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_1575130
_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         'C52 H53 Cl Mg N2 O P2, C4 H10 O'
_chemical_formula_sum            'C56 H63 Cl Mg N2 O2 P2'
_chemical_formula_weight         917.78
_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             2024-09-10
_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                88.6980(10)
_cell_angle_beta                 81.1000(10)
_cell_angle_gamma                64.7300(10)
_cell_formula_units_Z            4
_cell_length_a                   12.1739(4)
_cell_length_b                   12.6388(5)
_cell_length_c                   36.2781(12)
_cell_measurement_reflns_used    9880
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      29.25
_cell_measurement_theta_min      2.37
_cell_volume                     4981.1(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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_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  0.0772
_diffrn_reflns_av_unetI/netI     0.0502
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            119272
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.005
_diffrn_reflns_theta_max         25.005
_diffrn_reflns_theta_min         1.874
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.197
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6911
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1329 before and 0.0722 after correction.
The Ratio of minimum to maximum transmission is 0.9258.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.224
_exptl_crystal_description       plate
_exptl_crystal_F_000             1952
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.900
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1187
_refine_ls_number_reflns         17524
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.058
_refine_ls_R_factor_all          0.0621
_refine_ls_R_factor_gt           0.0471
_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^)+(0.0598P)^2^+2.9926P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1215
_refine_ls_wR_factor_ref         0.1295
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14067
_reflns_number_total             17524
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5sc03320a3.cif
_cod_data_source_block           siumbelia230505_1_0m
_cod_depositor_comments
'Adding full bibliography for 1575122--1575132.cif.'
_cod_database_code               1575130
_shelx_shelxl_version_number     2016/4
_shelx_estimated_absorpt_t_max   0.983
_shelx_estimated_absorpt_t_min   0.935
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Fixed Sof: H7BC(0.6) H7BD(0.6) H7AA(0.4) H7AB(0.4) H6BC(0.6) H6BD(0.6)
 H6AA(0.4) H6AB(0.4) C8A(0.6) H8AA(0.6) H8AB(0.6) C5A(0.6) H5AA(0.6) H5AB(0.6)
 C5B(0.4) H5BA(0.4) H5BB(0.4) C8B(0.4) H8BA(0.4) H8BB(0.4)
3.a Secondary CH2 refined with riding coordinates:
 C154(H15A,H15B), C156(H15F,H15G), C4(H4A,H4B), C150(H15K,H15L), C1(H1A,H1B),
 C152(H15M,H15N), C3(H3A,H3B), C2(H2A,H2B), C7(H7BC,H7BD), C7(H7AA,H7AB),
 C6(H6BC,H6BD), C6(H6AA,H6AB), C8A(H8AA,H8AB), C5A(H5AA,H5AB), C5B(H5BA,H5BB),
 C8B(H8BA,H8BB)
3.b Aromatic/amide H refined with riding coordinates:
 C51(H51), C125(H125), C111(H111), C123(H123), C105(H105), C52(H52),
 C113(H113), C82(H82), C91(H91), C14(H14), C104(H104), C72(H72), C112(H112),
 C41(H41), C121(H121), C42(H42), C44(H44), C124(H124), C45(H45), C122(H122),
 C12(H12), C55(H55), C115(H115), C101(H101), C31(H31), C32(H32), C43(H43),
 C103(H103), C25(H25), C21(H21), C102(H102), C13(H13), C92(H92), C114(H114),
 C64(H64), C84(H84), C53(H53), C83(H83), C22(H22), C33(H33), C95(H95), C34(H34),
  C24(H24), C74(H74), C35(H35), C142(H142), C23(H23), C93(H93), C54(H54),
 C94(H94), C144(H144), C132(H132), C62(H62), C134(H134)
3.c Idealised Me refined as rotating group:
 C76(H76A,H76B,H76C), C68(H68A,H68B,H68C), C136(H13A,H13B,H13C), C138(H13D,
 H13E,H13F), C155(H15C,H15D,H15E), C78(H78A,H78B,H78C), C66(H66A,H66B,H66C),
 C147(H14A,H14B,H14C), C67(H67A,H67B,H67C), C137(H13G,H13H,H13I), C77(H77A,H77B,
 H77C), C157(H15H,H15I,H15J), C148(H14D,H14E,H14F), C153(H15O,H15P,H15Q),
 C146(H14G,H14H,H14I), C151(H15R,H15S,H15T)
;
_shelx_res_checksum              91367
_olex2_submission_special_instructions 'No special instructions were received'