#------------------------------------------------------------------------------
#$Date: 2016-03-23 15:15:55 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179319 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/16/4321618.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_4321618
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            'C23 H19 Mn N2 O4 Sn'
_chemical_formula_weight         561.03
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   6.9720(10)
_cell_length_b                   15.678(2)
_cell_length_c                   19.032(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      24.28
_cell_measurement_theta_min      1.68
_cell_volume                     2080.3(5)
_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 0.986
_diffrn_measured_fraction_theta_max 0.986
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0156
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3316
_diffrn_reflns_theta_full        24.28
_diffrn_reflns_theta_max         24.28
_diffrn_reflns_theta_min         1.68
_exptl_absorpt_coefficient_mu    1.841
_exptl_absorpt_correction_T_max  0.8004
_exptl_absorpt_correction_T_min  0.7006
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.384
_refine_diff_density_min         -0.437
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         3316
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0288
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0629P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0733
_refine_ls_wR_factor_ref         0.0738
_reflns_number_gt                3174
_reflns_number_total             3316
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9915045_1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0629P)^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^)+(0.0629P)^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_database_code               4321618
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x+1/2, -y, 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_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.14291(4) 0.935899(15) 0.029595(15) 0.01986(10) Uani 1 d . . .
O1 O 0.3369(5) 0.8905(2) 0.10252(16) 0.0295(7) Uani 1 d . . .
C1 C 0.3198(7) 0.8490(3) 0.1632(2) 0.0265(10) Uani 1 d . . .
C2 C 0.4772(8) 0.8491(3) 0.2089(2) 0.0334(11) Uani 1 d . . .
H2 H 0.5892 0.8803 0.1967 0.040 Uiso 1 calc R . .
C3 C 0.4722(10) 0.8043(4) 0.2715(3) 0.0446(14) Uani 1 d . . .
H3 H 0.5792 0.8063 0.3023 0.054 Uiso 1 calc R . .
C4 C 0.3133(9) 0.7570(4) 0.2894(3) 0.0445(14) Uani 1 d . . .
H4 H 0.3134 0.7240 0.3313 0.053 Uiso 1 calc R . .
C5 C 0.1550(9) 0.7576(3) 0.2467(3) 0.0408(12) Uani 1 d . . .
H5 H 0.0447 0.7258 0.2600 0.049 Uiso 1 calc R . .
C6 C 0.1526(8) 0.8044(3) 0.1835(2) 0.0288(9) Uani 1 d . . .
C7 C -0.0211(7) 0.8035(3) 0.1437(2) 0.0267(10) Uani 1 d . . .
H7 H -0.1216 0.7678 0.1601 0.032 Uiso 1 calc R . .
N1 N -0.0531(5) 0.8468(2) 0.0876(2) 0.0244(8) Uani 1 d . . .
C8 C -0.2404(7) 0.8398(3) 0.0510(3) 0.0286(10) Uani 1 d . . .
H8A H -0.3068 0.8956 0.0508 0.034 Uiso 1 calc R . .
H8B H -0.3234 0.7976 0.0750 0.034 Uiso 1 calc R . .
C9 C -0.1980(6) 0.8111(3) -0.0238(3) 0.0279(9) Uani 1 d . . .
H9A H -0.1705 0.7492 -0.0245 0.033 Uiso 1 calc R . .
H9B H -0.3108 0.8219 -0.0541 0.033 Uiso 1 calc R . .
N2 N -0.0319(6) 0.8586(2) -0.05024(19) 0.0239(9) Uani 1 d . . .
C10 C -0.0047(7) 0.8670(3) -0.1167(2) 0.0272(10) Uani 1 d . . .
H10 H -0.1007 0.8469 -0.1479 0.033 Uiso 1 calc R . .
C11 C 0.1662(7) 0.9060(3) -0.1459(2) 0.0254(9) Uani 1 d . . .
C12 C 0.1624(8) 0.9294(3) -0.2173(2) 0.0363(11) Uani 1 d . . .
H12 H 0.0488 0.9207 -0.2440 0.044 Uiso 1 calc R . .
C13 C 0.3208(9) 0.9649(3) -0.2491(3) 0.0416(13) Uani 1 d . . .
H13 H 0.3159 0.9822 -0.2968 0.050 Uiso 1 calc R . .
C14 C 0.4890(9) 0.9749(3) -0.2100(3) 0.0385(12) Uani 1 d . . .
