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_1575132
_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 As Cl N2 P2, As2 Cl4 O, Cl, 0.5(C6 H4 F2), 1[C6H4F2]'
_chemical_formula_sum            'C57 H51 As3 Cl6 F3 N2 O P2'
_chemical_formula_weight         1336.40
_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
;
2025-04-25 deposited with the CCDC.	2025-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                106.082(2)
_cell_angle_beta                 93.732(2)
_cell_angle_gamma                105.763(2)
_cell_formula_units_Z            4
_cell_length_a                   12.9688(9)
_cell_length_b                   18.3595(12)
_cell_length_c                   26.9379(16)
_cell_measurement_reflns_used    9795
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.26
_cell_volume                     5862.5(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    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_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  0.0935
_diffrn_reflns_av_unetI/netI     0.0723
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            218773
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.560
_diffrn_reflns_theta_min         1.938
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.078
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6748
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0884 before and 0.0698 after correction.
The Ratio of minimum to maximum transmission is 0.9044.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.514
_exptl_crystal_description       block
_exptl_crystal_F_000             2692
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.17
_refine_diff_density_max         1.635
_refine_diff_density_min         -0.799
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1201
_refine_ls_number_reflns         35882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0837
_refine_ls_R_factor_gt           0.0451
_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^)+(0.0525P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1023
_refine_ls_wR_factor_ref         0.1150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23282
_reflns_number_total             35882
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           siumbelia230424_0m
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_database_code               1575132
_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:
 C84(H84), C13(H13), C83(H83), C12(H12), C82(H82), C121(H121), C115(H115),
 C101(H101), C14(H14), C111(H111), C114(H114), C25(H25), C21(H21), C125(H125),
 C22(H22), C112(H112), C91(H91), C132(H132), C105(H105), C123(H123), C24(H24),
 C31(H31), C142(H142), C35(H35), C134(H134), C55(H55), C113(H113), C124(H124),
 C102(H102), C122(H122), C103(H103), C23(H23), C95(H95), C45(H45), C93(H93),
 C104(H104), C54(H54), C74(H74), C33(H33), C34(H34), C41(H41), C92(H92),
 C62(H62), C94(H94), C64(H64), C144(H144), C44(H44), C53(H53), C52(H52),
 C42(H42), C32(H32), C72(H72), C43(H43), C51(H51), C153(H153), C155(H155),
 C152(H152), C154(H154)
2.b Idealised Me refined as rotating group:
 C148(H14A,H14B,H14C), C138(H13A,H13B,H13C), C68(H68A,H68B,H68C), C136(H13D,
 H13E,H13F), C137(H13G,H13H,H13I), C76(H76A,H76B,H76C), C66(H66A,H66B,H66C),
 C78(H78A,H78B,H78C), C147(H14D,H14E,H14F), C146(H14G,H14H,H14I), C77(H77A,H77B,
 H77C), C67(H67A,H67B,H67C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 236 electrons were 
found in a volume of 1076\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
1[C6H4F2] per Asymmetric Unit 
which account for 232 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              60200
_shelx_fab_checksum              74619
_olex2_submission_special_instructions 'No special instructions were received'