#------------------------------------------------------------------------------
#$Date: 2016-03-21 19:14:39 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178841 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/95/4109552.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4109552
loop_
_publ_author_name
'Julie A. Cissell'
'Thomas P. Vaid'
'Glenn P. A. Yap'
_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            'C44 H28 Ge N4'
_chemical_formula_weight         685.29
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           87
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4'
_symmetry_space_group_name_H-M   'I 4/m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.302(3)
_cell_length_b                   13.302(3)
_cell_length_c                   9.662(4)
_cell_measurement_reflns_used    904
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.16
_cell_measurement_theta_min      2.17
_cell_volume                     1709.6(9)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_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 0.954
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       ω
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0274
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7192
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.17
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.934
_exptl_absorpt_correction_T_max  0.8804
_exptl_absorpt_correction_T_min  0.8209
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.331
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.555
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     71
_refine_ls_number_reflns         1068
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0611
_refine_ls_R_factor_gt           0.0605
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0577P)²+8.9516P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1575
_refine_ls_wR_factor_ref         0.1577
_reflns_number_gt                1050
_reflns_number_total             1068
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja070794isi20070203_052825.cif
_cod_data_source_block           tomv002
_cod_original_cell_volume        1709.6(10)
_cod_database_code               4109552
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-y, x, z'
'y, -x, z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-y+1/2, x+1/2, z+1/2'
'y+1/2, -x+1/2, z+1/2'
'-x, -y, -z'
'x, y, -z'
'y, -x, -z'
'-y, x, -z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'y+1/2, -x+1/2, -z+1/2'
'-y+1/2, x+1/2, -z+1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Ge Ge 0.0000 0.0000 0.09022(13) 0.0202(3) Uani 0.50 4 d SP
N1 N 0.1472(3) 0.0351(3) 0.0000 0.0215(7) Uani 1 2 d S
C1 C 0.2269(3) -0.0310(3) 0.0000 0.0220(9) Uani 1 2 d S
C2 C 0.3201(3) 0.0232(3) 0.0000 0.0269(10) Uani 1 2 d S
H2A H 0.3858 -0.0050 0.0000 0.032 Uiso 1 2 calc SR
C3 C 0.2963(3) 0.1230(3) 0.0000 0.0257(9) Uani 1 2 d S
H3A H 0.3423 0.1777 0.0000 0.031 Uiso 1 2 calc SR
C4 C 0.1888(3) 0.1296(3) 0.0000 0.0219(9) Uani 1 2 d S
C5 C 0.1356(3) 0.2204(3) 0.0000 0.0212(8) Uani 1 2 d S
C6 C 0.1944(3) 0.3169(3) 0.0000 0.0215(9) Uani 1 2 d S
C7 C 0.2207(3) 0.3621(3) -0.1236(4) 0.0341(8) Uani 1 1 d .
H7A H 0.2015 0.3322 -0.2089 0.041 Uiso 1 1 calc R
C8 C 0.2756(3) 0.4518(3) -0.1232(5) 0.0391(9) Uani 1 1 d .
H8A H 0.2945 0.4821 -0.2084 0.047 Uiso 1 1 calc R
C9 C 0.3023(3) 0.4964(4) 0.0000 0.0342(11) Uani 1 2 d S
H9A H 0.3390 0.5576 0.0000 0.041 Uiso 1 2 calc SR
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Ge 0.0163(4) 0.0163(4) 0.0279(6) 0.000 0.000 0.000
N1 0.0151(16) 0.0142(15) 0.0351(19) 0.000 0.000 0.0012(12)
C1 0.0163(18) 0.021(2) 0.029(2) 0.000 0.000 0.0012(15)
C2 0.0143(18) 0.021(2) 0.045(3) 0.000 0.000 0.0017(15)
C3 0.020(2) 0.018(2) 0.040(2) 0.000 0.000 -0.0024(16)
C4 0.0179(19) 0.0187(19) 0.029(2) 0.000 0.000 -0.0019(15)
C5 0.0189(19) 0.0137(18) 0.031(2) 0.000 0.000 -0.0040(15)
C6 0.0167(18) 0.0130(18) 0.035(2) 0.000 0.000 -0.0006(14)
C7 0.0416(19) 0.0257(16) 0.0351(18) -0.0013(14) 0.0054(15) -0.0101(14)
C8 0.040(2) 0.0277(17) 0.050(2) 0.0100(16) 0.0081(17) -0.0077(14)
C9 0.018(2) 0.0144(19) 0.070(3) 0.000 0.000 -0.0033(16)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
Ge Ge N1 66.59(5) 9 11
Ge Ge N1 66.59(5) 9 9
N1 Ge N1 80.92(4) 11 9
Ge Ge N1 66.59(5) 9 .
