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_1575131
_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 Cl2 N2 P2, 0.5[CH2Cl2]'
_chemical_formula_sum            'C48.5 H46 Bi Cl3 N2 P2'
_chemical_formula_weight         1034.14
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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                 110.717(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.2659(14)
_cell_length_b                   19.0440(15)
_cell_length_c                   16.1671(14)
_cell_measurement_reflns_used    9696
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.45
_cell_volume                     4684.2(7)
_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    'SHELXS  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Venture D8'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0949
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            184799
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         33.141
_diffrn_reflns_theta_min         2.139
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.037
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.5947
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0988 before and 0.0660 after correction.
The Ratio of minimum to maximum transmission is 0.8801.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.466
_exptl_crystal_description       block
_exptl_crystal_F_000             2060
_exptl_crystal_size_max          0.232
_exptl_crystal_size_mid          0.188
_exptl_crystal_size_min          0.097
_refine_diff_density_max         1.069
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.140
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         17843
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0336
_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^)+(0.0383P)^2^+2.2602P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0863
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13977
_reflns_number_total             17843
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           siumbelia230504_0ma
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_original_formula_sum        'C48.50 H46 Bi Cl3 N2 P2'
_cod_database_code               1575131
_shelx_shelxl_version_number     2016/4
_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:
 C14(H14), C23(H23), C25(H25), C24(H24), C12(H12), C21(H21), C64(H64),
 C13(H13), C22(H22), C41(H41), C51(H51), C35(H35), C55(H55), C62(H62), C42(H42),
  C52(H52), C31(H31), C53(H53), C72(H72), C74(H74), C46(H46), C54(H54),
 C43(H43), C33(H33), C34(H34), C32(H32), C44(H44)
2.b Idealised Me refined as rotating group:
 C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C66(H66A,H66B,H66C), C78(H78A,H78B,
 H78C), C67(H67A,H67B,H67C), C77(H77A,H77B,H77C)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              75193
_shelx_fab_checksum              63076
_olex2_submission_special_instructions 'No special instructions were received'