Carbon–chalcogen bond formation initiated by [Al(NONDipp)(E)]− anions containing Al–E{16} (E{16} = S, Se) multiple bonds
Evans, Matthew J.; Anker, Mathew D.; McMullin, Claire L.; Neale, Samuel E.; Rajabi, Nasir A.; Coles, Martyn P.; Chemical Science  (2022) –; doi:10.1039/D2SC01064J

data_1566767
_publ_section_title
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 Carbon--chalcogen bond formation initiated by [Al(NONDipp)(E)]&#x2212;
 anions containing Al--E{16} (E{16} = S, Se) multiple bonds
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D2SC01064J
_journal_year                    2022
_chemical_formula_moiety         'C49  H66  N2  O3  Al1  Si2  K1  Se1'
_chemical_formula_sum            'C49 H66 Al K N2 O3 Se Si2'
_chemical_formula_weight         932.25
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4.3
_audit_creation_date             2020-06-08T14:10:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.7250(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.84213(8)
_cell_length_b                   13.02613(7)
_cell_length_c                   26.00620(15)
_cell_measurement_reflns_used    38632
_cell_measurement_temperature    119.97(11)
_cell_measurement_theta_max      73.392
_cell_measurement_theta_min      4.857
_cell_measurement_wavelength     1.54184
_cell_volume                     4884.35(5)
_computing_cell_refinement       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)'
_computing_molecular_graphics    'Ortep for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_diffrn_ambient_temperature      119.97(11)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9819
_diffrn_measured_fraction_theta_max 0.9962
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.014263
_diffrn_orient_matrix_UB_12      -0.0872717
_diffrn_orient_matrix_UB_13      -0.041165
_diffrn_orient_matrix_UB_21      -0.0415667
_diffrn_orient_matrix_UB_22      -0.0681492
_diffrn_orient_matrix_UB_23      0.0369523
_diffrn_orient_matrix_UB_31      -0.0973974
_diffrn_orient_matrix_UB_32      0.0416976
_diffrn_orient_matrix_UB_33      -0.0255728
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0304
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62964
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        74.3338
_diffrn_reflns_theta_max         73.5902
_diffrn_reflns_theta_min         3.3929
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.765
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.293
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
                        a multifaceted crystal model
        Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rhombohedral
_exptl_crystal_F_000             1968
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.307
_exptl_crystal_size_min          0.106
_refine_diff_density_max         2.141
_refine_diff_density_min         -0.786
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     514
_refine_ls_number_reflns         9821
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0452
_refine_ls_R_factor_gt           0.0438
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0564P)^2^+10.0806P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1139
_reflns_number_gt                9387
_reflns_number_total             9821
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01064j2.cif
_cod_data_source_block           K[4-Se]
_cod_original_cell_volume        4884.35(4)
_cod_database_code               1566767