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_7717791
_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         'C26 H31 Bi Cl2 N2, C5 H12'
_chemical_formula_sum            'C31 H43 Bi Cl2 N2'
_chemical_formula_weight         723.55
_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             2024-02-22
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-08-12 deposited with the CCDC.	2025-01-08 downloaded from the CCDC.
;
_cell_angle_alpha                113.090(3)
_cell_angle_beta                 92.143(3)
_cell_angle_gamma                98.505(3)
_cell_formula_units_Z            2
_cell_length_a                   8.0167(3)
_cell_length_b                   13.3464(5)
_cell_length_c                   15.4903(6)
_cell_measurement_reflns_used    11906
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.14
_cell_measurement_theta_min      1.72
_cell_volume                     1499.52(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
;
STOE & Cie GmbH, X-Area, software package for collecting single-crystal or
multi-domain crystal data on STOE area-detector diffractometers, for image 
processing, for the correction and scaling of reflection intensities and 
for outlier rejection, version 1.86, Darmstadt 2018
;
_computing_structure_refinement  'SHELXL 2018/3 (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 0.995
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_details
;
 224 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  0.0477
_diffrn_reflns_av_unetI/netI     0.0600
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13209
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.552
_diffrn_reflns_theta_min         1.719
_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    6.079
_exptl_absorpt_correction_T_max  0.0928
_exptl_absorpt_correction_T_min  0.0589
_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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.602
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             720
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: dichloromethane, pentane'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.434
_refine_diff_density_min         -2.982
_refine_diff_density_rms         0.270
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.140
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.140
_refine_ls_R_factor_all          0.0827
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0133P)^2^+30.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1191
_refine_ls_wR_factor_ref         0.1456
_reflns_d_resolution_high        0.768
_reflns_d_resolution_low         11.844
_reflns_Friedel_coverage         0.000
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              17
_reflns_limit_k_min              -17
_reflns_limit_l_max              20
_reflns_limit_l_min              -20
_reflns_number_gt                5518
_reflns_number_total             6856
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03304c2.cif
_cod_data_source_block           mmg17-2
_cod_depositor_comments
'Adding full bibliography for 7717790--7717791.cif.'
_cod_original_cell_volume        1499.52(10)
_cod_database_code               7717791
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.751
_shelx_estimated_absorpt_t_min   0.462
_olex2_refinement_description
;
1.a Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C29(H29A,H29B), C30(H30A,H30B), C7(H7A,H7B), C28(H28A,H28B)
1.b Aromatic/amide H refined with riding coordinates:
 C21(H21), C20(H20), C15(H15), C14(H14), C13(H13), C17(H17)
1.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C9(H9A,H9B,H9C), C11(H11A,H11B,H11C), C26(H26A,H26B,
 H26C), C8(H8A,H8B,H8C), C24(H24A,H24B,H24C), C31(H31A,H31B,H31C), C25(H25A,
 H25B,H25C), C27(H27A,H27B,H27C)
;
_shelx_res_checksum              74604
_shelx_hkl_checksum              60764
_olex2_submission_special_instructions 'No special instructions were received'