#------------------------------------------------------------------------------
#$Date: 2016-02-13 14:50:18 +0200 (Sat, 13 Feb 2016) $
#$Revision: 176428 $
#$URL: svn://www.crystallography.net/cod/cif/4/06/05/4060525.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_4060525
loop_
_publ_author_name
'Liddle, Stephen T.'
'Arnold, Polly L.'
_publ_section_title
;
Synthesis of Heteroleptic Cerium(III) Anionic Amido-Tethered N-Heterocyclic 
Carbene Complexes
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              2597
_journal_page_last               2605
_journal_paper_doi               10.1021/om050061b
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C59 H108 Ce2 I2 N8 Si4'
_chemical_formula_sum            'C59 H108 Ce2 I2 N8 Si4'
_chemical_formula_weight         1575.93
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           'enCIFer editing of SHELXL97 CIF output'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.499(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.287(4)
_cell_length_b                   21.230(4)
_cell_length_c                   14.748(2)
_cell_measurement_reflns_used    9550
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.39
_cell_volume                     7362(2)
_computing_cell_refinement       'Bruker SAINT version 6.36a (Bruker, 2000)'
_computing_data_collection       'Bruker SMART version 5.625 (Bruker, 2001)'
_computing_data_reduction        'Bruker SAINT; Bruker SHELXTL (Bruker, 2001)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material
'enCIFer(Allen et al.,2004);PLATON(Spek,2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART 1000 CCD diffractometer'
_diffrn_measurement_method       'ω rotation with narrow frames'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0357
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            27212
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.76
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.163
_exptl_absorpt_correction_T_max  0.5928
_exptl_absorpt_correction_T_min  0.4937
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.422
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.27
_refine_diff_density_max         2.313
_refine_diff_density_min         -2.321
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     244
_refine_ls_number_reflns         6486
_refine_ls_number_restraints     198
_refine_ls_restrained_S_all      1.146
_refine_ls_R_factor_all          0.0663
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0320P)²+199.9397P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1299
_refine_ls_wR_factor_ref         0.1330
_reflns_number_gt                5576
_reflns_number_total             6486
_reflns_threshold_expression     I>2σ(I)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4060525
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.246124(19) 0.19529(2) 0.14826(3) 0.02266(13) Uani 1 1 d U . .
I1 I 0.24660(2) 0.15904(2) -0.06599(4) 0.02925(16) Uani 1 1 d U . .
N1 N 0.3357(3) 0.2071(3) 0.2361(6) 0.0415(6) Uani 1 1 d U . .
N2 N 0.3269(3) 0.0565(3) 0.2282(5) 0.0355(6) Uani 1 1 d U . .
N3 N 0.2441(3) 0.0183(3) 0.1780(5) 0.0366(6) Uani 1 1 d U . .
C1 C 0.2730(4) 0.0728(4) 0.1824(6) 0.0343(6) Uani 1 1 d U . .
C2 C 0.3314(4) -0.0058(4) 0.2535(6) 0.0365(7) Uani 1 1 d U . .
H2A H 0.3647 -0.0274 0.2864 0.044 Uiso 1 1 calc R . .
C3 C 0.2788(4) -0.0301(4) 0.2222(6) 0.0370(7) Uani 1 1 d U . .
H3A H 0.2677 -0.0724 0.2292 0.044 Uiso 1 1 calc R . .
C4 C 0.1822(4) 0.0070(4) 0.1313(7) 0.0394(7) Uani 1 1 d U . .
C5 C 0.1796(4) -0.0367(4) 0.0489(7) 0.0410(8) Uani 1 1 d U . .
H5A H 0.1975 -0.0770 0.0716 0.061 Uiso 1 1 calc R . .
H5B H 0.1998 -0.0174 0.0061 0.061 Uiso 1 1 calc R . .
H5C H 0.1398 -0.0438 0.0156 0.061 Uiso 1 1 calc R . .
C6 C 0.1530(4) -0.0210(4) 0.2026(7) 0.0406(8) Uani 1 1 d U . .
H6A H 0.1563 0.0083 0.2549 0.061 Uiso 1 1 calc R . .
H6B H 0.1712 -0.0611 0.2260 0.061 Uiso 1 1 calc R . .
H6C H 0.1127 -0.0284 0.1725 0.061 Uiso 1 1 calc R . .
C7 C 0.1534(4) 0.0695(4) 0.0940(7) 0.0394(9) Uani 1 1 d U . .
H7A H 0.1544 0.0981 0.1465 0.059 Uiso 1 1 calc R . .
H7B H 0.1138 0.0615 0.0604 0.059 Uiso 1 1 calc R . .
H7C H 0.1737 0.0886 0.0512 0.059 Uiso 1 1 calc R . .
