Reversible Oxidation State Change in Germanium(tetraphenylporphyrin) Induced by a Dative Ligand: Aromatic GeII(TPP) and Antiaromatic GeIV(TPP)(pyridine)2
Julie A. Cissell; Thomas P. Vaid; Glenn P. A. Yap; Journal of the American Chemical Society 129 (2007) 7841–7847; doi:10.1021/ja070794i

data_4109554
_publ_section_title
;
 Reversible Oxidation State Change in Germanium(tetraphenylporphyrin)
 Induced by a Dative Ligand: Aromatic GeII(TPP) and Antiaromatic
 GeIV(TPP)(pyridine)2
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7841
_journal_page_last               7847
_journal_paper_doi               10.1021/ja070794i
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C67 H35 F24 Ge N7'
_chemical_formula_weight         1466.61
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_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                 99.981(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.003(3)
_cell_length_b                   17.824(4)
_cell_length_c                   20.177(3)
_cell_measurement_reflns_used    891
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      20.57
_cell_measurement_theta_min      2.35
_cell_volume                     6022.3(19)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2001)'
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.932
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0729
_diffrn_reflns_av_sigmaI/netI    0.0688
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            66134
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        1
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_T_max  0.9594
_exptl_absorpt_correction_T_min  0.7970
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2003)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.618
_exptl_crystal_description       plate
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_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.07
_platon_squeeze_details
;
PLATON Reference : Spek, A.L. (2003), J.Appl.Cryst. 36, 7-13
VOid space analysis consistent with initial structure 
solutions showing one disordered, noncoordinated
pyridine molecule in the asymmetric unit
located away from the compound molecule.
;
_refine_diff_density_max         0.846
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     858
_refine_ls_number_reflns         13880
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.070
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0566
_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^)+(0.0731P)^2] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1351
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                9690
_reflns_number_total             13880
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070794isi20070413_011733.cif
_cod_data_source_block           tomv004s
_cod_original_cell_volume        6022.4(18)
_cod_database_code               4109554