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_7718843
_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         'C H Cl3, 2(C41 H29 F6 N3 O2), 3[CHCl3]'
_chemical_formula_sum            'C86 H62 Cl12 F12 N6 O4'
_chemical_formula_weight         1896.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -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                94.700(9)
_cell_angle_beta                 97.835(13)
_cell_angle_gamma                98.350(13)
_cell_formula_units_Z            2
_cell_length_a                   15.138(3)
_cell_length_b                   15.4845(18)
_cell_length_c                   18.698(2)
_cell_measurement_reflns_used    29092
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.86
_cell_measurement_theta_min      1.82
_cell_volume                     4272.7(11)
_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  (Sheldrick, 2015)'
_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 0.994
_diffrn_measured_fraction_theta_max 0.967
_diffrn_measurement_details
;
 206 frames, detector distance = 80 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  0.0800
_diffrn_reflns_av_unetI/netI     0.1071
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.967
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            37377
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.967
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.761
_diffrn_reflns_theta_min         2.064
_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    0.469
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.4208
_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    yellow
_exptl_crystal_density_diffrn    1.474
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelette
_exptl_crystal_F_000             1928
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.546
_refine_diff_density_min         -0.616
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       0.0029(5)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2019/2 (Sheldrick 2019)'
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1123
_refine_ls_number_reflns         19498
_refine_ls_number_restraints     238
_refine_ls_restrained_S_all      0.984
_refine_ls_R_factor_all          0.1419
_refine_ls_R_factor_gt           0.0730
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1875
_refine_ls_wR_factor_ref         0.2226
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9541
_reflns_number_total             19498
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00869g2.cif
_cod_data_source_block           kvkd03-chcl3-evap
_cod_depositor_comments
'Adding full bibliography for 7718839--7718844.cif.'
_cod_database_code               7718843
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.955
_shelx_estimated_absorpt_t_min   0.705
_olex2_refinement_description
;
1. Restrained distances
 F8-C55 \\sim F8A-C55
 with sigma of 0.02
 F1-C14A \\sim F1A-C14
 with sigma of 0.02
 F9-C55 \\sim F9A-C55
 with sigma of 0.02
 F3-F1 \\sim F3A-F1A
 with sigma of 0.04
 F1-F2 \\sim F1A-F2A
 with sigma of 0.04
 F8-C55 \\sim F8-C55A
 with sigma of 0.02
 F7-C55 \\sim F7A-C55
 with sigma of 0.02
 F1-C11 \\sim F1A-C11
 with sigma of 0.04
 F3-C14A \\sim F3A-C14
 with sigma of 0.02
 F9-C55 \\sim F9-C55A
 with sigma of 0.02
 F7-C55 \\sim F7-C55A
 with sigma of 0.02
 F2-C14A \\sim F2A-C14
 with sigma of 0.02
 C11-C14A \\sim C11-C14
 with sigma of 0.02
 F3-F2 \\sim F3A-F2A
 with sigma of 0.04
 F3-C11 \\sim F3A-C11
 with sigma of 0.04
 F2-C11 \\sim F2A-C11
 with sigma of 0.04
 C52-C55 \\sim C52-C55A
 with sigma of 0.02
 C55-F8A \\sim C55A-F8A
 with sigma of 0.02
 C55-F9A \\sim C55A-F9A
 with sigma of 0.02
 C55-F7A \\sim C55A-F7A
 with sigma of 0.02
 O3-C59 \\sim O3A-C59A
 with sigma of 0.02
