#------------------------------------------------------------------------------
#$Date: 2016-03-23 01:31:04 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179144 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/05/4310562.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_4310562
loop_
_publ_author_name
'Peter B. Hitchcock'
'Alexander G. Hulkes'
'Michael F. Lappert'
_publ_section_title
;
 Oxidation in Nonclassical Organolanthanide Chemistry: Synthesis,
 Characterization, and X-ray Crystal Structures of Cerium(III) and -(IV)
 Amides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1031
_journal_page_last               1038
_journal_paper_doi               10.1021/ic035100v
_journal_volume                  43
_journal_year                    2004
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C32 H88 Ce2 Cl2 N4 O2 Si8'
_chemical_formula_structural     'C32 H88 Ce2 Cl2 N4 O2 Si8'
_chemical_formula_sum            'C32 H88 Ce2 Cl2 N4 O2 Si8'
_chemical_formula_weight         1136.92
_chemical_name_common            '[{CeCl(thf)(N(SiMe3)2)2}2]'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_conform_dict_location
ftp://ftp.iucr.org/cifdics/cif_core_2.1beta5.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_date             2000-05-16T08:28:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 113.789(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.506(3)
_cell_length_b                   13.065(3)
_cell_length_c                   16.779(3)
_cell_measurement_reflns_used    473206
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      3.705
_cell_measurement_wavelength     0.71073
_cell_volume                     2909.8(11)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_reduction
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.944
_diffrn_measured_fraction_theta_max 0.944
_diffrn_measurement_device       KappaCCD
_diffrn_measurement_method       CCD
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0898
_diffrn_reflns_av_sigmaI/netI    0.071
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15242
_diffrn_reflns_theta_full        25.04
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.89
_exptl_absorpt_coefficient_mu    1.828
_exptl_absorpt_correction_T_max  0.760
_exptl_absorpt_correction_T_min  0.489
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38]
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.215
_refine_diff_density_min         -1.021
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.824
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         4858
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.824
_refine_ls_R_factor_all          0.0876
_refine_ls_R_factor_gt           0.0543
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.2000P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1732
_refine_ls_wR_factor_ref         0.2199
_reflns_number_gt                3376
_reflns_number_total             4858
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035100vsi20030917_111540_2.cif
_cod_data_source_block           may1900
_cod_original_cell_volume        2909.8(10)
_cod_database_code               4310562
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce Ce 0.95428(3) 0.97961(4) 0.11462(3) 0.0623(3) Uani 1 1 d . . .
Cl Cl 1.06095(17) 1.11005(17) 0.04566(13) 0.0744(6) Uani 1 1 d . . .
Si1 Si 1.0385(2) 0.9426(2) 0.33955(16) 0.0761(6) Uani 1 1 d . . .
Si2 Si 1.2000(2) 0.9359(2) 0.26949(17) 0.0807(7) Uani 1 1 d . . .
Si3 Si 0.8694(2) 1.22199(19) 0.13242(18) 0.0784(7) Uani 1 1 d . . .
Si4 Si 0.70497(19) 1.0688(2) 0.04019(17) 0.0780(7) Uani 1 1 d . . .
N1 N 1.0765(5) 0.9499(5) 0.2552(4) 0.0713(17) Uani 1 1 d . . .
N2 N 0.8300(5) 1.1008(5) 0.0947(4) 0.0703(17) Uani 1 1 d . . .
C1 C 0.9008(9) 0.9820(9) 0.3013(8) 0.101(3) Uani 1 1 d . . .
H1A H 0.8593 0.9392 0.2518 0.152 Uiso 1 1 calc R . .
H1B H 0.8934 1.054 0.2833 0.152 Uiso 1 1 calc R . .
H1C H 0.8789 0.9732 0.349 0.152 Uiso 1 1 calc R . .
C2 C 1.1122(10) 1.0275(9) 0.4330(7) 0.106(4) Uani 1 1 d . . .
H2A H 1.1115 1.0976 0.4118 0.158 Uiso 1 1 calc R . .
H2B H 1.1818 1.003 0.4604 0.158 Uiso 1 1 calc R . .
H2C H 1.0819 1.0267 0.4756 0.158 Uiso 1 1 calc R . .
C3 C 1.0424(8) 0.8111(10) 0.3827(6) 0.106(4) Uani 1 1 d . . .
H3A H 1.0049 0.7646 0.3347 0.159 Uiso 1 1 calc R . .
H3B H 1.0117 0.811 0.4252 0.159 Uiso 1 1 calc R . .
