Amination Reaction on Copper and Germanium β-Nitrocorrolates
Manuela Stefanelli; Federica Mandoj; Marco Mastroianni; Sara Nardis; Pruthviray Mohite; Frank R. Fronczek; Kevin M. Smith; Karl M. Kadish; Xiao Xiao; Zhongping Ou; Ping Chen; Roberto Paolesse; Inorganic Chemistry 50 (2011) 8281–8292; doi:10.1021/ic2008073

data_4326041
_publ_section_title
;
 Amination Reaction on Copper and Germanium \b-Nitrocorrolates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8281
_journal_page_last               8292
_journal_paper_doi               10.1021/ic2008073
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C38 H26 Ge N6 O3'
_chemical_formula_sum            'C38 H26 Ge N6 O3'
_chemical_formula_weight         687.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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
_cell_angle_beta                 92.646(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.6310(5)
_cell_length_b                   18.9383(10)
_cell_length_c                   15.0218(9)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    90.0(5)
_cell_measurement_theta_max      68.5
_cell_measurement_theta_min      3.7
_cell_volume                     3021.2(3)
_computing_cell_refinement       'Bruker Apex-II '
_computing_data_collection       'Bruker Apex-II'
_computing_data_reduction        'Bruker Apex-II '
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90.0(5)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_device_type  'Bruker Kappa Apex-II CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_sigmaI/netI    0.0266
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            23268
_diffrn_reflns_theta_full        66.6
_diffrn_reflns_theta_max         68.9
_diffrn_reflns_theta_min         3.7
_exptl_absorpt_coefficient_mu    1.797
_exptl_absorpt_correction_T_max  0.884
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.40
_refine_diff_density_min         -0.42
_refine_diff_density_rms         0.058
_refine_ls_extinction_coef       0.00014(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.086
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     445
_refine_ls_number_reflns         5398
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.086
_refine_ls_R_factor_all          0.034
_refine_ls_R_factor_gt           0.031
_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^)+(0.0412P)^2^+1.9302P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.081
_refine_ls_wR_factor_ref         0.083
_reflns_number_gt                4951
_reflns_number_total             5398
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic2008073_si_002.cif
_cod_data_source_block           2-NH2-3-NO2-TPCorrGe(OCH3)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               4326041