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_7711235
_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 H51 N2 O8 Sb'
_chemical_formula_sum            'C44 H51 N2 O8 Sb'
_chemical_formula_weight         857.61
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2022-09-12 deposited with the CCDC.	2022-09-13 downloaded from the CCDC.
;
_cell_angle_alpha                89.581(8)
_cell_angle_beta                 71.665(9)
_cell_angle_gamma                66.480(9)
_cell_formula_units_Z            2
_cell_length_a                   11.361(3)
_cell_length_b                   14.190(3)
_cell_length_c                   15.078(3)
_cell_measurement_reflns_used    8784
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.2449
_cell_measurement_theta_min      2.2750
_cell_volume                     2096.1(8)
_computing_cell_refinement       'APEX4 v2022.1-1 (Bruker AXS)'
_computing_data_collection       'Bruker Instrument Service vV6.2.3'
_computing_data_reduction        'SAINT V8.40B (Bruker AXS Inc., 2019)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.986
_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  0.0413
_diffrn_reflns_av_unetI/netI     0.0356
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            41762
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.986
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.362
_diffrn_reflns_theta_min         2.173
_diffrn_source                   'sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.712
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6136
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Krause, L., Herbst-Irmer, R., Sheldrick, G. M., Stalke, D. (2015).
"Comparison of silver and molybdenum microfocus X-ray sources for
single-crystal structure determination"
J. Appl. Cryst. 48, 3-10.
doi:10.1107/S1600576714022985
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       block
_exptl_crystal_F_000             888
_exptl_crystal_size_max          0.826
_exptl_crystal_size_mid          0.543
_exptl_crystal_size_min          0.347
_refine_diff_density_max         0.611
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     508
_refine_ls_number_reflns         10322
_refine_ls_number_restraints     429
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.0369
_refine_ls_R_factor_gt           0.0282
_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^)+(0.0323P)^2^+1.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0644
_refine_ls_wR_factor_ref         0.0684
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9170
_reflns_number_total             10322
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02499c1.cif
_cod_data_source_block           ld210407Sb1
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Multi-Scan' was
changed to 'multi-scan' in accordance with the
/home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_database_code               7711235
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.591
_shelx_estimated_absorpt_t_max   0.790
_exptl_absorpt_special_details
;
The ratio of minimum to maximum
apparent transmission was 0.823
;
_shelx_res_checksum              29931
_shelx_hkl_checksum              12718