sim C1 \\sim C2 \\sim S0AA \\sim C4: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02
3. Others
 Sof(H2B)=Sof(H1B)=Sof(S1)=Sof(C3)=Sof(H3)=1-FVAR(1)
 Sof(H2A)=Sof(H1A)=Sof(S0AA)=Sof(C0AA)=Sof(H0AA)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C21(H21), C16(H16), C23(H23), C24(H24), C20(H20), C17(H17), C2(H2B),
  C2(H2A), C12(H12), C6(H6), C5(H5), C1(H1B), C1(H1A), C13(H13), C14(H14),
 C8(H8), C18(H18), C3(H3), C0AA(H0AA)
4.b Idealised Me refined as rotating group:
 C28(H28A,H28B,H28C)
;
_olex2_submission_special_instructions 'No special instructions were received'