H14 H 0.5993 0.9989 -0.2316 0.046 Uiso 1 calc R . .
C15 C 0.4971(7) 0.9506(3) -0.1409(3) 0.0324(10) Uani 1 d . . .
H15 H 0.6134 0.9572 -0.1155 0.039 Uiso 1 calc R . .
C16 C 0.3367(7) 0.9162(3) -0.1073(2) 0.0249(9) Uani 1 d . . .
O2 O 0.3532(5) 0.89232(19) -0.03923(15) 0.0264(6) Uani 1 d . . .
Mn1 Mn 0.08154(9) 1.08930(4) 0.02914(4) 0.02459(16) Uani 1 d . . .
C17 C -0.1006(7) 1.0766(3) 0.0928(3) 0.0339(11) Uani 1 d . . .
O3 O -0.2202(6) 1.0665(3) 0.1348(2) 0.0517(10) Uani 1 d . . .
C18 C -0.0840(7) 1.0830(3) -0.0414(3) 0.0346(12) Uani 1 d . . .
O4 O -0.1870(6) 1.0841(2) -0.0894(2) 0.0505(11) Uani 1 d . . .
C19 C 0.3878(7) 1.1049(3) 0.0269(4) 0.0418(12) Uani 1 d . . .
H19 H 0.4781 1.0595 0.0257 0.050 Uiso 1 calc R . .
C20 C 0.3149(9) 1.1423(3) 0.0876(3) 0.0486(16) Uani 1 d . . .
H20 H 0.3454 1.1269 0.1346 0.058 Uiso 1 calc R . .
C21 C 0.1860(8) 1.2078(3) 0.0663(3) 0.0383(13) Uani 1 d . . .
H21 H 0.1150 1.2443 0.0965 0.046 Uiso 1 calc R . .
C22 C 0.1830(7) 1.2089(3) -0.0069(3) 0.0333(12) Uani 1 d . . .
H22 H 0.1097 1.2464 -0.0354 0.040 Uiso 1 calc R . .
C23 C 0.3079(7) 1.1444(3) -0.0315(4) 0.0401(11) Uani 1 d . . .
H23 H 0.3326 1.1305 -0.0792 0.048 Uiso 1 calc R . .
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'
Mn Mn 0.3368 0.7283 '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
O1 Sn1 O2 81.29(11) . . ?
O1 Sn1 N1 81.58(13) . . ?
O2 Sn1 N1 122.29(12) . . ?
O1 Sn1 N2 127.67(13) . . ?
O2 Sn1 N2 77.52(14) . . ?
N1 Sn1 N2 70.94(15) . . ?
O1 Sn1 Mn1 117.16(10) . . ?
O2 Sn1 Mn1 116.38(9) . . ?
N1 Sn1 Mn1 120.52(10) . . ?
N2 Sn1 Mn1 115.14(9) . . ?
C1 O1 Sn1 133.9(3) . . ?
O1 C1 C2 117.9(4) . . ?
O1 C1 C6 123.5(4) . . ?
C2 C1 C6 118.6(4) . . ?
C3 C2 C1 121.0(5) . . ?
C4 C3 C2 120.5(5) . . ?
C5 C4 C3 119.8(5) . . ?
C4 C5 C6 121.2(6) . . ?
C5 C6 C1 118.7(5) . . ?
C5 C6 C7 117.2(5) . . ?
C1 C6 C7 124.0(4) . . ?
N1 C7 C6 125.7(4) . . ?
C7 N1 C8 120.2(4) . . ?
C7 N1 Sn1 129.2(3) . . ?
C8 N1 Sn1 110.6(3) . . ?
N1 C8 C9 106.8(4) . . ?
N2 C9 C8 108.9(4) . . ?
C10 N2 C9 120.4(4) . . ?
C10 N2 Sn1 121.2(3) . . ?
C9 N2 Sn1 117.4(3) . . ?
N2 C10 C11 122.9(4) . . ?
C16 C11 C12 119.3(4) . . ?
C16 C11 C10 122.8(4) . . ?
C12 C11 C10 117.8(4) . . ?
C13 C12 C11 120.9(5) . . ?
C12 C13 C14 119.0(4) . . ?
C15 C14 C13 120.9(5) . . ?
C14 C15 C16 120.9(5) . . ?
O2 C16 C15 118.5(4) . . ?
