Beyond simple hetero Diels-Alder Cycloadditions. A New Type of Element-Ligand Cooperativity at N,C,N-coordinated Arsinidene and Stibinidene Centres in the Reaction with an Electron Deficient Alkyne.
Hejda, Martin; Zechovský, Jan; Kremláček, Vít; Erben, Milan; Rychagova, Elena A.; Jambor, Roman; R°užička, Aleš; Ketkov, Sergey Yu.; Dostál, Libor; Dalton Transactions  (2022) –; doi:10.1039/D2DT02499C

data_7711230
_publ_section_title
;
 Beyond simple hetero Diels-Alder Cycloadditions. A New Type of
 Element-Ligand Cooperativity at N,C,N-coordinated Arsinidene and
 Stibinidene Centres in the Reaction with an Electron Deficient Alkyne.
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02499C
_journal_year                    2022
_chemical_formula_moiety         'C38 H45 Bi N2 O4'
_chemical_formula_sum            'C38 H45 Bi N2 O4'
_chemical_formula_weight         802.74
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-07-27 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   22.8568(7)
_cell_length_b                   10.9255(4)
_cell_length_c                   28.4085(8)
_cell_measurement_reflns_used    65003
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     7094.2(4)
_computing_cell_refinement       'APEX3 v2018.1-0 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.38A (Bruker AXS Inc., 2016)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker D8 - Venture'
_diffrn_measurement_method       '\f and \w scans to fill the Ewald sphere'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1668
_diffrn_reflns_av_unetI/netI     0.1513
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            65003
_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         27.524
_diffrn_reflns_theta_min         2.287
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    5.011
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6121
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 - Bruker AXS area detector
scaling and absorption correction
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.503
_exptl_crystal_description       needle
_exptl_crystal_F_000             3216
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.114
_exptl_crystal_size_min          0.070
_refine_diff_density_max         1.646
_refine_diff_density_min         -1.857
_refine_diff_density_rms         0.197
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.450(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     827
_refine_ls_number_reflns         16139
_refine_ls_number_restraints     809
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.1213
_refine_ls_R_factor_gt           0.0632
_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^)+(0.0244P)^2^+4.5740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0928
_reflns_Friedel_coverage         0.961
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                10821
_reflns_number_total             16139
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02499c1.cif
_cod_data_source_block           ld210222Bi1
_cod_database_code               7711230
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.821
;
_shelx_res_checksum              7190
_shelx_hkl_checksum              87340