#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321619.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_4321619
loop_
_publ_author_name
'Dominique Agustin'
'Ghassoub Rima'
'Heinz Gornitzka'
'Jacques Barrau'
_publ_section_title
;
 (Schiff Base) Divalent Group 14 Element Species: Manganese and Iron
 Complexes (Salen)MMn(CO)2(η5-C5H5) (M14= Ge, Sn, Pb) and
 (Salen)SnFe(CO)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5492
_journal_page_last               5495
_journal_paper_doi               10.1021/ic9915045
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C20 H14 Fe N2 O6 Sn'
_chemical_formula_weight         552.87
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.55(3)
_cell_angle_beta                 105.15(3)
_cell_angle_gamma                100.84(3)
_cell_formula_units_Z            2
_cell_length_a                   8.465(2)
_cell_length_b                   9.795(3)
_cell_length_c                   13.213(4)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.3
_cell_measurement_theta_min      2.2
_cell_volume                     978.7(6)
_computing_cell_refinement       STOE-IPDS
_computing_data_collection       STOE-IPDS
_computing_data_reduction        STOE-IPDS
_computing_molecular_graphics    'ZORTEP (Zsolnai, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  STOE-IPDS
_diffrn_measurement_method       phi-rotation
_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  0.0798
_diffrn_reflns_av_sigmaI/netI    0.0648
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7995
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    2.058
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.876
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             544
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         1.924
_refine_diff_density_min         -1.438
_refine_diff_density_rms         0.261
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     271
_refine_ls_number_reflns         2664
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.074
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0552
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1108P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1414
_refine_ls_wR_factor_ref         0.1457
_reflns_number_gt                2297
_reflns_number_total             2664
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9915045_2.cif
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1108P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        978.7(5)
_cod_database_code               4321619
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.33052(6) 0.55721(5) 0.33756(4) 0.0222(2) Uani 1 d . . .
Fe1 Fe 0.12160(13) 0.63153(11) 0.20760(9) 0.0256(3) Uani 1 d . . .
O1 O 0.2764(7) 0.5567(5) 0.4809(5) 0.0294(12) Uani 1 d . . .
O2 O 0.2890(6) 0.3357(5) 0.3090(5) 0.0265(11) Uani 1 d . . .
O3 O 0.3690(9) 0.6882(9) 0.0944(6) 0.0538(18) Uani 1 d . . .
O4 O -0.0879(8) 0.3252(6) 0.1279(5) 0.0404(14) Uani 1 d . . .
O5 O -0.1545(10) 0.6962(9) 0.0620(7) 0.063(2) Uani 1 d . . .
O6 O 0.1113(8) 0.8697(7) 0.3942(6) 0.0448(15) Uani 1 d . . .
N1 N 0.5627(8) 0.7289(7) 0.4606(6) 0.0294(15) Uani 1 d . . .
N2 N 0.5477(8) 0.5292(7) 0.2767(6) 0.0297(15) Uani 1 d . . .
C1 C 0.2833(10) 0.6819(8) 0.5551(6) 0.0263(16) Uani 1 d . . .
C2 C 0.1596(10) 0.6843(9) 0.6071(7) 0.0322(18) Uani 1 d . . .
H2 H 0.0720 0.5964 0.5885 0.039 Uiso 1 calc R . .
C3 C 0.1613(12) 0.8100(9) 0.6842(8) 0.039(2) Uani 1 d . . .
H3 H 0.0738 0.8088 0.7169 0.046 Uiso 1 calc R . .
C4 C 0.2915(12) 0.9416(9) 0.7157(8) 0.038(2) Uani 1 d . . .
H4 H 0.2917 1.0293 0.7686 0.046 Uiso 1 calc R . .
C5 C 0.4152(12) 0.9407(9) 0.6698(7) 0.037(2) Uani 1 d . . .
H5 H 0.5057 1.0281 0.6935 0.044 Uiso 1 calc R . .
C6 C 0.4157(10) 0.8153(9) 0.5879(7) 0.0303(17) Uani 1 d . . .
C7 C 0.5568(10) 0.8214(8) 0.5490(7) 0.0291(17) Uani 1 d . . .
H7 H 0.6562 0.9007 0.5919 0.035 Uiso 1 calc R . .
C8 C 0.7225(10) 0.7352(9) 0.4376(7) 0.0317(18) Uani 1 d . . .
H8A H 0.7883 0.6812 0.4779 0.038 Uiso 1 calc R . .
H8B H 0.7916 0.8390 0.4631 0.038 Uiso 1 calc R . .
C9 C 0.6833(10) 0.6660(9) 0.3139(8) 0.0332(19) Uani 1 d . . .
H9A H 0.6459 0.7335 0.2749 0.040 Uiso 1 calc R . .
H9B H 0.7859 0.6452 0.2980 0.040 Uiso 1 calc R . .
C10 C 0.5450(10) 0.4119(9) 0.2035(7) 0.0308(18) Uani 1 d . . .
H10 H 0.6351 0.4168 0.1731 0.037 Uiso 1 calc R . .
C11 C 0.4162(9) 0.2732(8) 0.1636(7) 0.0240(16) Uani 1 d . . .
C12 C 0.2951(9) 0.2411(8) 0.2172(6) 0.0247(16) Uani 1 d . . .
C13 C 0.1840(10) 0.0992(8) 0.1733(7) 0.0312(17) Uani 1 d . . .
H13 H 0.1052 0.0729 0.2092 0.037 Uiso 1 calc R . .
C14 C 0.1850(10) -0.0035(9) 0.0799(7) 0.0319(18) Uani 1 d . . .