O2 C16 C11 122.7(4) . . ?
C15 C16 C11 118.8(4) . . ?
C16 O2 Sn1 116.8(3) . . ?
C17 Mn1 C18 92.6(2) . . ?
C17 Mn1 C21 96.8(2) . . ?
C18 Mn1 C21 121.7(2) . . ?
C17 Mn1 C22 124.2(2) . . ?
C18 Mn1 C22 91.2(2) . . ?
C21 Mn1 C22 38.42(19) . . ?
C17 Mn1 C23 161.2(2) . . ?
C18 Mn1 C23 95.4(2) . . ?
C21 Mn1 C23 64.6(2) . . ?
C22 Mn1 C23 38.8(2) . . ?
C17 Mn1 C20 103.5(2) . . ?
C18 Mn1 C20 155.6(2) . . ?
C21 Mn1 C20 39.1(2) . . ?
C22 Mn1 C20 64.6(2) . . ?
C23 Mn1 C20 64.0(2) . . ?
C17 Mn1 C19 137.8(3) . . ?
C18 Mn1 C19 129.7(3) . . ?
C21 Mn1 C19 64.2(2) . . ?
C22 Mn1 C19 63.97(19) . . ?
C23 Mn1 C19 37.8(2) . . ?
C20 Mn1 C19 37.8(3) . . ?
C17 Mn1 Sn1 90.69(16) . . ?
C18 Mn1 Sn1 93.54(15) . . ?
C21 Mn1 Sn1 143.38(16) . . ?
C22 Mn1 Sn1 144.49(15) . . ?
C23 Mn1 Sn1 105.69(14) . . ?
C20 Mn1 Sn1 104.31(15) . . ?
C19 Mn1 Sn1 86.44(12) . . ?
O3 C17 Mn1 178.7(5) . . ?
O4 C18 Mn1 175.2(4) . . ?
C23 C19 C20 109.3(4) . . ?
C23 C19 Mn1 70.6(3) . . ?
C20 C19 Mn1 70.6(3) . . ?
C19 C20 C21 107.3(5) . . ?
C19 C20 Mn1 71.5(3) . . ?
C21 C20 Mn1 69.6(3) . . ?
C22 C21 C20 107.6(5) . . ?
C22 C21 Mn1 70.8(3) . . ?
C20 C21 Mn1 71.3(3) . . ?
C21 C22 C23 108.2(5) . . ?
C21 C22 Mn1 70.8(3) . . ?
C23 C22 Mn1 71.3(3) . . ?
C19 C23 C22 107.5(5) . . ?
C19 C23 Mn1 71.6(3) . . ?
C22 C23 Mn1 69.9(3) . . ?
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 O1 2.064(3) . ?
Sn1 O2 2.082(3) . ?
Sn1 N1 2.244(4) . ?
Sn1 N2 2.294(4) . ?
Sn1 Mn1 2.4428(7) . ?
O1 C1 1.331(5) . ?
C1 C2 1.400(7) . ?
C1 C6 1.413(7) . ?
C2 C3 1.382(8) . ?
C3 C4 1.376(9) . ?
C4 C5 1.371(8) . ?
C5 C6 1.410(7) . ?
C6 C7 1.428(7) . ?
C7 N1 1.284(6) . ?
N1 C8 1.484(6) . ?
C8 C9 1.522(7) . ?
C9 N2 1.466(6) . ?
N2 C10 1.285(6) . ?
C10 C11 1.450(7) . ?
C11 C16 1.407(7) . ?
C11 C12 1.408(6) . ?
C12 C13 1.376(8) . ?
C13 C14 1.398(8) . ?
C14 C15 1.370(7) . ?
C15 C16 1.396(7) . ?
C16 O2 1.354(5) . ?
Mn1 C17 1.766(5) . ?
Mn1 C18 1.773(5) . ?
Mn1 C21 2.117(4) . ?
Mn1 C22 2.118(4) . ?
Mn1 C23 2.137(6) . ?
Mn1 C20 2.139(5) . ?
Mn1 C19 2.150(5) . ?
C17 O3 1.167(7) . ?
C18 O4 1.162(6) . ?
C19 C23 1.389(9) . ?
C19 C20 1.391(9) . ?
C20 C21 1.424(8) . ?
C21 C22 1.393(7) . ?
C22 C23 1.413(8) . ?
