#------------------------------------------------------------------------------
#$Date: 2016-03-21 15:14:41 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178741 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/52/4085236.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_4085236
loop_
_publ_author_name
'El Ezzi, Mohammad'
'Kocsor, Tibor-Gabor'
'D’Accriscio, Florian'
'Madec, David'
'Mallet-Ladeira, Sonia'
'Castel, Annie'
_publ_section_title
;
 Iron Complexes with Stabilized Germylenes: Syntheses and
 Characterizations
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              571
_journal_paper_doi               10.1021/om500903g
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C38 H46 Fe2 Ge2 N4 O9'
_chemical_formula_weight         959.67
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                90.00
_cell_angle_beta                 114.730(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   23.6993(13)
_cell_length_b                   10.2634(6)
_cell_length_c                   19.5151(10)
_cell_measurement_reflns_used    7982
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      27.60
_cell_measurement_theta_min      2.20
_cell_volume                     4311.4(4)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker kappa APEX-II CCD Quazar'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0350
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            39979
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         5.14
_exptl_absorpt_coefficient_mu    2.095
_exptl_absorpt_correction_T_max  0.8503
_exptl_absorpt_correction_T_min  0.6794
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker-AXS)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.478
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       blcok
_exptl_crystal_F_000             1960
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.110
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         5314
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0477
_refine_ls_R_factor_gt           0.0312
_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/[σ²(Fo²)+(0.0281P)²+5.9227P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0733
_reflns_number_gt                4235
_reflns_number_total             5314
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om500903g_si_001.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2935 2014-11-11 08:27:57Z andrius 

 Adding full bibliography for 4085233--4085238.cif.
;
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4085236
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+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
Ge1 Ge 0.421744(10) 0.81090(2) 0.223962(12) 0.02193(7) Uani 1 1 d .
N1 N 0.39645(9) 0.66646(17) 0.26973(10) 0.0251(4) Uani 1 1 d .
N2 N 0.41297(8) 0.86176(17) 0.31601(10) 0.0237(4) Uani 1 1 d .
C1 C 0.39267(9) 0.7430(2) 0.32240(11) 0.0232(4) Uani 1 1 d .
C2 C 0.36844(11) 0.7039(2) 0.37830(12) 0.0288(5) Uani 1 1 d .
C3 C 0.30549(12) 0.7161(3) 0.35969(15) 0.0382(6) Uani 1 1 d .
H3 H 0.2780 0.7464 0.3111 0.046 Uiso 1 1 calc R
C4 C 0.28282(15) 0.6836(3) 0.41271(18) 0.0537(8) Uani 1 1 d .
H4 H 0.2397 0.6920 0.4005 0.064 Uiso 1 1 calc R
C5 C 0.32260(17) 0.6396(3) 0.48259(18) 0.0601(9) Uani 1 1 d .
H5 H 0.3069 0.6187 0.5188 0.072 Uiso 1 1 calc R
C6 C 0.38531(17) 0.6252(3) 0.50098(17) 0.0592(9) Uani 1 1 d .
H6 H 0.4124 0.5934 0.5493 0.071 Uiso 1 1 calc R
C7 C 0.40840(13) 0.6573(3) 0.44876(14) 0.0422(6) Uani 1 1 d .
H7 H 0.4514 0.6474 0.4611 0.051 Uiso 1 1 calc R
C8 C 0.38861(11) 0.5247(2) 0.25805(13) 0.0304(5) Uani 1 1 d .
C9 C 0.32457(14) 0.4791(3) 0.24773(19) 0.0545(8) Uani 1 1 d .
H9A H 0.3208 0.4869 0.2957 0.082 Uiso 1 1 calc R
H9B H 0.3188 0.3879 0.2313 0.082 Uiso 1 1 calc R
H9C H 0.2928 0.5331 0.2095 0.082 Uiso 1 1 calc R
C10 C 0.43880(16) 0.4526(3) 0.32375(18) 0.0581(8) Uani 1 1 d .
H10A H 0.4794 0.4911 0.3343 0.087 Uiso 1 1 calc R
H10B H 0.4389 0.3605 0.3105 0.087 Uiso 1 1 calc R
H10C H 0.4303 0.4600 0.3686 0.087 Uiso 1 1 calc R
C11 C 0.39608(15) 0.4983(3) 0.18535(17) 0.0506(7) Uani 1 1 d .
H11A H 0.3633 0.5438 0.1434 0.076 Uiso 1 1 calc R
H11B H 0.3929 0.4044 0.1752 0.076 Uiso 1 1 calc R
H11C H 0.4368 0.5297 0.1908 0.076 Uiso 1 1 calc R
C12 C 0.40932(11) 0.9875(2) 0.35062(13) 0.0300(5) Uani 1 1 d .
C13 C 0.46291(12) 1.0686(2) 0.34975(15) 0.0382(6) Uani 1 1 d .
H13A H 0.5023 1.0248 0.3797 0.057 Uiso 1 1 calc R
H13B H 0.4627 1.1547 0.3714 0.057 Uiso 1 1 calc R
H13C H 0.4581 1.0786 0.2977 0.057 Uiso 1 1 calc R
C14 C 0.34701(12) 1.0523(3) 0.30389(17) 0.0494(7) Uani 1 1 d .
