Germanium(iii) corrole complex: reactivity and mechanistic studies of visible-light promoted N‒H bond activations
Fang, Huayi; Ling, Zhen; Lang, Ke; Brothers, Penelope J.; de Bruin, Bas; Fu, Xuefeng; Chemical Science 5 (2014) 916–; doi:10.1039/c3sc52326h

data_1513655
_publ_section_title
;
 Germanium(iii) corrole complex: reactivity and mechanistic studies of
 visible-light promoted N--H bond activations
;
_journal_issue                   3
_journal_name_full               'Chemical Science'
_journal_page_first              916
_journal_paper_doi               10.1039/c3sc52326h
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         '2(C37 H9 F15 Ge N4 O), C6 H14'
_chemical_formula_sum            'C80 H32 F30 Ge2 N8 O2'
_chemical_formula_weight         1852.32
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                102.173(4)
_cell_angle_beta                 103.316(5)
_cell_angle_gamma                99.283(3)
_cell_formula_units_Z            2
_cell_length_a                   13.016(4)
_cell_length_b                   15.843(5)
_cell_length_c                   18.314(6)
_cell_measurement_reflns_used    11898
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.4615
_cell_measurement_theta_min      1.1827
_cell_volume                     3503.9(19)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics
;
 Mercury: visualization and analysis of crystal structures, C. F. Macrae,
 P. R. Edgington, P. McCabe, E. Pidcock, G. P. Shields, R. Taylor,
 M. Towler and J. van de Streek, J. Appl. Cryst., 39, 453-457, 2006.
;
_computing_publication_material  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELX-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELX-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Saturn724+ CCD'
_diffrn_measurement_method       '\w scans at fixed \c = 45\%'
_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  0.0690
_diffrn_reflns_av_sigmaI/netI    0.0677
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            38156
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.01
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6114
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'CrystalClear (Rigaku Inc., 2008)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1836
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.804
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.181
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1101
_refine_ls_number_reflns         12355
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0926
_refine_ls_R_factor_gt           0.0789
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0456P)^2^+6.8585P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1620
_refine_ls_wR_factor_ref         0.1701
_reflns_number_gt                10569
_reflns_number_total             12355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3sc52326h.txt
_cod_data_source_block           (TPFC)Ge-OH
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1513655