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_7711231
_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         'C44 H50 As N2 O8'
_chemical_formula_sum            'C44 H50 As N2 O8'
_chemical_formula_weight         809.78
_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
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                72.640(8)
_cell_angle_beta                 70.438(9)
_cell_angle_gamma                68.085(9)
_cell_formula_units_Z            2
_cell_length_a                   11.405(2)
_cell_length_b                   14.254(3)
_cell_length_c                   14.960(3)
_cell_measurement_reflns_used    31555
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1
_cell_volume                     2083.8(7)
_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 0.969
_diffrn_measured_fraction_theta_max 0.965
_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  0.0902
_diffrn_reflns_av_unetI/netI     0.0819
_diffrn_reflns_Laue_measured_fraction_full 0.969
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            31555
_diffrn_reflns_point_group_measured_fraction_full 0.969
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.497
_diffrn_reflns_theta_min         2.358
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.869
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4304
_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    1.291
_exptl_crystal_description       plate
_exptl_crystal_F_000             850
_exptl_crystal_size_max          0.594
_exptl_crystal_size_mid          0.259
_exptl_crystal_size_min          0.056
_refine_diff_density_max         0.820
_refine_diff_density_min         -1.333
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     517
_refine_ls_number_reflns         7492
_refine_ls_number_restraints     458
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0874
_refine_ls_R_factor_gt           0.0617
_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^)+(0.1052P)^2^+1.2705P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1599
_refine_ls_wR_factor_ref         0.1712
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6079
_reflns_number_total             7492
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02499c1.cif
_cod_data_source_block           ld210504As1_5As
_cod_database_code               7711231
_shelx_shelxl_version_number     2017/1
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.577
;
_shelx_res_checksum              36463
_shelx_hkl_checksum              41710