 O3-C62 \\sim O3A-C62A
 with sigma of 0.02
 C60-C61 \\sim C60A-C61A
 with sigma of 0.02
 C60-C59 \\sim C60A-C59A
 with sigma of 0.02
 C56-C46 \\sim C56A-C46
 with sigma of 0.02
 C56-C61 \\sim C56A-C61A
 with sigma of 0.02
 C56-C57 \\sim C56A-C57A
 with sigma of 0.02
 C59-C58 \\sim C59A-C58A
 with sigma of 0.02
 C57-C58 \\sim C57A-C58A
 with sigma of 0.02
 O3-C60 \\sim O3A-C60A
 with sigma of 0.04
 O3-C58 \\sim O3A-C58A
 with sigma of 0.04
 C60-C56 \\sim C60A-C56A
 with sigma of 0.04
 C60-C58 \\sim C60A-C58A
 with sigma of 0.04
 C56-C58 \\sim C56A-C58A
 with sigma of 0.04
 C46-C61 \\sim C46-C61A
 with sigma of 0.04
 C46-C57 \\sim C46-C57A
 with sigma of 0.04
 C61-C59 \\sim C61A-C59A
 with sigma of 0.04
 C61-C57 \\sim C61A-C57A
 with sigma of 0.04
 C59-C57 \\sim C59A-C57A
 with sigma of 0.04
 C59-C62 \\sim C59A-C62A
 with sigma of 0.04
 C56-C61 \\sim C60-C59 \\sim C58-C57
 with sigma of 0.02
2. Restrained planarity
 C56, C61, C60, C59, C58, C57
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
Uanis(F8A) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F9A) \\sim Ueq, Uanis(C55)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F2A) \\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(F1A) \\sim Ueq, Uanis(F3A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(F9A) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(F7A) \\sim Ueq, Uanis(F8A)
\\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C57) \\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C59) \\sim Ueq, Uanis(C60)
\\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C56) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(C56) \\sim Ueq, Uanis(C61) \\sim Ueq, Uanis(C60) \\sim Ueq, Uanis(C59)
\\sim Ueq, Uanis(C58) \\sim Ueq, Uanis(C57) \\sim Ueq, Uanis(O3) \\sim Ueq,
Uanis(C62) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01
Uanis(C56A) \\sim Ueq, Uanis(C57A) \\sim Ueq, Uanis(C61A) \\sim Ueq,
Uanis(C60A) \\sim Ueq, Uanis(C58A) \\sim Ueq, Uanis(C59A) \\sim Ueq, Uanis(O3A)
\\sim Ueq, Uanis(C62A) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(Cl3) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 F8, F9, C55, F7
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
 F1, F3, C14A, F2
 with sigma for 1-2 distances of 0.0001 and sigma for 1-3 distances of 0.0001
5. Others
 Fixed Sof: F3(0.75) O3(0.5) F8(0.75) F1(0.75) F9(0.75) F2(0.75) C60(0.5)
 H60(0.5) C56(0.5) F7(0.75) C61(0.5) H61(0.5) C59(0.5) C57(0.5) H57(0.5)
 C58(0.5) H58(0.5) C14A(0.75) C55(0.75) F8A(0.25) F9A(0.25) F7A(0.25) F2A(0.25)
 F1A(0.25) F3A(0.25) C14(0.25) C55A(0.25) C62(0.5) H62A(0.5) H62B(0.5)
 H62C(0.5) C56A(0.5) C57A(0.5) H57A(0.5) C61A(0.5) H61A(0.5) C60A(0.5)
 H60A(0.5) C59A(0.5) C58A(0.5) H58A(0.5) O3A(0.5) C62A(0.5) H62D(0.5) H62E(0.5)
 H62F(0.5)
6.a Ternary CH refined with riding coordinates:
 C83(H83)
6.b Aromatic/amide H refined with riding coordinates:
 N1(H1), N6(H6), N4(H4), N3(H3), C67(H67), C80(H80), C71(H71), C6(H6A),
 C22(H22), C81(H81), C74(H74), C2(H2), C20(H20), C73(H73), C29(H29), C26(H26),
 C60(H60), C9(H9), C40(H40), C77(H77), C43(H43), C19(H19), C30(H30), C16(H16),
 C70(H70), C78(H78), C1(H1A), C47(H47), C63(H63), C10(H10), C13(H13), C32(H32),
 C33(H33), C50(H50), C54(H54), C39(H39), C42(H42), C17(H17), C61(H61), C36(H36),
  C37(H37), C12(H12), C51(H51), C53(H53), C57(H57), C58(H58), C57A(H57A),
 C61A(H61A), C60A(H60A), C58A(H58A)
6.c Idealised Me refined as rotating group:
 C21(H21A,H21B,H21C), C41(H41A,H41B,H41C), C82(H82A,H82B,H82C), C62(H62A,H62B,
 H62C), C62A(H62D,H62E,H62F)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              59547
_shelx_hkl_checksum              39549
_shelx_fab_checksum              76847
_olex2_submission_special_instructions 'No special instructions were received'