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_1575127
_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 N2 P2 Sb, C4 H8 Al Cl3 O, 0.75(C4 H8 O)'
_chemical_formula_sum            'C55 H59 Al Cl3 N2 O1.75 P2 Sb'
_chemical_formula_weight         1093.06
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-10-25
_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                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.7633(6)
_cell_length_b                   16.3853(4)
_cell_length_c                   26.2160(4)
_cell_measurement_reflns_used    9863
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      31.01
_cell_measurement_theta_min      2.20
_cell_volume                     10637.2(4)
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_measured_fraction_theta_full 0.999
_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  0.0679
_diffrn_reflns_av_unetI/netI     0.0543
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            66916
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.504
_diffrn_reflns_theta_min         2.062
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.787
_exptl_absorpt_correction_T_max  0.7471
_exptl_absorpt_correction_T_min  0.6362
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.0603 before and 0.0440 after correction.
The Ratio of minimum to maximum transmission is 0.8516.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             4496
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.216
_refine_diff_density_min         -0.887
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     620
_refine_ls_number_reflns         12226
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0573
_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^)+(0.0545P)^2^+18.4957P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1301
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9395
_reflns_number_total             12226
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           siumbelia230614_0ma
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_database_code               1575127
_shelx_shelxl_version_number     2016/4
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 Sb1-N1 \\sim Sb2-N1
 with sigma of 0.02
 Sb1-N2 \\sim Sb2-N2
 with sigma of 0.02
 Sb1-C10 \\sim Sb2-C10
 with sigma of 0.02
3. Others
 Sof(Sb2)=1-FVAR(1)
 Sof(Sb1)=FVAR(1)
 Fixed Sof: O2(0.75) C8(0.75) H8A(0.75) H8B(0.75) C7(0.75) H7A(0.75) H7B(0.75)
 C6(0.75) H6A(0.75) H6B(0.75) C5(0.75) H5A(0.75) H5B(0.75)
4.a Secondary CH2 refined with riding coordinates:
 C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B), C8(H8A,H8B), C3(H3A,H3B), C7(H7A,H7B),
 C6(H6A,H6B), C5(H5A,H5B)
4.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C12(H12), C13(H13), C31(H31), C64(H64), C51(H51), C21(H21),
 C25(H25), C55(H55), C52(H52), C35(H35), C62(H62), C22(H22), C54(H54), C74(H74),
  C24(H24), C53(H53), C32(H32), C33(H33), C41(H41), C23(H23), C72(H72),
 C44(H44), C34(H34), C45(H45), C43(H43), C42(H42)
4.c Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C68(H68A,H68B,H68C), C76(H76A,H76B,H76C), C67(H67A,H67B,
 H67C), C78(H78A,H78B,H78C), C77(H77A,H77B,H77C)
;
_shelx_res_checksum              92374
_olex2_submission_special_instructions 'No special instructions were received'