Reactions of In‒Zn Bonds with Organic Azides: Products that Result from Hetero- and Homo-bimetallic Behaviour
Anker, Mathew David; Altaf, Yasir; Lein, Matthias; Coles, Martyn P.; Dalton Transactions  (2019) –; doi:10.1039/C9DT03990B

data_7701395
_publ_section_title
;
 Reactions of In--Zn Bonds with Organic Azides: Products that Result from
 Hetero- and Homo-bimetallic Behaviour
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C9DT03990B
_journal_year                    2019
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C63 H85 In N8 O Si2 Zn'
_chemical_formula_sum            'C63 H85 In N8 O Si2 Zn'
_chemical_formula_weight         1206.75
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      9
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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             2019-10-17T13:11:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_audit_update_record
;
2019-10-17 deposited with the CCDC.    2019-10-21 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.2676(11)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.7935(2)
_cell_length_b                   15.08451(15)
_cell_length_c                   20.4019(2)
_cell_measurement_reflns_used    15820
_cell_measurement_temperature    119.97(10)
_cell_measurement_theta_max      72.031
_cell_measurement_theta_min      4.4
_cell_measurement_wavelength     1.54184
_cell_volume                     6296.78(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0856
_diffrn_measured_fraction_theta_full 0.9995
_diffrn_measured_fraction_theta_max 0.8378
_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      -0.0266912
_diffrn_orient_matrix_UB_12      0.0511648
_diffrn_orient_matrix_UB_13      -0.0644305
_diffrn_orient_matrix_UB_21      0.0700364
_diffrn_orient_matrix_UB_22      0.0280462
_diffrn_orient_matrix_UB_23      -0.00566
_diffrn_orient_matrix_UB_31      0.0071219
_diffrn_orient_matrix_UB_32      -0.0838071
_diffrn_orient_matrix_UB_33      -0.0413234
_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  0.0536
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 1
_diffrn_reflns_Laue_measured_fraction_max 0.986
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20779
_diffrn_reflns_point_group_measured_fraction_full 0.868
_diffrn_reflns_point_group_measured_fraction_max 0.846
_diffrn_reflns_theta_full        66.9682
_diffrn_reflns_theta_max         72.2126
_diffrn_reflns_theta_min         3.6404
_diffrn_source                   'micro-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.103
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.344
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
        CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_density_diffrn    1.273
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2536.0
_exptl_crystal_size_max          0.298
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.125
_refine_diff_density_max         0.437
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.044
_refine_ls_abs_structure_details
;
 Flack x determined using 4198 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.016(3)
_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     705
_refine_ls_number_reflns         10513
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0259
_refine_ls_R_factor_gt           0.0254
_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^)+(0.0367P)^2^+2.3117P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0637
_refine_ls_wR_factor_ref         0.0641
_reflns_number_gt                10368
_reflns_number_total             10513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt03990b2.cif
_cod_data_source_block           Compound-6
_cod_original_cell_volume        6296.75(12)
_cod_database_code               7701395