Site-Selective Nitrenoid Insertions Utilizing Postfunctionalized Bifunctional Rhodium(II) Catalysts
Berndt, Jan Philipp; Radchenko, Yevhenii; Becker, Jonathan; Logemann, Christian; Bhandari, Dhaka Ram; Hrdina, Radim; SCHREINER, Peter Richard; Chemical Science  (2019) –; doi:10.1039/C8SC05733H

data_1550574
_publ_section_title
;
 Site-Selective Nitrenoid Insertions Utilizing Postfunctionalized
 Bifunctional Rhodium(II) Catalysts
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C8SC05733H
_journal_year                    2019
_chemical_formula_moiety
'C84 H88 F24 N8 O14 Rh2 S2, 2(C2 H6 O S) [+ solvent]'
_chemical_formula_sum            'C88 H100 F24 N8 O16 Rh2 S4'
_chemical_formula_weight         2315.81
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2018-06-28 deposited with the CCDC.
2019-02-06 downloaded from the CCDC.
;
_cell_angle_alpha                89.158(2)
_cell_angle_beta                 89.755(2)
_cell_angle_gamma                62.152(2)
_cell_formula_units_Z            1
_cell_length_a                   14.0242(9)
_cell_length_b                   14.3859(9)
_cell_length_c                   17.8002(11)
_cell_measurement_reflns_used    9889
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.54
_cell_measurement_theta_min      2.77
_cell_volume                     3174.9(4)
_computing_cell_refinement       'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_data_collection       'APEX2 v2011.4.0 (Bruker-AXS, 2015)'
_computing_data_reduction        'SAINT 7.46A (Bruker-AXS, 2015)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXT-2015 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
'BRUKER D8 Venture, Bruker Photon 100 CMOS detector'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0583
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            1105708
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         32.577
_diffrn_reflns_theta_min         2.289
_diffrn_source                   'ImuS microfocus source'
_exptl_absorpt_coefficient_mu    0.412
_exptl_absorpt_correction_T_max  0.7467
_exptl_absorpt_correction_T_min  0.6673
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.211
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1182
_exptl_crystal_size_max          0.745
_exptl_crystal_size_mid          0.410
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.950
_refine_diff_density_min         -0.641
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     790
_refine_ls_number_reflns         23108
_refine_ls_number_restraints     1848
_refine_ls_restrained_S_all      1.217
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0342
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+2.4934P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0799
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                20294
_reflns_number_total             23108
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8sc05733h2.cif
_cod_data_source_block           D17074_sq
_cod_original_cell_volume        3174.9(3)
_cod_database_code               1550574
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.749
_shelx_estimated_absorpt_t_max   0.913
_shelx_res_checksum              26669
_shelx_fab_checksum              32181