N1 Ge N1 80.91(4) 11 .
N1 Ge N1 133.17(10) 9 .
Ge Ge N1 66.59(5) 9 3
N1 Ge N1 133.17(10) 11 3
N1 Ge N1 80.91(4) 9 3
N1 Ge N1 80.91(4) . 3
C4 N1 C1 105.9(3) . .
C4 N1 Ge 123.7(2) . 9
C1 N1 Ge 123.5(2) . 9
C4 N1 Ge 123.7(2) . .
C1 N1 Ge 123.5(2) . .
Ge N1 Ge 46.83(10) 9 .
N1 C1 C5 126.2(4) . 11
N1 C1 C2 110.2(4) . .
C5 C1 C2 123.6(4) 11 .
C3 C2 C1 106.7(4) . .
C2 C3 C4 106.9(4) . .
N1 C4 C5 125.9(4) . .
N1 C4 C3 110.3(4) . .
C5 C4 C3 123.8(4) . .
C1 C5 C4 123.9(4) 3 .
C1 C5 C6 117.8(4) 3 .
C4 C5 C6 118.3(4) . .
C7 C6 C7 119.6(4) . 10
C7 C6 C5 120.2(2) . .
C7 C6 C5 120.2(2) 10 .
C6 C7 C8 120.1(4) . .
C9 C8 C7 120.2(4) . .
C8 C9 C8 119.8(4) 10 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge Ge 1.743(3) 9
Ge N1 2.194(3) 11
Ge N1 2.194(3) 9
Ge N1 2.194(3) .
Ge N1 2.194(3) 3
N1 C4 1.373(5) .
N1 C1 1.376(5) .
N1 Ge 2.194(3) 9
C1 C5 1.394(6) 11
C1 C2 1.435(6) .
C2 C3 1.366(6) .
C3 C4 1.433(6) .
C4 C5 1.401(6) .
C5 C1 1.394(6) 3
C5 C6 1.503(5) .
C6 C7 1.381(4) .
C6 C7 1.382(4) 10
C7 C8 1.399(5) .
C8 C9 1.376(5) .
C9 C8 1.376(5) 10
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_4
Ge Ge N1 C4 106.78(17) 9 .
N1 Ge N1 C4 175.10(16) 11 .
N1 Ge N1 C4 106.77(17) 9 .
N1 Ge N1 C4 38.45(19) 3 .
Ge Ge N1 C1 -106.63(17) 9 .
N1 Ge N1 C1 -38.30(19) 11 .
N1 Ge N1 C1 -106.63(17) 9 .
N1 Ge N1 C1 -174.96(16) 3 .
N1 Ge N1 Ge 68.33(4) 11 9
N1 Ge N1 Ge 0.0 9 9
N1 Ge N1 Ge -68.33(4) 3 9
C4 N1 C1 C5 180.0 . 11
Ge N1 C1 C5 -28.44(12) 9 11
Ge N1 C1 C5 28.44(12) . 11
C4 N1 C1 C2 0.0 . .
Ge N1 C1 C2 151.56(12) 9 .
Ge N1 C1 C2 -151.56(12) . .
N1 C1 C2 C3 0.0 . .
C5 C1 C2 C3 180.0 11 .
C1 C2 C3 C4 0.0 . .
C1 N1 C4 C5 180.0 . .
Ge N1 C4 C5 28.53(12) 9 .
Ge N1 C4 C5 -28.53(12) . .
C1 N1 C4 C3 0.0 . .
Ge N1 C4 C3 -151.47(12) 9 .
Ge N1 C4 C3 151.47(12) . .
C2 C3 C4 N1 0.0 . .
C2 C3 C4 C5 180.0 . .
N1 C4 C5 C1 0.0 . 3
C3 C4 C5 C1 180.0 . 3
N1 C4 C5 C6 180.0 . .
C3 C4 C5 C6 0.0 . .
C1 C5 C6 C7 -89.3(4) 3 .
C4 C5 C6 C7 90.7(4) . .
C1 C5 C6 C7 89.3(4) 3 10
C4 C5 C6 C7 -90.7(4) . 10
C7 C6 C7 C8 1.4(7) 10 .
C5 C6 C7 C8 -179.9(4) . .
C6 C7 C8 C9 -1.0(6) . .
C7 C8 C9 C8 0.6(7) . 10
