Nature of the heavy formal double bonds As[double bond, length as m-dash]Ch, Sb[double bond, length as m-dash]Ch and Bi[double bond, length as m-dash]Ch (Ch = S, Se, Te) in NCN-pincer supported arsinidene, stibinidene and bismuthinidene chalcogenides.
Meyer, Fabio; Siumbeli, Arina; Dostál, Libor; Hupf, Emanuel; Beckmann, Jens; Chemical science 16 (2025) 16232–16239; doi:10.1039/d5sc03320a

data_1575129
_publ_section_title
;
 Nature of the heavy formal double bonds As[double bond, length as
 m-dash]Ch, Sb[double bond, length as m-dash]Ch and Bi[double bond, length
 as m-dash]Ch (Ch = S, Se, Te) in NCN-pincer supported arsinidene,
 stibinidene and bismuthinidene chalcogenides.
;
_journal_issue                   35
_journal_name_full               'Chemical science'
_journal_page_first              16232
_journal_page_last               16239
_journal_paper_doi               10.1039/d5sc03320a
_journal_volume                  16
_journal_year                    2025
_chemical_formula_moiety         'C48 H45 Bi N2 P2 Te, 3(C4 H8 O)'
_chemical_formula_sum            'C60 H69 Bi N2 O3 P2 Te'
_chemical_formula_weight         1264.69
_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             2024-09-10
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-04-25 deposited with the CCDC.	2025-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.585(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1844(7)
_cell_length_b                   15.2867(12)
_cell_length_c                   34.707(2)
_cell_measurement_reflns_used    9243
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      27.14
_cell_measurement_theta_min      2.22
_cell_volume                     5356.1(6)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/4 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0907
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            171563
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.024
_diffrn_reflns_theta_max         25.024
_diffrn_reflns_theta_min         2.026
_diffrn_source                   'microfocus Ims X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.932
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5300
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1291 before and 0.0832 after correction.
The Ratio of minimum to maximum transmission is 0.7105.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.568
_exptl_crystal_description       plate
_exptl_crystal_F_000             2528
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.884
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     637
_refine_ls_number_reflns         9450
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0393
_refine_ls_R_factor_gt           0.0340
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0190P)^2^+18.4176P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0716
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8574
_reflns_number_total             9450
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           meyerf240905_0m
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_original_cell_volume        5356.1(7)
_cod_database_code               1575129
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.828
_shelx_estimated_absorpt_t_min   0.340
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H92A(0.45) H92B(0.45) H92C(0.55) H92D(0.55) C91(0.45) H91A(0.45)
 H91B(0.45) H89A(0.45) H89B(0.45) H89C(0.55) H89D(0.55) C90(0.55) H90A(0.55)
 H90B(0.55)
3.a Secondary CH2 refined with riding coordinates:
 C88(H88A,H88B), C87(H87A,H87B), C92(H92A,H92B), C92(H92C,H92D), C86(H86A,
 H86B), C80(H80A,H80B), C91(H91A,H91B), C89(H89A,H89B), C89(H89C,H89D),
 C85(H85A,H85B), C84(H84A,H84B), C83(H83A,H83B), C81(H81A,H81B), C82(H82A,H82B),
  C90(H90A,H90B)
3.b Aromatic/amide H refined with riding coordinates:
 C72(H72), C13(H13), C35(H35), C12(H12), C14(H14), C54(H54), C31(H31),
 C25(H25), C23(H23), C41(H41), C74(H74), C52(H52), C21(H21), C51(H51), C64(H64),
  C55(H55), C45(H45), C62(H62), C42(H42), C24(H24), C22(H22), C34(H34),
 C32(H32), C53(H53), C44(H44), C33(H33), C43(H43)
3.c Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C77(H77A,H77B,H77C), C66(H66A,H66B,
 H66C), C78(H78A,H78B,H78C), C67(H67A,H67B,H67C)
;
_shelx_res_checksum              96437
_olex2_submission_special_instructions 'No special instructions were received'