Reduction of Organic Azides by Indyl-Anions. Isolation and Reactivity Studies of Indium-Nitrogen Multiple Bonds
Anker, Mathew; Lein, Matthias; Coles, Martyn P.; Chemical Science  (2019) –; doi:10.1039/C8SC04078H

data_1550228
_publ_section_title
;
 Reduction of Organic Azides by Indyl-Anions. Isolation and Reactivity
 Studies of Indium-Nitrogen Multiple Bonds
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC04078H
_journal_year                    2019
_chemical_formula_moiety         'C36 H66 K2 N2 O3 Si2'
_chemical_formula_sum            'C36 H66 K2 N2 O3 Si2'
_chemical_formula_weight         709.28
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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             2015-05-20T17:50:42-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2018-08-23 deposited with the CCDC.
2018-11-12 downloaded from the CCDC.
;
_cell_angle_alpha                93.171(4)
_cell_angle_beta                 96.478(4)
_cell_angle_gamma                92.102(4)
_cell_formula_units_Z            2
_cell_length_a                   10.0422(4)
_cell_length_b                   11.9620(6)
_cell_length_c                   17.7445(10)
_cell_measurement_reflns_used    3927
_cell_measurement_temperature    120.01(10)
_cell_measurement_theta_max      28.517
_cell_measurement_theta_min      3.778
_cell_measurement_wavelength     0.71073
_cell_volume                     2112.72(18)
_computing_cell_refinement
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_computing_data_collection
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_computing_data_reduction
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
;
_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      120.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1712
_diffrn_measured_fraction_theta_full 0.9871
_diffrn_measured_fraction_theta_max 0.8209
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0082073
_diffrn_orient_matrix_UB_12      -0.0583648
_diffrn_orient_matrix_UB_13      -0.0058406
_diffrn_orient_matrix_UB_21      0.0081422
_diffrn_orient_matrix_UB_22      0.007301
_diffrn_orient_matrix_UB_23      -0.038637
_diffrn_orient_matrix_UB_31      0.070207
_diffrn_orient_matrix_UB_32      0.0085821
_diffrn_orient_matrix_UB_33      0.0098651
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0681
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.821
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            15308
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.821
_diffrn_reflns_theta_full        26.3154
_diffrn_reflns_theta_max         29.2917
_diffrn_reflns_theta_min         3.3452
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.312
_exptl_absorpt_correction_T_max  0.991
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro, Agilent Technologies,
        Version 1.171.37.35h (release 09-02-2015 CrysAlis171 .NET)
        (compiled Feb  9 2015,16:26:32)
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_density_diffrn    1.115
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Plate
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.2348
_exptl_crystal_size_mid          0.1728
_exptl_crystal_size_min          0.0389
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     406
_refine_ls_number_reflns         9496
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.1066
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0633P)^2^+1.1161P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1375
_refine_ls_wR_factor_ref         0.1593
_reflns_number_gt                6409
_reflns_number_total             9496
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04078h2.cif
_cod_data_source_block           1-(Et2O)2
_cod_original_cell_volume        2112.73(18)
_cod_database_code               1550228