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#$Date: 2016-03-23 03:07:59 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179232 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/52/4315214.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_4315214
loop_
_publ_author_name
'Anukul Jana'
'Herbert W. Roesky'
'Carola Schulzke'
'Prinson P. Samuel'
_publ_section_title
;
 An Efficient Route for the Synthesis of a Tin(II) Substituted
 Carbodiimide from a Diazo Compound
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3461
_journal_page_last               3464
_journal_paper_doi               10.1021/ic100031d
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C37 H50 Fe N4 O4 Si Sn'
_chemical_formula_weight         817.44
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   23.764(5)
_cell_length_b                   16.231(3)
_cell_length_c                   10.373(2)
_cell_measurement_reflns_used    15052
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      51.7
_cell_measurement_theta_min      3.0
_cell_volume                     4001.0(14)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  IPDSII
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0225
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            14172
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    1.057
_exptl_absorpt_correction_T_max  0.9064
_exptl_absorpt_correction_T_min  0.6385
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'face indexed'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.357
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.11
_refine_diff_density_max         2.739
_refine_diff_density_min         -2.985
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     237
_refine_ls_number_reflns         3837
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.0421
_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)+(0.0566P)²+9.2823P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1049
_refine_ls_wR_factor_ref         0.1091
_reflns_number_gt                3288
_reflns_number_total             3837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic100031d_si_001_2.cif
_cod_data_source_block           ja65
_cod_original_cell_volume        4001.3(14)
_cod_database_code               4315214
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'-x-1/2, y-1/2, z-1/2'
'x, -y-1/2, 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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Sn1 Sn 0.582915(13) 0.2500 0.14085(3) 0.02217(12) Uani 1 2 d S . .
Fe1 Fe 0.47891(3) 0.2500 0.15746(7) 0.02555(18) Uani 1 2 d S . .
Si1 Si 0.76598(10) 0.2500 -0.1884(2) 0.0715(7) Uani 1 2 d SD . .
N1 N 0.6152(3) 0.2500 -0.0457(6) 0.0713(15) Uani 1 2 d S A .
N2 N 0.6971(3) 0.2500 -0.1689(6) 0.0713(15) Uani 1 2 d S A .
N3 N 0.63818(11) 0.15843(19) 0.2135(3) 0.0249(6) Uani 1 1 d . . .
O1 O 0.35657(18) 0.2500 0.1662(5) 0.0559(12) Uani 1 2 d S . .
O2 O 0.47352(12) 0.4055(2) 0.3017(3) 0.0415(7) Uani 1 1 d . . .
O3 O 0.47584(17) 0.2500 -0.1269(4) 0.0381(9) Uani 1 2 d S . .
C1 C 0.6567(3) 0.2500 -0.0998(7) 0.0713(15) Uani 1 2 d S . .
C2 C 0.4044(2) 0.2500 0.1616(6) 0.0375(13) Uani 1 2 d S . .
C3 C 0.47903(14) 0.3453(3) 0.2459(4) 0.0316(8) Uani 1 1 d . . .
C4 C 0.4789(2) 0.2500 -0.0160(5) 0.0309(11) Uani 1 2 d S . .
C5 C 0.61641(14) 0.0771(2) 0.2432(3) 0.0265(7) Uani 1 1 d . . .
C6 C 0.60623(15) 0.0210(2) 0.1433(3) 0.0297(8) Uani 1 1 d . . .
C7 C 0.58248(16) -0.0547(3) 0.1746(4) 0.0347(8) Uani 1 1 d . . .
H7 H 0.5749 -0.0934 0.1080 0.042 Uiso 1 1 calc R . .
C8 C 0.56977(17) -0.0747(3) 0.3000(4) 0.0374(9) Uani 1 1 d . . .
H8 H 0.5529 -0.1264 0.3193 0.045 Uiso 1 1 calc R . .
C9 C 0.58151(16) -0.0198(3) 0.3978(4) 0.0380(9) Uani 1 1 d . . .
H9 H 0.5733 -0.0347 0.4843 0.046 Uiso 1 1 calc R . .
C10 C 0.60503(16) 0.0570(3) 0.3726(3) 0.0330(8) Uani 1 1 d . . .
C11 C 0.62018(16) 0.0402(3) 0.0036(3) 0.0332(8) Uani 1 1 d . . .
H11 H 0.6417 0.0931 0.0013 0.040 Uiso 1 1 calc R . .
