Room-temperature near-infrared phosphorescence of a bismuthinidene N,C,N pincer complex.
Deuter, Katharina L.; Balaba, Daisy J. J.; Linseis, Michael; Winter, Rainer F.; Chemical communications (Cambridge, England) 61 (2025) 3548–3551; doi:10.1039/d5cc00127g

data_7134204
_publ_section_title
;
 Room-temperature near-infrared phosphorescence of a bismuthinidene N,C,N
 pincer complex.
;
_journal_issue                   17
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3548
_journal_page_last               3551
_journal_paper_doi               10.1039/d5cc00127g
_journal_volume                  61
_journal_year                    2025
_chemical_formula_moiety         'C26 H27 Bi Br2 N2, 0.25[CH2Cl2]'
_chemical_formula_sum            'C26.25 H27.5 Bi Br2 Cl0.5 N2'
_chemical_formula_weight         757.53
_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     dual
_audit_creation_date             2024-10-04
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-10-30 deposited with the CCDC.	2025-01-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.531(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2163(6)
_cell_length_b                   8.2052(2)
_cell_length_c                   28.5094(12)
_cell_measurement_reflns_used    19636
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      2.51
_cell_volume                     3071.6(2)
_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 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 0.980
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_details
;
 138 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  0.0460
_diffrn_reflns_av_unetI/netI     0.0444
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.979
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            13046
_diffrn_reflns_point_group_measured_fraction_full 0.980
_diffrn_reflns_point_group_measured_fraction_max 0.979
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.500
_diffrn_reflns_theta_min         2.510
_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    8.399
_exptl_absorpt_correction_T_max  0.8745
_exptl_absorpt_correction_T_min  0.1768
_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, "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.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1442
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: CD2Cl2'
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.01
_refine_diff_density_max         2.165
_refine_diff_density_min         -2.436
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         6242
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0489
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0849P)^2^+12.4152P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1319
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4915
_reflns_number_total             6242
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5cc00127g2.cif
_cod_data_source_block           kd109-nmr
_cod_depositor_comments
'Adding full bibliography for 7134204--7134205.cif.'
_cod_original_formula_sum        'C26.25 H27.50 Bi Br2 Cl0.50 N2'
_cod_database_code               7134204
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.921
_shelx_estimated_absorpt_t_min   0.102
_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
2.a Aromatic/amide H refined with riding coordinates:
 C1(H1), C15(H15), C2(H2), C24(H24), C11(H11), C22(H22), C9(H9), C23(H23),
 C10(H10)
2.b Idealised Me refined as rotating group:
 C27(H27A,H27B,H27C), C19(H19A,H19B,H19C), C6(H6A,H6B,H6C), C13(H13A,H13B,
 H13C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 42 electrons were 
found in a volume of 800\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
0.25[CH2Cl2] per formula unit 
which account for 42 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              82886
_shelx_hkl_checksum              84263
_shelx_fab_checksum              49165
_olex2_submission_special_instructions 'No special instructions were received'