#------------------------------------------------------------------------------
#$Date: 2016-03-23 23:39:14 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179510 $
#$URL: svn://www.crystallography.net/cod/cif/4/34/07/4340793.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_4340793
loop_
_publ_author_name
'Cabeza, Javier A.'
'García-Álvarez, Pablo'
'Pérez-Carreño, Enrique'
'Polo, Diego'
_publ_section_title
;
 Conversion of a Monodentate Amidinate-Germylene Ligand into Chelating
 Imine-Germanate Ligands (on Mononuclear Manganese Complexes).
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              8735
_journal_page_last               8741
_journal_paper_doi               10.1021/ic501418p
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         'C21 H28 F Ge Mn N2 O4'
_chemical_formula_sum            'C21 H28 F Ge Mn N2 O4'
_chemical_formula_weight         518.98
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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                 104.035(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.8389(3)
_cell_length_b                   9.2287(2)
_cell_length_c                   18.2058(4)
_cell_measurement_reflns_used    3249
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      68.2220
_cell_measurement_theta_min      4.4080
_cell_volume                     2418.74(9)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'MERCUY CSD 3.1 (Build RC5)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Giacovazzo, 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_diffrn_measurement_device_type  'Xcalibur, Onyx, Nova'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0443
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            9963
_diffrn_reflns_theta_full        69.31
_diffrn_reflns_theta_max         69.31
_diffrn_reflns_theta_min         4.41
_exptl_absorpt_coefficient_mu    6.079
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89254
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             1064
_exptl_crystal_size_max          0.0538
_exptl_crystal_size_mid          0.0439
_exptl_crystal_size_min          0.0302
_refine_diff_density_max         1.480
_refine_diff_density_min         -0.432
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.150
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         4421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.150
_refine_ls_R_factor_all          0.0648
_refine_ls_R_factor_gt           0.0484
_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)+(0.0792P)²+0.4504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1370
_refine_ls_wR_factor_ref         0.1486
_reflns_number_gt                3450
_reflns_number_total             4421
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic501418p_si_002.cif
_cod_data_source_block           xn14_036_dp408
_cod_depositor_comments
'Adding full bibliography for 4340791--4340795.cif.'
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4340793
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
C1 C -0.0946(4) 0.0181(7) 0.8044(4) 0.0693(15) Uani 1 1 d .
H1A H -0.0589 -0.0156 0.7689 0.104 Uiso 1 1 calc R
H1B H -0.1499 -0.0428 0.7995 0.104 Uiso 1 1 calc R
H1C H -0.0561 0.0118 0.8562 0.104 Uiso 1 1 calc R
C2 C -0.1739(3) 0.2409(6) 0.8398(3) 0.0485(11) Uani 1 1 d .
H2A H -0.2248 0.1780 0.8460 0.073 Uiso 1 1 calc R
H2B H -0.1992 0.3342 0.8186 0.073 Uiso 1 1 calc R
H2C H -0.1307 0.2567 0.8891 0.073 Uiso 1 1 calc R
C3 C -0.1233(3) 0.1700(5) 0.7869(3) 0.0484(11) Uani 1 1 d .
H3 H -0.1722 0.1619 0.7385 0.058 Uiso 1 1 calc R
C4 C 0.0233(3) 0.3218(5) 0.8154(2) 0.0371(9) Uani 1 1 d .
C5 C 0.0646(3) 0.2336(5) 0.8842(2) 0.0396(9) Uani 1 1 d .
C6 C 0.1201(3) 0.1157(5) 0.8752(3) 0.0455(10) Uani 1 1 d .
H6 H 0.1304 0.0946 0.8269 0.055 Uiso 1 1 calc R
C7 C 0.1601(3) 0.0295(6) 0.9370(3) 0.0569(13) Uani 1 1 d .
H7 H 0.1983 -0.0502 0.9314 0.068 Uiso 1 1 calc R
C8 C 0.1437(4) 0.0608(6) 1.0068(3) 0.0634(16) Uani 1 1 d .