H14A H 0.3428 1.0660 0.2523 0.074 Uiso 1 1 calc R
H14B H 0.3449 1.1364 0.3265 0.074 Uiso 1 1 calc R
H14C H 0.3132 0.9960 0.3029 0.074 Uiso 1 1 calc R
C15 C 0.41791(14) 0.9731(3) 0.43276(15) 0.0463(7) Uani 1 1 d .
H15A H 0.3814 0.9298 0.4339 0.070 Uiso 1 1 calc R
H15B H 0.4227 1.0595 0.4559 0.070 Uiso 1 1 calc R
H15C H 0.4551 0.9208 0.4609 0.070 Uiso 1 1 calc R
Fe1 Fe 0.358019(15) 0.88576(3) 0.106194(17) 0.02805(9) Uani 1 1 d .
C16 C 0.29531(12) 0.8353(3) 0.12887(15) 0.0389(6) Uani 1 1 d .
C17 C 0.38413(11) 1.0483(3) 0.13190(14) 0.0353(5) Uani 1 1 d .
C18 C 0.30642(13) 0.9295(3) 0.01243(15) 0.0426(6) Uani 1 1 d .
C19 C 0.40226(13) 0.7812(3) 0.07362(14) 0.0380(6) Uani 1 1 d .
O1 O 0.5000 0.7773(2) 0.2500 0.0360(5) Uani 1 2 d S
O2 O 0.25530(9) 0.8071(2) 0.14417(13) 0.0615(6) Uani 1 1 d .
O3 O 0.39866(10) 1.15491(19) 0.14656(12) 0.0547(5) Uani 1 1 d .
O4 O 0.27336(10) 0.9599(2) -0.04721(11) 0.0645(6) Uani 1 1 d .
O5 O 0.43046(11) 0.7173(2) 0.05148(12) 0.0600(6) Uani 1 1 d .
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'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 '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
O1 Ge1 N1 102.11(9) .
O1 Ge1 N2 107.06(6) .
N1 Ge1 N2 67.21(7) .
O1 Ge1 Fe1 122.29(3) .
N1 Ge1 Fe1 120.96(6) .
N2 Ge1 Fe1 123.43(5) .
C1 N1 C8 131.31(18) .
C1 N1 Ge1 92.19(13) .
C8 N1 Ge1 136.34(14) .
C1 N2 C12 131.52(18) .
C1 N2 Ge1 91.32(13) .
C12 N2 Ge1 134.45(14) .
N1 C1 N2 108.92(18) .
N1 C1 C2 125.6(2) .
N2 C1 C2 125.50(19) .
C3 C2 C7 120.3(2) .
C3 C2 C1 119.2(2) .
C7 C2 C1 120.5(2) .
C2 C3 C4 119.5(3) .
C5 C4 C3 120.0(3) .
C4 C5 C6 120.7(3) .
C7 C6 C5 119.8(3) .
C6 C7 C2 119.7(3) .
N1 C8 C9 112.3(2) .
N1 C8 C11 105.25(18) .
C9 C8 C11 108.7(2) .
N1 C8 C10 110.2(2) .
C9 C8 C10 110.3(2) .
C11 C8 C10 110.0(2) .
N2 C12 C13 105.29(18) .
N2 C12 C14 109.57(19) .
C13 C12 C14 111.0(2) .
N2 C12 C15 112.7(2) .
C13 C12 C15 108.5(2) .
C14 C12 C15 109.8(2) .
C17 Fe1 C18 93.55(12) .
C17 Fe1 C19 118.42(12) .
C18 Fe1 C19 92.21(12) .
C17 Fe1 C16 115.32(12) .
C18 Fe1 C16 92.44(12) .
C19 Fe1 C16 125.59(12) .
C17 Fe1 Ge1 91.50(8) .
C18 Fe1 Ge1 174.95(10) .
C19 Fe1 Ge1 85.24(8) .
C16 Fe1 Ge1 85.54(8) .
O2 C16 Fe1 177.8(3) .
O3 C17 Fe1 177.3(2) .
O4 C18 Fe1 178.7(3) .
O5 C19 Fe1 178.0(2) .
Ge1 O1 Ge1 157.13(16) 2_655
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ge1 O1 1.7402(6) .
Ge1 N1 1.9499(17) .
Ge1 N2 1.9633(17) .
Ge1 Fe1 2.2911(4) .
N1 C1 1.326(3) .
N1 C8 1.473(3) .
N2 C1 1.335(3) .
N2 C12 1.476(3) .
C1 C2 1.485(3) .
C2 C3 1.386(3) .
C2 C7 1.388(3) .
C3 C4 1.391(4) .
C4 C5 1.370(5) .
C5 C6 1.383(5) .
C6 C7 1.383(4) .
C8 C9 1.519(3) .
C8 C11 1.525(3) .
C8 C10 1.526(4) .
C12 C13 1.525(3) .
C12 C14 1.526(3) .
C12 C15 1.536(3) .
Fe1 C17 1.777(3) .
Fe1 C18 1.781(3) .
Fe1 C19 1.793(3) .
Fe1 C16 1.795(3) .
C16 O2 1.144(3) .
C17 O3 1.147(3) .
C18 O4 1.142(3) .
C19 O5 1.142(3) .
O1 Ge1 1.7402(6) 2_655