H14 H 0.1049 -0.0980 0.0514 0.038 Uiso 1 calc R . .
C15 C 0.3007(11) 0.0281(9) 0.0260(7) 0.0327(18) Uani 1 d . . .
H15 H 0.3001 -0.0429 -0.0394 0.039 Uiso 1 calc R . .
C16 C 0.4163(10) 0.1656(9) 0.0705(7) 0.0317(18) Uani 1 d . . .
H16 H 0.4991 0.1876 0.0363 0.038 Uiso 1 calc R . .
C17 C 0.2723(11) 0.6656(10) 0.1400(7) 0.0352(19) Uani 1 d . . .
C18 C 0.0003(10) 0.4453(9) 0.1621(7) 0.0297(17) Uani 1 d . . .
C19 C -0.0466(11) 0.6705(9) 0.1177(8) 0.037(2) Uani 1 d . . .
C20 C 0.1216(10) 0.7751(9) 0.3237(8) 0.0328(19) Uani 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'
Fe Fe 0.3463 0.8444 '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'
Sn Sn -0.6537 1.4246 '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
_geom_angle_publ_flag
O2 Sn1 O1 83.2(2) . . ?
O2 Sn1 N2 82.4(2) . . ?
O1 Sn1 N2 135.2(2) . . ?
O2 Sn1 N1 124.6(2) . . ?
O1 Sn1 N1 81.4(2) . . ?
N2 Sn1 N1 72.6(3) . . ?
O2 Sn1 Fe1 116.19(16) . . ?
O1 Sn1 Fe1 114.02(16) . . ?
N2 Sn1 Fe1 110.44(18) . . ?
N1 Sn1 Fe1 118.77(16) . . ?
C18 Fe1 C17 114.6(4) . . ?
C18 Fe1 C19 89.9(4) . . ?
C17 Fe1 C19 96.7(4) . . ?
C18 Fe1 C20 125.4(4) . . ?
C17 Fe1 C20 119.5(4) . . ?
C19 Fe1 C20 90.9(4) . . ?
C18 Fe1 Sn1 84.7(3) . . ?
C17 Fe1 Sn1 89.3(3) . . ?
C19 Fe1 Sn1 173.2(3) . . ?
C20 Fe1 Sn1 88.9(3) . . ?
C1 O1 Sn1 120.6(4) . . ?
C12 O2 Sn1 123.5(4) . . ?
C7 N1 C8 120.7(7) . . ?
C7 N1 Sn1 121.5(5) . . ?
C8 N1 Sn1 117.8(5) . . ?
C10 N2 C9 122.3(7) . . ?
C10 N2 Sn1 123.9(5) . . ?
C9 N2 Sn1 113.1(5) . . ?
O1 C1 C2 119.3(7) . . ?
O1 C1 C6 123.2(7) . . ?
C2 C1 C6 117.4(7) . . ?
C3 C2 C1 121.6(8) . . ?
C2 C3 C4 120.8(8) . . ?
C5 C4 C3 118.7(8) . . ?
C4 C5 C6 122.4(8) . . ?
C5 C6 C7 118.6(7) . . ?
C5 C6 C1 119.0(8) . . ?
C7 C6 C1 122.1(7) . . ?
N1 C7 C6 126.0(7) . . ?
N1 C8 C9 108.7(6) . . ?
N2 C9 C8 107.3(7) . . ?
N2 C10 C11 125.2(7) . . ?
C16 C11 C12 119.6(7) . . ?
C16 C11 C10 117.3(7) . . ?
C12 C11 C10 123.0(7) . . ?
O2 C12 C13 119.2(7) . . ?
O2 C12 C11 123.8(6) . . ?
C13 C12 C11 116.9(7) . . ?
C14 C13 C12 122.0(8) . . ?
C13 C14 C15 121.3(7) . . ?
C16 C15 C14 117.7(8) . . ?
C15 C16 C11 122.3(8) . . ?
O3 C17 Fe1 178.9(8) . . ?
O4 C18 Fe1 175.6(7) . . ?
O5 C19 Fe1 178.8(9) . . ?
O6 C20 Fe1 175.1(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Sn1 O2 2.044(5) . ?
Sn1 O1 2.063(5) . ?
Sn1 N2 2.224(7) . ?
Sn1 N1 2.226(6) . ?
Sn1 Fe1 2.4846(14) . ?
Fe1 C18 1.769(8) . ?
Fe1 C17 1.770(9) . ?
Fe1 C19 1.774(9) . ?
Fe1 C20 1.782(9) . ?
O1 C1 1.329(10) . ?
O2 C12 1.334(10) . ?
O3 C17 1.159(11) . ?
O4 C18 1.163(10) . ?
O5 C19 1.128(11) . ?
O6 C20 1.159(11) . ?
N1 C7 1.292(11) . ?
N1 C8 1.455(11) . ?
N2 C10 1.280(11) . ?
N2 C9 1.459(10) . ?
C1 C2 1.395(12) . ?
C1 C6 1.429(11) . ?
C2 C3 1.366(12) . ?
C3 C4 1.410(13) . ?
C4 C5 1.341(14) . ?
C5 C6 1.404(12) . ?
C6 C7 1.416(13) . ?
C8 C9 1.509(13) . ?
C10 C11 1.439(11) . ?
C11 C16 1.389(12) . ?
C11 C12 1.425(11) . ?
C12 C13 1.394(11) . ?
C13 C14 1.370(12) . ?
C14 C15 1.390(13) . ?
C15 C16 1.377(12) . ?