H8 H 0.1706 0.0014 1.0490 0.076 Uiso 1 1 calc R
C9 C 0.0889(4) 0.1770(7) 1.0162(3) 0.0612(14) Uani 1 1 d .
H9 H 0.0786 0.1977 1.0646 0.073 Uiso 1 1 calc R
C10 C 0.0492(3) 0.2632(5) 0.9544(3) 0.0467(11) Uani 1 1 d .
H10 H 0.0111 0.3430 0.9605 0.056 Uiso 1 1 calc R
C11 C 0.1494(3) 0.4884(5) 0.8576(3) 0.0509(12) Uani 1 1 d .
H11 H 0.1689 0.4051 0.8930 0.061 Uiso 1 1 calc R
C12 C 0.2300(3) 0.5180(7) 0.8205(4) 0.0716(17) Uani 1 1 d .
H12A H 0.2389 0.4340 0.7901 0.107 Uiso 1 1 calc R
H12B H 0.2870 0.5355 0.8599 0.107 Uiso 1 1 calc R
H12C H 0.2157 0.6035 0.7878 0.107 Uiso 1 1 calc R
C13 C 0.1302(4) 0.6144(6) 0.9049(4) 0.0683(16) Uani 1 1 d .
H13A H 0.1118 0.6992 0.8724 0.102 Uiso 1 1 calc R
H13B H 0.1864 0.6370 0.9441 0.102 Uiso 1 1 calc R
H13C H 0.0800 0.5883 0.9288 0.102 Uiso 1 1 calc R
C14 C -0.0854(3) 0.2161(6) 0.5889(3) 0.0496(11) Uani 1 1 d .
C15 C 0.0062(4) 0.1325(7) 0.6082(3) 0.0642(15) Uani 1 1 d .
H15A H 0.0058 0.0592 0.5692 0.096 Uiso 1 1 calc R
H15B H 0.0137 0.0850 0.6574 0.096 Uiso 1 1 calc R
H15C H 0.0579 0.1998 0.6103 0.096 Uiso 1 1 calc R
C16 C -0.1676(4) 0.1120(7) 0.5787(4) 0.0757(18) Uani 1 1 d .
H16A H -0.2256 0.1674 0.5686 0.113 Uiso 1 1 calc R
H16B H -0.1617 0.0547 0.6250 0.113 Uiso 1 1 calc R
H16C H -0.1681 0.0470 0.5360 0.113 Uiso 1 1 calc R
C17 C -0.0932(5) 0.3007(8) 0.5158(3) 0.0715(17) Uani 1 1 d .
H17A H -0.0917 0.2333 0.4745 0.107 Uiso 1 1 calc R
H17B H -0.0410 0.3686 0.5222 0.107 Uiso 1 1 calc R
H17C H -0.1518 0.3547 0.5036 0.107 Uiso 1 1 calc R
C101 C 0.0902(4) 0.4996(6) 0.6568(3) 0.0592(13) Uani 1 1 d .
C102 C 0.0686(4) 0.7411(6) 0.7316(4) 0.0605(14) Uani 1 1 d .
C103 C -0.0815(3) 0.6159(5) 0.7608(3) 0.0441(10) Uani 1 1 d .
C104 C -0.0643(4) 0.6550(6) 0.6200(3) 0.0586(13) Uani 1 1 d .
F1 F -0.20555(16) 0.3895(3) 0.65986(15) 0.0490(6) Uani 1 1 d .
Ge1 Ge -0.08488(3) 0.35986(6) 0.67015(3) 0.03826(17) Uani 1 1 d .
Mn1 Mn 0.00447(5) 0.57206(8) 0.70541(4) 0.0440(2) Uani 1 1 d .
N1 N -0.0535(2) 0.2693(4) 0.76684(19) 0.0374(8) Uani 1 1 d .
N2 N 0.0636(2) 0.4420(4) 0.8014(2) 0.0389(8) Uani 1 1 d .