C12 C 0.56656(18) 0.0514(3) -0.0762(4) 0.0407(10) Uani 1 1 d . . .
H12A H 0.5442 0.0007 -0.0732 0.061 Uiso 1 1 calc R . .
H12B H 0.5767 0.0636 -0.1658 0.061 Uiso 1 1 calc R . .
H12C H 0.5445 0.0971 -0.0409 0.061 Uiso 1 1 calc R . .
C13 C 0.6569(2) -0.0269(3) -0.0566(4) 0.0484(11) Uani 1 1 d . . .
H13A H 0.6905 -0.0351 -0.0035 0.073 Uiso 1 1 calc R . .
H13B H 0.6681 -0.0100 -0.1436 0.073 Uiso 1 1 calc R . .
H13C H 0.6355 -0.0784 -0.0613 0.073 Uiso 1 1 calc R . .
C14 C 0.6181(2) 0.1144(3) 0.4838(4) 0.0457(11) Uani 1 1 d . . .
H14 H 0.6350 0.1661 0.4482 0.055 Uiso 1 1 calc R . .
C15 C 0.5648(2) 0.1372(3) 0.5578(4) 0.0525(12) Uani 1 1 d . . .
H15A H 0.5386 0.1657 0.4999 0.079 Uiso 1 1 calc R . .
H15B H 0.5745 0.1735 0.6299 0.079 Uiso 1 1 calc R . .
H15C H 0.5470 0.0870 0.5909 0.079 Uiso 1 1 calc R . .
C16 C 0.6606(2) 0.0750(5) 0.5768(5) 0.0702(17) Uani 1 1 d . . .
H16A H 0.6436 0.0266 0.6176 0.105 Uiso 1 1 calc R . .
H16B H 0.6711 0.1151 0.6434 0.105 Uiso 1 1 calc R . .
H16C H 0.6943 0.0583 0.5289 0.105 Uiso 1 1 calc R . .
C17 C 0.73253(16) 0.0995(3) 0.2344(4) 0.0398(10) Uani 1 1 d . . .
H17A H 0.7253 0.0736 0.3182 0.060 Uiso 1 1 calc R . .
H17B H 0.7717 0.1182 0.2307 0.060 Uiso 1 1 calc R . .
H17C H 0.7257 0.0595 0.1655 0.060 Uiso 1 1 calc R . .
C18 C 0.69382(14) 0.1723(2) 0.2173(3) 0.0279(8) Uani 1 1 d . . .
C19 C 0.7178(2) 0.2500 0.2081(5) 0.0323(12) Uani 1 2 d S . .
H19 H 0.7572 0.2500 0.1929 0.039 Uiso 1 2 calc SR . .
C20 C 0.7832(5) 0.2500 -0.3628(10) 0.116(5) Uani 1 2 d SD A .
H20A H 0.8242 0.2500 -0.3738 0.175 Uiso 1 2 calc SR . .
H20B H 0.7673 0.2993 -0.4033 0.175 Uiso 0.50 1 calc PR . .
H20C H 0.7673 0.2007 -0.4033 0.175 Uiso 0.50 1 calc PR . .
C21 C 0.7736(4) 0.1376(7) -0.1450(10) 0.069(4) Uani 0.50 1 d PD A 1
H21A H 0.7644 0.1298 -0.0537 0.103 Uiso 1 1 calc R A 1
H21B H 0.8125 0.1199 -0.1606 0.103 Uiso 1 1 calc R A 1
H21C H 0.7480 0.1046 -0.1981 0.103 Uiso 1 1 calc R A 1
C21A C 0.8174(4) 0.2020(8) -0.0724(9) 0.0713(15) Uani 0.50 1 d PD . 2
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'
Si Si 0.0817 0.0704 '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'
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
N1 Sn1 N3 95.87(15) . 8_565 ?
N1 Sn1 N3 95.87(15) . . ?
N3 Sn1 N3 88.93(16) 8_565 . ?
N1 Sn1 Fe1 115.59(18) . . ?
N3 Sn1 Fe1 126.36(8) 8_565 . ?
N3 Sn1 Fe1 126.36(8) . . ?
C2 Fe1 C3 89.38(15) . . ?
C2 Fe1 C3 89.38(15) . 8_565 ?
C3 Fe1 C3 118.7(2) . 8_565 ?
C2 Fe1 C4 91.4(2) . . ?
C3 Fe1 C4 120.67(12) . . ?
C3 Fe1 C4 120.67(12) 8_565 . ?