H3C H 1.1125 0.7882 0.411 0.159 Uiso 1 1 calc R . .
C4 C 1.2756(9) 0.8527(11) 0.3630(7) 0.132(5) Uani 1 1 d . . .
H4A H 1.2747 0.8811 0.4168 0.198 Uiso 1 1 calc R . .
H4B H 1.3452 0.8494 0.368 0.198 Uiso 1 1 calc R . .
H4C H 1.2466 0.7837 0.3536 0.198 Uiso 1 1 calc R . .
C5 C 1.2054(9) 0.8748(8) 0.1702(7) 0.099(3) Uani 1 1 d . . .
H5A H 1.1655 0.9154 0.1186 0.149 Uiso 1 1 calc R . .
H5B H 1.1778 0.8053 0.1636 0.149 Uiso 1 1 calc R . .
H5C H 1.2755 0.8719 0.1765 0.149 Uiso 1 1 calc R . .
C6 C 1.2666(8) 1.0626(11) 0.2848(8) 0.120(4) Uani 1 1 d . . .
H6A H 1.2286 1.108 0.2361 0.18 Uiso 1 1 calc R . .
H6B H 1.3344 1.0521 0.2869 0.18 Uiso 1 1 calc R . .
H6C H 1.2714 1.0939 0.3395 0.18 Uiso 1 1 calc R . .
C7 C 1.0035(7) 1.2210(9) 0.2179(6) 0.093(3) Uani 1 1 d . . .
H7A H 1.0081 1.1752 0.2656 0.14 Uiso 1 1 calc R . .
H7B H 1.0229 1.2904 0.2406 0.14 Uiso 1 1 calc R . .
H7C H 1.049 1.1968 0.1917 0.14 Uiso 1 1 calc R . .
C8 C 0.7932(10) 1.2788(10) 0.1884(9) 0.121(4) Uani 1 1 d . . .
H8A H 0.7945 1.2329 0.2351 0.181 Uiso 1 1 calc R . .
H8B H 0.7235 1.288 0.1463 0.181 Uiso 1 1 calc R . .
H8C H 0.8217 1.3453 0.2133 0.181 Uiso 1 1 calc R . .
C9 C 0.8679(9) 1.3090(8) 0.0443(7) 0.107(3) Uani 1 1 d . . .
H9A H 0.9071 1.2785 0.0145 0.16 Uiso 1 1 calc R . .
H9B H 0.8976 1.375 0.0694 0.16 Uiso 1 1 calc R . .
H9C H 0.7982 1.3194 0.0024 0.16 Uiso 1 1 calc R . .
C10 C 0.6253(8) 1.1709(9) -0.0344(6) 0.097(3) Uani 1 1 d . . .
H10A H 0.6544 1.1906 -0.0757 0.146 Uiso 1 1 calc R . .
H10B H 0.6231 1.2308 0 0.146 Uiso 1 1 calc R . .
H10C H 0.5569 1.1448 -0.0664 0.146 Uiso 1 1 calc R . .
C11 C 0.6938(8) 0.9530(9) -0.0298(8) 0.106(3) Uani 1 1 d . . .
H11A H 0.7255 0.9673 -0.0703 0.159 Uiso 1 1 calc R . .
H11B H 0.6225 0.9366 -0.0628 0.159 Uiso 1 1 calc R . .
H11C H 0.7277 0.8948 0.0073 0.159 Uiso 1 1 calc R . .
C12 C 0.6438(10) 1.0362(10) 0.1170(9) 0.115(4) Uani 1 1 d . . .
H12A H 0.6825 0.9821 0.157 0.172 Uiso 1 1 calc R . .
H12B H 0.5748 1.0122 0.0835 0.172 Uiso 1 1 calc R . .
H12C H 0.6422 1.0972 0.1504 0.172 Uiso 1 1 calc R . .
C13 C 0.9693(10) 0.7162(11) 0.1320(9) 0.123(4) Uani 1 1 d . . .
H13A H 1.0354 0.7307 0.1799 0.147 Uiso 1 1 calc R . .
H13B H 0.9785 0.7108 0.0768 0.147 Uiso 1 1 calc R . .
C14 C 0.9261(17) 0.6205(10) 0.1493(13) 0.166(7) Uani 1 1 d . . .
H14A H 0.9255 0.5669 0.1074 0.2 Uiso 1 1 calc R . .
H14B H 0.9674 0.5958 0.2089 0.2 Uiso 1 1 calc R . .
