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_1566766
_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_absolute_configuration ad
_chemical_formula_moiety         'C74 H132 Al2 K2 N4 O10 S2 Si4'
_chemical_formula_sum            'C74 H132 Al2 K2 N4 O10 S2 Si4'
_chemical_formula_weight         1546.48
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      4
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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             2020-07-04T15:45:03-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2020-10-15 deposited with the CCDC.	2022-03-31 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3187(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.27766(9)
_cell_length_b                   24.87997(17)
_cell_length_c                   14.90060(11)
_cell_measurement_reflns_used    41269
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.426
_cell_measurement_theta_min      4.502
_cell_measurement_wavelength     1.54184
_cell_volume                     4538.73(6)
_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      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9861
_diffrn_measured_fraction_theta_max 0.965
_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      0.0453437
_diffrn_orient_matrix_UB_12      -0.0577674
_diffrn_orient_matrix_UB_13      0.0023362
_diffrn_orient_matrix_UB_21      0.0840842
_diffrn_orient_matrix_UB_22      0.0156557
_diffrn_orient_matrix_UB_23      0.0775505
_diffrn_orient_matrix_UB_31      -0.0818995
_diffrn_orient_matrix_UB_32      -0.0159076
_diffrn_orient_matrix_UB_33      0.0687702
_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  0.049
_diffrn_reflns_av_unetI/netI     0.043
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            63075
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        74.0807
_diffrn_reflns_theta_max         73.5958
_diffrn_reflns_theta_min         3.553
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    2.447
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.475
_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    1.132
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1672
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.251
_exptl_crystal_size_min          0.172
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
;
 Flack x determined using 7937 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     944
_refine_ls_number_reflns         17697
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0568P)^2^+1.1872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0955
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                17308
_reflns_number_total             17697
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2sc01064j2.cif
_cod_data_source_block           '[(K(Et2O))(2-S)]2'
_cod_database_code               1566766