C2 Fe1 Sn1 177.4(2) . . ?
C3 Fe1 Sn1 91.94(11) . . ?
C3 Fe1 Sn1 91.94(11) 8_565 . ?
C4 Fe1 Sn1 85.98(16) . . ?
N2 Si1 C20 109.8(5) . . ?
N2 Si1 C21A 124.4(4) . . ?
C20 Si1 C21A 118.7(5) . . ?
N2 Si1 C21A 124.4(4) . 8_565 ?
C20 Si1 C21A 118.7(5) . 8_565 ?
C21A Si1 C21A 48.8(9) . 8_565 ?
N2 Si1 C21 93.8(3) . 8_565 ?
C20 Si1 C21 102.2(3) . 8_565 ?
C21A Si1 C21 100.6(6) . 8_565 ?
C21A Si1 C21 52.1(5) 8_565 8_565 ?
N2 Si1 C21 93.8(3) . . ?
C20 Si1 C21 102.2(3) . . ?
C21A Si1 C21 52.1(5) . . ?
C21A Si1 C21 100.6(6) 8_565 . ?
C21 Si1 C21 150.2(7) 8_565 . ?
C1 N1 Sn1 141.2(7) . . ?
C1 N2 Si1 150.3(7) . . ?
C18 N3 C5 119.9(3) . . ?
C18 N3 Sn1 120.2(2) . . ?
C5 N3 Sn1 119.5(2) . . ?
N1 C1 N2 172.9(10) . . ?
O1 C2 Fe1 179.0(6) . . ?
O2 C3 Fe1 173.3(3) . . ?
O3 C4 Fe1 176.3(4) . . ?
C6 C5 C10 121.4(4) . . ?
C6 C5 N3 119.7(3) . . ?
C10 C5 N3 118.8(3) . . ?
C7 C6 C5 118.1(3) . . ?
C7 C6 C11 119.5(3) . . ?
C5 C6 C11 122.4(3) . . ?
C8 C7 C6 121.3(4) . . ?
C7 C8 C9 119.9(4) . . ?
C8 C9 C10 121.5(4) . . ?
C9 C10 C5 117.7(4) . . ?
C9 C10 C14 119.4(3) . . ?
C5 C10 C14 122.9(4) . . ?
C6 C11 C13 111.7(3) . . ?
C6 C11 C12 111.0(3) . . ?
C13 C11 C12 109.8(3) . . ?
C10 C14 C15 111.2(4) . . ?
C10 C14 C16 110.9(4) . . ?
C15 C14 C16 109.3(4) . . ?
N3 C18 C19 123.7(3) . . ?
N3 C18 C17 118.2(3) . . ?
C19 C18 C17 118.0(3) . . ?
C18 C19 C18 130.8(5) 8_565 . ?
C21A C21A Si1 65.6(4) 8_565 . ?
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 N1 2.081(6) . ?
Sn1 N3 2.122(3) 8_565 ?
Sn1 N3 2.122(3) . ?
Sn1 Fe1 2.4777(9) . ?
Fe1 C2 1.770(6) . ?
Fe1 C3 1.799(4) . ?
Fe1 C3 1.799(4) 8_565 ?
Fe1 C4 1.799(6) . ?
Si1 N2 1.649(7) . ?
Si1 C20 1.855(9) . ?
Si1 C21A 1.883(9) . ?
Si1 C21A 1.883(9) 8_565 ?
Si1 C21 1.889(10) 8_565 ?
Si1 C21 1.889(10) . ?
N1 C1 1.136(9) . ?
N2 C1 1.198(9) . ?
N3 C18 1.342(4) . ?
N3 C5 1.451(5) . ?
O1 C2 1.139(7) . ?
O2 C3 1.144(5) . ?
O3 C4 1.153(7) . ?
C5 C6 1.401(5) . ?
C5 C10 1.408(5) . ?
C6 C7 1.391(6) . ?
C6 C11 1.518(5) . ?
C7 C8 1.374(6) . ?
C8 C9 1.379(6) . ?
C9 C10 1.390(6) . ?
C10 C14 1.516(6) . ?
C11 C13 1.528(5) . ?
C11 C12 1.531(5) . ?
C14 C15 1.527(7) . ?
C14 C16 1.536(7) . ?
C17 C18 1.508(5) . ?
C18 C19 1.387(4) . ?
C19 C18 1.387(4) 8_565 ?
C21A C21A 1.56(3) 8_565 ?
