Oxidative Addition Versus Substitution Reactions of Group 14 Dialkylamino Metalylenes with Pentafluoropyridine
Prinson P. Samuel; Amit Pratap Singh; Sankaranarayana Pillai Sarish; Julia Matussek; Ina Objartel; Herbert W. Roesky; Dietmar Stalke; Inorganic Chemistry 52 (2013) 1544–1549; doi:10.1021/ic302344a

data_4333728
_publ_section_title
;
 Oxidative Addition Versus Substitution Reactions of Group 14 Dialkylamino
 Metalylenes with Pentafluoropyridine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1544
_journal_page_last               1549
_journal_paper_doi               10.1021/ic302344a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C26 H37 F5 Ge N4'
_chemical_formula_weight         573.19
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 112.05(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.122(2)
_cell_length_b                   19.248(2)
_cell_length_c                   19.887(3)
_cell_measurement_reflns_used    9955
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.5025
_cell_measurement_theta_min      2.21
_cell_volume                     5365.1(14)
_computing_cell_refinement       'SAINT V7.68A'
_computing_data_collection       'APEX2 v2011.2'
_computing_data_reduction        'SAINT V7.68A'
_computing_molecular_graphics    'shelXle v0.477'
_computing_structure_refinement  'SHELXL-2012(Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      101(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker Smart Apex II Quazar'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0364
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            98347
_diffrn_reflns_theta_full        27.52
_diffrn_reflns_theta_max         27.52
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    1.198
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2012/1
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_description       block
_exptl_crystal_F_000             2384
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.377
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         12310
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0246
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0244P)^2^+2.7100P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0577
_refine_ls_wR_factor_ref         0.0595
_reflns_number_gt                10909
_reflns_number_total             12312
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302344a_si_002_2.cif
_cod_data_source_block           8
_cod_original_cell_volume        5365.1(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4333728