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_1550233
_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         'C58 H92 In K N6 O7 Si2, 2(C7 H8)'
_chemical_formula_sum            'C72 H108 In K N6 O7 Si2'
_chemical_formula_weight         1379.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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             2018-06-06T11:21:22-00:00
_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                 103.5966(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.16789(17)
_cell_length_b                   26.8940(3)
_cell_length_c                   19.8817(2)
_cell_measurement_reflns_used    37428
_cell_measurement_temperature    120.02(10)
_cell_measurement_theta_max      73.468
_cell_measurement_theta_min      3.992
_cell_measurement_wavelength     1.54184
_cell_volume                     7363.24(15)
_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      120.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9994
_diffrn_measured_fraction_theta_max 0.9995
_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      -0.1006383
_diffrn_orient_matrix_UB_12      -0.0249686
_diffrn_orient_matrix_UB_13      -0.0149854
_diffrn_orient_matrix_UB_21      0.0153106
_diffrn_orient_matrix_UB_22      -0.0131674
_diffrn_orient_matrix_UB_23      0.0772448
_diffrn_orient_matrix_UB_31      -0.0463309
_diffrn_orient_matrix_UB_32      0.0498385
_diffrn_orient_matrix_UB_33      0.0129183
_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  0.0299
_diffrn_reflns_av_unetI/netI     0.0418
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 1
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            63102
_diffrn_reflns_point_group_measured_fraction_full 1
_diffrn_reflns_point_group_measured_fraction_max 1
_diffrn_reflns_theta_full        68.1328
_diffrn_reflns_theta_max         68.2474
_diffrn_reflns_theta_min         3.6059
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    3.806
_exptl_absorpt_correction_T_max  0.815
_exptl_absorpt_correction_T_min  0.591
_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            'pale yellow'
_exptl_crystal_density_diffrn    1.245
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2936.0
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.151
_exptl_crystal_size_min          0.103
_refine_diff_density_max         0.967
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.126
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     805
_refine_ls_number_reflns         13462
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_R_factor_all          0.0371
_refine_ls_R_factor_gt           0.0355
_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^)+(0.0233P)^2^+13.3225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0857
_refine_ls_wR_factor_ref         0.0866
_reflns_number_gt                12853
_reflns_number_total             13462
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc04078h2.cif
_cod_data_source_block           7a-18-c-6
_cod_original_cell_volume        7363.25(14)
_cod_database_code               1550233