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_4135505
_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         'C18 H17 Bi N2, 2(C F3 O3 S), 2(H2 O)'
_chemical_formula_sum            'C20 H21 Bi F6 N2 O8 S2'
_chemical_formula_weight         804.49
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_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                 97.887(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.628(14)
_cell_length_b                   15.700(12)
_cell_length_c                   19.843(15)
_cell_measurement_reflns_used    9479
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      26.521
_cell_measurement_theta_min      2.583
_cell_volume                     5440(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    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  Stoe
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0686
_diffrn_reflns_av_unetI/netI     0.0554
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            56901
_diffrn_reflns_theta_full        26.72
_diffrn_reflns_theta_max         26.72
_diffrn_reflns_theta_min         1.45
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    6.723
_exptl_absorpt_correction_T_max  0.3466
_exptl_absorpt_correction_T_min  0.3466
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.964
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         2.765
_refine_diff_density_min         -0.977
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     719
_refine_ls_number_reflns         11238
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0653
_refine_ls_R_factor_gt           0.0398
_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^)+(0.0303P)^2^+16.6988P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0838
_refine_ls_wR_factor_ref         0.0930
_reflns_number_gt                8334
_reflns_number_total             11238
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0c12015_si_002.cif
_cod_data_source_block           1
_cod_depositor_comments
;
Adding full bibliography for 4135504--4135506.cif.

2025-07-29
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C40 H42 Bi2 F12 N4 O16 S4'
_cod_original_formula_weight         1608.98
_cod_original_formula_moiety         '2(C18 H17 Bi N2), 4(C F3 O3 S), 4(H2 O)'
_cod_original_formula_units_Z            4
_cod_database_code               4135505
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H,H) groups
2.a Free rotating group:
 O13(H13A,H13B), O14(H14A,H14B), O16(H16A,H16B), O15(H15A,H15B)
2.b Aromatic/amide H refined with riding coordinates:
 C8(H8), C2(H2), C11(H11), C4(H4), C5(H5), C23(H23), C21(H21), C29(H29),
 C26(H26), C20(H20), C9(H9), C14(H14), C18(H18), C17(H17), C15(H15), C16(H16),
 C33(H33), C28(H28), C32(H32), C35(H35), C34(H34), C36(H36)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C30(H30A,H30B,H30C), C3(H3A,H3B,H3C), C19(H19A,H19B,H19C)
;
_olex2_submission_special_instructions 'No special instructions were received'