Room-temperature phosphorescence and static excimer excitation of pyrene-modified (<i>NCN</i>) pincer bismuth complexes.
Geppert, Marcel; Müller, Michelle; Linseis, Michael; Winter, Rainer F.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 1779–1783; doi:10.1039/d4dt03304c

data_7717790
_publ_section_title
;
 Room-temperature phosphorescence and static excimer excitation of
 pyrene-modified (<i>NCN</i>) pincer bismuth complexes.
;
_journal_issue                   5
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1779
_journal_page_last               1783
_journal_paper_doi               10.1039/d4dt03304c
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C44 H37 Bi N2, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C45.5 H40 Bi Cl3 N2'
_chemical_formula_weight         930.12
_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     iterative
_audit_creation_date             2024-08-08
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-08-12 deposited with the CCDC.	2025-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.972(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0114(6)
_cell_length_b                   20.1875(8)
_cell_length_c                   15.1534(6)
_cell_measurement_reflns_used    22959
_cell_measurement_temperature    100
_cell_measurement_theta_max      27.91
_cell_measurement_theta_min      1.89
_cell_volume                     3885.5(3)
_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 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 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 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 153 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  0.0453
_diffrn_reflns_av_unetI/netI     0.0569
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16241
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.250
_diffrn_reflns_theta_min         2.504
_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    4.779
_exptl_absorpt_correction_T_max  0.3543
_exptl_absorpt_correction_T_min  0.2321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.590
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1844
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.075
_refine_diff_density_max         1.625
_refine_diff_density_min         -1.932
_refine_diff_density_rms         0.241
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.205
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     482
_refine_ls_number_reflns         7021
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.202
_refine_ls_R_factor_all          0.1136
_refine_ls_R_factor_gt           0.0815
_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^)+(0.0217P)^2^+154.7005P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2091
_reflns_d_resolution_high        0.765
_reflns_d_resolution_low         8.134
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              18
_reflns_limit_h_min              -18
_reflns_limit_k_max              26
_reflns_limit_k_min              -26
_reflns_limit_l_max              19
_reflns_limit_l_min              -19
_reflns_number_gt                5268
_reflns_number_total             7021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03304c2.cif
_cod_data_source_block           mg19
_cod_depositor_comments
'Adding full bibliography for 7717790--7717791.cif.'
_cod_original_formula_sum        'C45.50 H40 Bi Cl3 N2'
_cod_database_code               7717790
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.716
_shelx_estimated_absorpt_t_min   0.381
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 C1, C2, C3, C4, C5, C6
 with sigma for 1-2 distances of 0.002 and sigma for 1-3 distances of 0.002
2. Others
 Fixed Sof: Cl1(0.5) Cl2(0.5) C45(0.5) H45A(0.5) H45B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C7(H7A,H7B), C46(H46A,H46B), C45(H45A,H45B)
3.b Aromatic/amide H refined with riding coordinates:
 C31(H31), C24(H24), C34(H34), C14(H14), C25(H25), C30(H30), C40(H40),
 C22(H22), C41(H41), C18(H18), C4(H4), C36(H36), C15(H15), C5(H5), C17(H17),
 C33(H33), C38(H38), C37(H37), C21(H21), C3(H3), C20(H20)
3.c Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C)
;
_shelx_res_checksum              26347
_shelx_hkl_checksum              45309
_olex2_submission_special_instructions 'No special instructions were received'