C8 C 0.3769(4) 0.0971(4) 0.2525(7) 0.0367(6) Uani 1 1 d U . .
H8A H 0.4093 0.0748 0.2375 0.044 Uiso 1 1 calc R . .
H8B H 0.3868 0.1047 0.3209 0.044 Uiso 1 1 calc R . .
C9 C 0.3691(4) 0.1608(4) 0.2019(7) 0.0376(6) Uani 1 1 d U . .
H9A H 0.4072 0.1789 0.2060 0.045 Uiso 1 1 calc R . .
H9B H 0.3511 0.1532 0.1348 0.045 Uiso 1 1 calc R . .
C10 C 0.3697(4) 0.2524(4) 0.3042(7) 0.0466(8) Uani 1 1 d U . .
C11 C 0.3257(4) 0.2917(4) 0.3364(7) 0.0475(9) Uani 1 1 d U . .
H11A H 0.3040 0.2645 0.3685 0.071 Uiso 1 1 calc R . .
H11B H 0.2998 0.3113 0.2819 0.071 Uiso 1 1 calc R . .
H11C H 0.3450 0.3245 0.3794 0.071 Uiso 1 1 calc R . .
C12 C 0.4054(4) 0.2953(4) 0.2560(7) 0.0480(9) Uani 1 1 d U . .
H12A H 0.4339 0.2698 0.2360 0.072 Uiso 1 1 calc R . .
H12B H 0.4246 0.3276 0.3003 0.072 Uiso 1 1 calc R . .
H12C H 0.3804 0.3156 0.2013 0.072 Uiso 1 1 calc R . .
C13 C 0.4094(4) 0.2210(4) 0.3899(7) 0.0483(9) Uani 1 1 d U . .
H13A H 0.3869 0.1946 0.4218 0.072 Uiso 1 1 calc R . .
H13B H 0.4292 0.2535 0.4330 0.072 Uiso 1 1 calc R . .
H13C H 0.4373 0.1947 0.3695 0.072 Uiso 1 1 calc R . .
N4 N 0.1669(4) 0.2160(5) 0.2082(6) 0.0628(9) Uani 1 1 d U . .
Si1 Si 0.17199(16) 0.19725(19) 0.3220(2) 0.0659(9) Uani 1 1 d U . .
C14 C 0.1125(7) 0.1508(9) 0.3429(12) 0.114(4) Uani 1 1 d U . .
H14A H 0.1029 0.1659 0.3999 0.171 Uiso 1 1 calc R . .
H14B H 0.1234 0.1063 0.3504 0.171 Uiso 1 1 calc R . .
H14C H 0.0793 0.1555 0.2895 0.171 Uiso 1 1 calc R . .
C15 C 0.1765(8) 0.2683(8) 0.3981(10) 0.114(4) Uani 1 1 d U . .
H15A H 0.1535 0.2616 0.4432 0.172 Uiso 1 1 calc R . .
H15B H 0.1621 0.3050 0.3592 0.172 Uiso 1 1 calc R . .
H15C H 0.2162 0.2755 0.4318 0.172 Uiso 1 1 calc R . .
C16 C 0.2344(6) 0.1447(7) 0.3689(8) 0.080(4) Uani 1 1 d U . .
H16A H 0.2336 0.1299 0.4315 0.120 Uiso 1 1 calc R . .
H16B H 0.2697 0.1682 0.3727 0.120 Uiso 1 1 calc R . .
H16C H 0.2327 0.1085 0.3271 0.120 Uiso 1 1 calc R . .
Si2 Si 0.10826(10) 0.25195(12) 0.13732(17) 0.0317(5) Uani 1 1 d U . .
C17 C 0.0381(5) 0.2192(8) 0.1449(9) 0.086(3) Uani 1 1 d U . .
H17A H 0.0343 0.2232 0.2093 0.129 Uiso 1 1 calc R . .
H17B H 0.0358 0.1747 0.1269 0.129 Uiso 1 1 calc R . .
H17C H 0.0074 0.2426 0.1025 0.129 Uiso 1 1 calc R . .
C18 C 0.1069(6) 0.3374(5) 0.1635(8) 0.059(3) Uani 1 1 d U . .
H18A H 0.1062 0.3432 0.2291 0.089 Uiso 1 1 calc R . .
H18B H 0.0728 0.3565 0.1228 0.089 Uiso 1 1 calc R . .
H18C H 0.1408 0.3576 0.1524 0.089 Uiso 1 1 calc R . .
C19 C 0.1102(4) 0.2416(5) 0.0119(6) 0.0399(19) Uani 1 1 d U . .
H19A H 0.1461 0.2583 0.0029 0.060 Uiso 1 1 calc R . .
H19B H 0.0783 0.2643 -0.0287 0.060 Uiso 1 1 calc R . .
