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_1550235
_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         'C106 H152 In2 K2 N12 O2 Si4, 2(C7 H8)'
_chemical_formula_sum            'C120 H168 In2 K2 N12 O2 Si4'
_chemical_formula_weight         2230.86
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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             2018-05-23T16:45:16-00:00
_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                90
_cell_angle_beta                 102.941(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.1290(8)
_cell_length_b                   12.5964(3)
_cell_length_c                   30.8350(12)
_cell_measurement_reflns_used    4581
_cell_measurement_temperature    119.97(11)
_cell_measurement_theta_max      26.739
_cell_measurement_theta_min      3.508
_cell_measurement_wavelength     0.71073
_cell_volume                     11783.7(6)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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 16.1712
_diffrn_measured_fraction_theta_full 0.9967
_diffrn_measured_fraction_theta_max 0.9967
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0104974
_diffrn_orient_matrix_UB_12      -0.0243176
_diffrn_orient_matrix_UB_13      -0.020395
_diffrn_orient_matrix_UB_21      0.0043392
_diffrn_orient_matrix_UB_22      0.0457435
_diffrn_orient_matrix_UB_23      -0.0117169
_diffrn_orient_matrix_UB_31      0.0204326
_diffrn_orient_matrix_UB_32      -0.0221721
_diffrn_orient_matrix_UB_33      -0.0018969
_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  0.0503
_diffrn_reflns_av_unetI/netI     0.0852
_diffrn_reflns_Laue_measured_fraction_full 0.972
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            25851
_diffrn_reflns_point_group_measured_fraction_full 0.972
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.2956
_diffrn_reflns_theta_max         25.3494
_diffrn_reflns_theta_min         3.2844
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    0.556
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.897
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             4720
_exptl_crystal_size_max          0.154
_exptl_crystal_size_mid          0.084
_exptl_crystal_size_min          0.059
_refine_diff_density_max         1.137
_refine_diff_density_min         -1.236
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.174
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     625
_refine_ls_number_reflns         10356
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.174
_refine_ls_R_factor_all          0.0984
_refine_ls_R_factor_gt           0.0705
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0168P)^2^+80.2464P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1263
_reflns_number_gt                7995
_reflns_number_total             10356
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04078h2.cif
_cod_data_source_block           7a-tol
_cod_database_code               1550235