The influence of charge transfer on the emissive properties of pyridine dipyrrolide bismuth complexes.
Deuter, Katharina L.; Vollmar, Katharina; Rieser, Jan; Linseis, Michael; Winter, Rainer F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9921–9929; doi:10.1039/d5dt00869g

data_7718842
_publ_section_title
;
 The influence of charge transfer on the emissive properties of pyridine
 dipyrrolide bismuth complexes.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9921
_journal_page_last               9929
_journal_paper_doi               10.1039/d5dt00869g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         '2(C20.5 H11.5 F6 N1.5), 0.5[C6H6]'
_chemical_formula_sum            'C44 H26 F12 N3'
_chemical_formula_weight         824.68
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2025-02-07
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-09 deposited with the CCDC.	2025-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.385(4)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   25.6962(13)
_cell_length_b                   17.1867(8)
_cell_length_c                   17.4886(9)
_cell_measurement_reflns_used    11244
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.05
_cell_measurement_theta_min      2.37
_cell_volume                     7329.3(7)
_computing_cell_refinement
;
X-Area Recipe 1.33.0.0 (STOE, 2015)
;
_computing_data_collection
;
X-Area WinXpose 2.0.22.0 (STOE, 2016)
;
_computing_data_reduction
;
X-Area Integrate 1.74.2.0 (STOE, 2018)
X-Area LANA 1.75.3.0 (STOE, 2018)
;
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'image plate (34 cm diameter)'
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            'STOE Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
 296 frames, detector distance = 60 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_collimation    '0.5 mm diameter, monocapillary'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_polarisn_norm  0
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0779
_diffrn_reflns_av_unetI/netI     0.0830
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            18693
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.027
_diffrn_reflns_theta_min         2.370
_diffrn_source
'Sealed Mo X-ray tube, 12 x 0.4 mm long-fine focus'
_diffrn_source_current           40
_diffrn_source_power             2.000
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    0.131
_exptl_absorpt_correction_T_max  0.9537
_exptl_absorpt_correction_T_min  0.3852
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE LANA, absorption correction by scaling of reflection intensities.
J. Koziskova, F. Hahn, J. Richter, J. Kozisek, "Comparison of different
absorption corrections on the model structure of tetrakis(\m~2~-acetato)-
diaqua-di-copper(II)", Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136 - 140.
Afterwards a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.495
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3352
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.233
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.259
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     633
_refine_ls_number_reflns         7109
_refine_ls_number_restraints     114
_refine_ls_restrained_S_all      1.011
_refine_ls_R_factor_all          0.1949
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1017P)^2^+6.7137P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1798
_refine_ls_wR_factor_ref         0.2405
_reflns_d_resolution_high        0.810
_reflns_d_resolution_low         8.613
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              31
_reflns_limit_h_min              -31
_reflns_limit_k_max              21
_reflns_limit_k_min              -21
_reflns_limit_l_max              21
_reflns_limit_l_min              -20
_reflns_number_gt                2994
_reflns_number_total             7109
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00869g2.cif
_cod_data_source_block           kvkd04_2
_cod_depositor_comments
'Adding full bibliography for 7718839--7718844.cif.'
_cod_original_cell_volume        7329.3(6)
_cod_database_code               7718842
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.981
_shelx_estimated_absorpt_t_min   0.962
_olex2_refinement_description
;
1. Restrained distances
 F9-C35 \\sim F9A-C35
 with sigma of 0.02
 F5-C21 \\sim F5A-C21
 with sigma of 0.02
 F6-C21 \\sim F6A-C21
 with sigma of 0.02
 F4-C21 \\sim F4A-C21
 with sigma of 0.02
 C35-F7 \\sim C35-F7A
 with sigma of 0.02
 C35-F8 \\sim C35-F8A
 with sigma of 0.02
2. Uiso/Uaniso restraints and constraints
Uanis(F7A) \\sim Ueq, Uanis(F8) \\sim Ueq, Uanis(F8A) \\sim Ueq, Uanis(F9)
\\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(F7) \\sim Ueq, Uanis(F4A) \\sim Ueq,
Uanis(F4) \\sim Ueq, Uanis(F5A) \\sim Ueq, Uanis(F5) \\sim Ueq, Uanis(F6A)
\\sim Ueq, Uanis(F6) \\sim Ueq: with sigma of 0.03 and sigma for terminal atoms
of 0.06
3. Rigid body (RIGU) restrains
 C45, C44, C43, C48, C47, C46
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(F12A)=Sof(F11A)=Sof(F10A)=1-FVAR(1)
 Sof(F12)=Sof(F11)=Sof(F10)=FVAR(1)
 Sof(F7A)=Sof(F8A)=Sof(F9A)=1-FVAR(2)
 Sof(F9)=Sof(F7)=Sof(F8)=FVAR(2)
 Sof(F4A)=Sof(F5A)=Sof(F6A)=1-FVAR(3)
 Sof(F5)=Sof(F4)=Sof(F6)=FVAR(3)
 Fixed Sof: C45(0.5) H45(0.5) C46(0.5) H46(0.5) C47(0.5) H47(0.5) C48(0.5)
 H48(0.5) C43(0.5) H43(0.5) C44(0.5) H44(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N2(H2), N4(H4), C12(H12), C23(H23), C41(H41), C30(H30), C22(H22), C40(H40),
 C13(H13), C6(H6), C9(H9), C10(H10), C27(H27), C31(H31), C37(H37), C38(H38),
 C20(H20), C33(H33), C2(H2A), C19(H19), C34(H34), C1(H1), C17(H17), C16(H16),
 C45(H45), C46(H46), C47(H47), C48(H48), C43(H43), C44(H44)
5.b Fitted hexagon refined as free rotating group:
 C45(C46,C47,C48,C43,C44)
;
_shelx_res_checksum              51064
_shelx_hkl_checksum              17589
_olex2_submission_special_instructions 'No special instructions were received'