H19C H 0.1074 0.1967 -0.0041 0.060 Uiso 1 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'
Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ce Ce -0.2486 2.6331 '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 Ce1 N4 121.8(3) . . ?
N1 Ce1 C1 81.2(3) . . ?
N4 Ce1 C1 107.0(3) . . ?
N1 Ce1 C9 27.8(3) . . ?
N4 Ce1 C9 143.7(3) . . ?
C1 Ce1 C9 62.3(3) . . ?
N1 Ce1 I1 110.3(2) . . ?
N4 Ce1 I1 127.7(2) . . ?
C1 Ce1 I1 83.9(2) . . ?
C9 Ce1 I1 87.28(19) . . ?
N1 Ce1 I1 88.53(19) . 7 ?
N4 Ce1 I1 94.9(2) . 7 ?
C1 Ce1 I1 158.0(2) . 7 ?
C9 Ce1 I1 100.54(17) . 7 ?
I1 Ce1 I1 81.547(18) . 7 ?
Ce1 I1 Ce1 98.453(18) . 7 ?
C9 N1 C10 114.2(8) . . ?
C9 N1 Ce1 105.7(5) . . ?
C10 N1 Ce1 139.2(6) . . ?
C1 N2 C2 112.4(7) . . ?
C1 N2 C8 127.6(7) . . ?
C2 N2 C8 120.0(7) . . ?
C1 N3 C3 111.5(7) . . ?
C1 N3 C4 127.3(7) . . ?
C3 N3 C4 121.2(7) . . ?
N3 C1 N2 103.3(7) . . ?
N3 C1 Ce1 136.2(6) . . ?
N2 C1 Ce1 119.7(6) . . ?
C3 C2 N2 105.8(8) . . ?
C2 C3 N3 106.9(8) . . ?
N3 C4 C5 107.4(8) . . ?
N3 C4 C6 109.2(7) . . ?
C5 C4 C6 112.3(8) . . ?
N3 C4 C7 109.8(7) . . ?
C5 C4 C7 108.4(8) . . ?
C6 C4 C7 109.6(8) . . ?
N2 C8 C9 114.1(7) . . ?
N1 C9 C8 116.3(8) . . ?
N1 C9 Ce1 46.5(4) . . ?
C8 C9 Ce1 109.8(6) . . ?
N1 C10 C11 104.5(8) . . ?
N1 C10 C13 113.9(7) . . ?
C11 C10 C13 109.0(9) . . ?
N1 C10 C12 110.6(8) . . ?
C11 C10 C12 109.8(8) . . ?
C13 C10 C12 108.9(8) . . ?
Si1 N4 Si2 123.3(5) . . ?
Si1 N4 Ce1 117.6(4) . . ?
Si2 N4 Ce1 119.0(4) . . ?
N4 Si1 C14 115.2(7) . . ?
N4 Si1 C15 112.5(7) . . ?
C14 Si1 C15 105.2(9) . . ?
N4 Si1 C16 110.9(5) . . ?
C14 Si1 C16 102.5(7) . . ?
C15 Si1 C16 109.8(7) . . ?
N4 Si2 C18 111.3(6) . . ?
N4 Si2 C17 115.3(6) . . ?
C18 Si2 C17 106.6(7) . . ?
N4 Si2 C19 109.0(4) . . ?
C18 Si2 C19 109.0(5) . . ?
C17 Si2 C19 105.3(5) . . ?
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
Ce1 N1 2.249(7) . ?
Ce1 N4 2.352(8) . ?
Ce1 C1 2.697(8) . ?
Ce1 C9 2.983(9) . ?
Ce1 I1 3.2551(8) . ?
Ce1 I1 3.3429(8) 7 ?
I1 Ce1 3.3429(8) 7 ?
N1 C9 1.445(12) . ?
N1 C10 1.483(11) . ?
N2 C1 1.361(11) . ?
N2 C2 1.371(11) . ?
N2 C8 1.459(11) . ?
N3 C1 1.346(11) . ?
N3 C3 1.384(11) . ?
N3 C4 1.508(11) . ?
C2 C3 1.347(13) . ?
C4 C5 1.518(13) . ?
C4 C6 1.528(14) . ?
C4 C7 1.536(12) . ?
C8 C9 1.534(11) . ?
C10 C11 1.523(15) . ?
C10 C13 1.537(12) . ?
C10 C12 1.548(15) . ?
N4 Si1 1.700(8) . ?
N4 Si2 1.719(9) . ?
Si1 C14 1.838(16) . ?
Si1 C15 1.866(16) . ?
Si1 C16 1.869(11) . ?
Si2 C18 1.857(11) . ?
Si2 C17 1.870(11) . ?
Si2 C19 1.876(9) . ?