O101 O 0.1443(3) 0.4556(5) 0.6274(3) 0.0805(13) Uani 1 1 d .
O102 O 0.1039(3) 0.8511(4) 0.7417(3) 0.0803(13) Uani 1 1 d .
O103 O -0.1321(2) 0.6390(4) 0.7968(2) 0.0571(9) Uani 1 1 d .
O104 O -0.1095(3) 0.7061(5) 0.5668(2) 0.0784(12) 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 0.0181 0.0091 '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'
F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Mn Mn -0.5299 2.8052 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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
C1 C3 N1 117.0(4)
C1 C3 C2 116.0(5)
N1 C3 C2 111.9(4)
N2 C4 N1 121.7(4)
N2 C4 C5 120.6(4)
N1 C4 C5 117.5(4)
C10 C5 C6 119.9(4)
C10 C5 C4 122.8(4)
C6 C5 C4 117.3(4)
C7 C6 C5 119.9(5)
C8 C7 C6 119.4(5)
C7 C8 C9 121.1(5)
C8 C9 C10 119.4(5)
C5 C10 C9 120.3(5)
N2 C11 C13 111.3(4)
N2 C11 C12 112.2(5)
C13 C11 C12 112.8(5)
C17 C14 C15 109.6(4)
C17 C14 C16 109.1(5)
C15 C14 C16 110.5(5)
C17 C14 Ge1 107.1(4)
C15 C14 Ge1 108.9(3)
C16 C14 Ge1 111.6(4)
O101 C101 Mn1 179.0(6)
O102 C102 Mn1 173.7(6)
O103 C103 Mn1 177.3(4)
O104 C104 Mn1 178.4(5)
F1 Ge1 N1 100.37(13)
F1 Ge1 C14 101.70(17)
N1 Ge1 C14 110.62(18)
F1 Ge1 Mn1 112.68(10)
N1 Ge1 Mn1 96.73(11)
C14 Ge1 Mn1 130.99(16)
C104 Mn1 C102 90.7(3)
C104 Mn1 C101 93.0(2)
C102 Mn1 C101 93.4(3)
C104 Mn1 C103 93.2(2)
C102 Mn1 C103 93.1(2)
C101 Mn1 C103 170.9(2)
C104 Mn1 N2 168.3(2)
C102 Mn1 N2 100.5(2)
C101 Mn1 N2 89.70(19)
C103 Mn1 N2 82.93(17)
C104 Mn1 Ge1 87.40(19)
C102 Mn1 Ge1 177.33(17)
C101 Mn1 Ge1 88.62(19)
C103 Mn1 Ge1 85.07(15)
N2 Mn1 Ge1 81.26(10)
C4 N1 C3 125.8(4)
C4 N1 Ge1 115.3(3)
C3 N1 Ge1 117.9(3)
C4 N2 C11 117.5(4)
C4 N2 Mn1 121.3(3)
C11 N2 Mn1 121.0(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
C1 C3 1.477(8)
C2 C3 1.506(7)
C3 N1 1.494(6)
C4 N2 1.314(6)
C4 N1 1.352(5)
C4 C5 1.495(6)
C5 C10 1.379(6)
C5 C6 1.398(7)
C6 C7 1.388(7)
C7 C8 1.379(9)
C8 C9 1.382(9)
C9 C10 1.388(7)
C11 N2 1.490(6)
C11 C13 1.515(8)
C11 C12 1.534(7)
C14 C17 1.523(7)
C14 C15 1.528(7)
C14 C16 1.528(9)
C14 Ge1 1.986(5)
C101 O101 1.142(7)
C101 Mn1 1.843(6)
C102 O102 1.136(7)
C102 Mn1 1.829(6)
C103 O103 1.130(6)
C103 Mn1 1.853(5)
C104 O104 1.138(6)
C104 Mn1 1.810(6)
F1 Ge1 1.776(2)
Ge1 N1 1.901(3)
Ge1 Mn1 2.3647(9)
Mn1 N2 2.126(4)