C15 C 0.8258(14) 0.6412(13) 0.1403(10) 0.152(6) Uani 1 1 d . . .
H15A H 0.7764 0.6045 0.0893 0.183 Uiso 1 1 calc R . .
H15B H 0.8166 0.6192 0.1931 0.183 Uiso 1 1 calc R . .
C16 C 0.8129(11) 0.7465(12) 0.1290(11) 0.164(8) Uani 1 1 d . . .
H16A H 0.799 0.7755 0.1775 0.196 Uiso 1 1 calc R . .
H16B H 0.7537 0.7604 0.0741 0.196 Uiso 1 1 calc R . .
O O 0.8984(5) 0.7955(4) 0.1261(4) 0.0828(17) 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 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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'
Cl Cl 0.1484 0.1585 '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'
O O 0.0106 0.006 '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
N2 Ce N1 119.1(2) . . ?
N2 Ce O 113.5(2) . . ?
N1 Ce O 84.4(2) . . ?
N2 Ce Cl 92.93(18) . . ?
N1 Ce Cl 101.20(18) . . ?
O Ce Cl 146.23(15) . . ?
N2 Ce Cl 112.55(17) . 3_775 ?
N1 Ce Cl 128.27(18) . 3_775 ?
O Ce Cl 77.28(15) . 3_775 ?
Cl Ce Cl 73.20(7) . 3_775 ?
Ce Cl Ce 106.80(7) . 3_775 ?
N1 Si1 C3 113.8(4) . . ?
N1 Si1 C2 113.2(5) . . ?
C3 Si1 C2 107.8(5) . . ?
N1 Si1 C1 110.4(4) . . ?
C3 Si1 C1 104.2(5) . . ?
C2 Si1 C1 106.9(6) . . ?
N1 Si2 C4 114.0(5) . . ?
N1 Si2 C5 109.6(4) . . ?
C4 Si2 C5 106.2(5) . . ?
N1 Si2 C6 111.9(5) . . ?
C4 Si2 C6 107.7(7) . . ?
C5 Si2 C6 107.0(6) . . ?
N2 Si3 C9 112.1(4) . . ?
N2 Si3 C8 112.0(5) . . ?
C9 Si3 C8 109.7(6) . . ?
N2 Si3 C7 111.1(4) . . ?
C9 Si3 C7 106.6(5) . . ?
C8 Si3 C7 104.9(5) . . ?
N2 Si3 Ce 36.8(2) . . ?
N2 Si4 C10 114.5(4) . . ?
N2 Si4 C11 109.5(4) . . ?
C10 Si4 C11 106.3(5) . . ?
N2 Si4 C12 112.2(5) . . ?
C10 Si4 C12 106.5(5) . . ?
C11 Si4 C12 107.4(6) . . ?
Si1 N1 Si2 122.9(4) . . ?
Si1 N1 Ce 118.4(4) . . ?
Si2 N1 Ce 118.8(4) . . ?
Si3 N2 Si4 122.9(4) . . ?
Si3 N2 Ce 116.9(3) . . ?
Si4 N2 Ce 120.1(4) . . ?
O C13 C14 106.0(12) . . ?
C15 C14 C13 108.3(14) . . ?
C16 C15 C14 106.0(12) . . ?
C15 C16 O 112.4(13) . . ?
C16 O C13 106.5(9) . . ?
C16 O Ce 137.2(8) . . ?
C13 O Ce 116.3(6) . . ?
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
Ce N2 2.320(7) . ?
Ce N1 2.342(7) . ?
Ce O 2.570(6) . ?
Ce Cl 2.843(2) . ?
Ce Cl 2.859(2) 3_775 ?
Si1 N1 1.716(7) . ?
Si1 C3 1.856(12) . ?
Si1 C2 1.865(10) . ?
Si1 C1 1.905(12) . ?
Si2 N1 1.719(8) . ?
Si2 C4 1.859(11) . ?
Si2 C5 1.877(10) . ?
Si2 C6 1.882(12) . ?
Si3 N2 1.715(7) . ?
Si3 C9 1.859(11) . ?
Si3 C8 1.870(11) . ?
Si3 C7 1.895(10) . ?
Si4 N2 1.721(7) . ?
Si4 C10 1.875(10) . ?
Si4 C11 1.881(12) . ?
Si4 C12 1.885(12) . ?
C13 O 1.435(14) . ?
C13 C14 1.478(18) . ?
C14 C15 1.43(2) . ?
C15 C16 1.391(19) . ?
C16 O 1.414(13) . ?
