Mechanistic studies of the rhodium-catalyzed direct C-h amination reaction using azides as the nitrogen source.
Park, Sae Hume; Kwak, Jaesung; Shin, Kwangmin; Ryu, Jaeyune; Park, Yoonsu; Chang, Sukbok; Journal of the American Chemical Society 136 (2014) 2492–2502; doi:10.1021/ja411072a

data_4120550
_publ_section_title
;
 Mechanistic studies of the rhodium-catalyzed direct C-h amination
 reaction using azides as the nitrogen source.
;
_journal_issue                   6
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2492
_journal_page_last               2502
_journal_paper_doi               10.1021/ja411072a
_journal_volume                  136
_journal_year                    2014
_chemical_formula_moiety         C30H36Cl2F6N2O4Rh1S1Sb1
_chemical_formula_sum            'C30 H36 Cl2 F6 N2 O4 Rh S Sb'
_chemical_formula_weight         930.23
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.307(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   24.728(4)
_cell_length_b                   10.6883(16)
_cell_length_c                   28.583(4)
_cell_measurement_reflns_used    9978
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      29.88
_cell_measurement_theta_min      1.54
_cell_volume                     6989.1(18)
_computing_cell_refinement       'Bruker APEX II'
_computing_data_collection       'Bruker APEX II'
_computing_data_reduction        'Bruker APEX II'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_sigmaI/netI    0.0310
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            56264
_diffrn_reflns_theta_full        29.88
_diffrn_reflns_theta_max         29.88
_diffrn_reflns_theta_min         1.54
_exptl_absorpt_coefficient_mu    1.527
_exptl_absorpt_correction_T_max  0.941
_exptl_absorpt_correction_T_min  0.930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.768
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Rod
_exptl_crystal_F_000             3696
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.511
_refine_diff_density_min         -1.072
_refine_diff_density_rms         0.146
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     439
_refine_ls_number_reflns         9978
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0870
_refine_ls_R_factor_gt           0.0604
_refine_ls_shift/su_max          0.130
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1182P)^2^+30.6327P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1804
_refine_ls_wR_factor_ref         0.2073
_reflns_number_gt                7109
_reflns_number_total             9978
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja411072a_si_003.cif
_cod_data_source_block           sbc002-1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/usr/data/users/saulius/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 
;
_cod_original_cell_volume        6989.0(18)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4120550