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_1575125
_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 Se, C4 H8 O'
_chemical_formula_sum            'C52 H53 N2 O P2 Sb Se'
_chemical_formula_weight         984.61
_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             2024-10-21
_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                 101.2820(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.0961(3)
_cell_length_b                   18.1134(4)
_cell_length_c                   22.9780(6)
_cell_measurement_reflns_used    3771
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.23
_cell_volume                     4529.1(2)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0483
_diffrn_reflns_av_unetI/netI     0.0227
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            127829
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.519
_diffrn_reflns_theta_min         2.232
_exptl_absorpt_coefficient_mu    1.524
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.5352
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1391 before and 0.0546 after correction.
The Ratio of minimum to maximum transmission is 0.7177.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.444
_exptl_crystal_description       block
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.386
_refine_diff_density_min         -0.411
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         11479
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0231
_refine_ls_R_factor_gt           0.0208
_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^)+(0.0208P)^2^+3.1094P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0506
_refine_ls_wR_factor_ref         0.0517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10739
_reflns_number_total             11479
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           meyerf241021
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_database_code               1575125
_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.a Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C4(H4A,H4B), C1(H1A,H1B), C2(H2A,H2B)
2.b Aromatic/amide H refined with riding coordinates:
 C55(H55), C61(H61), C25(H25), C72(H72), C21(H21), C24(H24), C82(H82),
 C51(H51), C62(H62), C13(H13), C65(H65), C31(H31), C23(H23), C22(H22), C54(H54),
  C35(H35), C12(H12), C63(H63), C74(H74), C14(H14), C64(H64), C84(H84),
 C53(H53), C52(H52), C32(H32), C33(H33), C34(H34)
2.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C86(H86A,H86B,H86C), C88(H88A,H88B,H88C), C78(H78A,H78B,
 H78C), C77(H77A,H77B,H77C), C87(H87A,H87B,H87C)
;
_shelx_res_checksum              9264
_olex2_submission_special_instructions 'No special instructions were received'