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_1575124
_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 Cl2 N2 P2 Sb, C3 H6 O'
_chemical_formula_sum            'C51 H51 Cl2 N2 O P2 Sb'
_chemical_formula_weight         962.53
_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     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                90
_cell_angle_beta                 90.795(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.682(4)
_cell_length_b                   18.781(9)
_cell_length_c                   22.801(10)
_cell_measurement_reflns_used    9935
_cell_measurement_temperature    107.00
_cell_measurement_theta_max      35.58
_cell_measurement_theta_min      2.36
_cell_volume                     4574(3)
_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      107.00
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0652
_diffrn_reflns_av_unetI/netI     0.0474
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            131308
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         35.717
_diffrn_reflns_theta_min         2.595
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.830
_exptl_absorpt_correction_T_max  0.7470
_exptl_absorpt_correction_T_min  0.6574
_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            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             1976
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.640
_refine_diff_density_min         -1.011
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     540
_refine_ls_number_reflns         21115
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0548
_refine_ls_R_factor_gt           0.0410
_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^)+(0.0203P)^2^+4.4804P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0770
_refine_ls_wR_factor_ref         0.0817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17645
_reflns_number_total             21115
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           siumbelia230522_0m
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_original_cell_volume        4574(4)
_cod_database_code               1575124
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.907
_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:
 C64(H64), C13(H13), C14(H14), C42(H42), C45(H45), C51(H51), C41(H41),
 C32(H32), C74(H74), C25(H25), C31(H31), C35(H35), C62(H62), C33(H33), C12(H12),
  C44(H44), C34(H34), C43(H43), C24(H24), C52(H52), C72(H72), C54(H54),
 C55(H55), C23(H23), C53(H53), C22(H22), C21(H21)
2.b Idealised Me refined as rotating group:
 C66(H66A,H66B,H66C), C78(H78A,H78B,H78C), C68(H68A,H68B,H68C), C77(H77A,H77B,
 H77C), C76(H76A,H76B,H76C), C67(H67A,H67B,H67C), C2(H2A,H2B,H2C), C3(H3A,H3B,
 H3C)
;
_shelx_res_checksum              12468
_olex2_submission_special_instructions 'No special instructions were received'