#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:08:49 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178618 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/29/4072914.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_4072914
loop_
_publ_author_name
'Maynadié, Jérôme'
'Berthet, Jean-Claude'
'Thuéry, Pierre'
'Ephritikhine, Michel'
_publ_section_title
;
 Cyanide Metallocenes of Trivalent f-Elements
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2623
_journal_page_last               2629
_journal_paper_doi               10.1021/om061131x
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C55 H102 Ce N5'
_chemical_formula_weight         973.54
_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           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 120.9867(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.8298(4)
_cell_length_b                   14.7017(3)
_cell_length_c                   20.2229(4)
_cell_measurement_reflns_used    88329
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.68
_cell_measurement_theta_min      2.45
_cell_volume                     5564.0(2)
_computing_cell_refinement       'HKL2000 (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Hooft, 1998)'
_computing_data_reduction        'HKL2000 (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 1999)'
_computing_publication_material
'SHELXTL (Sheldrick, 1999); PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type
'Nonius Kappa-CCD area-detector diffractometer'
_diffrn_measurement_method       'two φ and four ω scans with 2° steps'
_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  0.0198
_diffrn_reflns_av_sigmaI/netI    0.0135
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            88329
_diffrn_reflns_theta_full        25.68
_diffrn_reflns_theta_max         25.68
_diffrn_reflns_theta_min         2.45
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_exptl_absorpt_coefficient_mu    0.855
_exptl_absorpt_correction_T_max  0.865
_exptl_absorpt_correction_T_min  0.554
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   'program DELABS from PLATON (Spek, 2003)'
_exptl_crystal_colour            'translucent dark yellow'
_exptl_crystal_density_diffrn    1.162
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             2100
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         5268
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0183
_refine_ls_R_factor_gt           0.0175
_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)+(0.0243P)²+5.8832P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0469
_refine_ls_wR_factor_ref         0.0473
_reflns_number_gt                5118
_reflns_number_total             5268
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om061131xsi20070308_094205.cif
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4072914
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
Ce Ce 0.5000 0.332913(7) 0.7500 0.01465(4) Uani 1 2 d S
N1 N 0.5000 0.59325(13) 0.7500 0.0276(4) Uani 1 2 d S
N2 N 0.31715(7) 0.40112(11) 0.71658(8) 0.0330(3) Uani 1 1 d .
N3 N 0.35030(6) 0.68258(8) 0.82359(7) 0.0180(2) Uani 1 1 d .
C1 C 0.5000 0.51478(15) 0.7500 0.0228(4) Uani 1 2 d S
C2 C 0.37188(8) 0.38013(10) 0.72468(8) 0.0202(3) Uani 1 1 d .
C3 C 0.47073(8) 0.19772(10) 0.63633(8) 0.0203(3) Uani 1 1 d .
C4 C 0.40476(7) 0.24338(10) 0.61067(8) 0.0193(3) Uani 1 1 d .
C5 C 0.41120(8) 0.33293(9) 0.58872(8) 0.0184(3) Uani 1 1 d .
C6 C 0.48100(8) 0.34280(10) 0.60129(8) 0.0185(3) Uani 1 1 d .
C7 C 0.51748(7) 0.25881(10) 0.62997(8) 0.0194(3) Uani 1 1 d .
C8 C 0.48526(9) 0.09810(10) 0.65572(9) 0.0273(3) Uani 1 1 d .
H8A H 0.4780 0.0653 0.6112 0.041 Uiso 1 1 calc R
H8B H 0.4533 0.0753 0.6712 0.041 Uiso 1 1 calc R
H8C H 0.5337 0.0903 0.6971 0.041 Uiso 1 1 calc R
C9 C 0.33891(8) 0.20116(11) 0.60381(9) 0.0274(3) Uani 1 1 d .
H9A H 0.3045 0.2478 0.5940 0.041 Uiso 1 1 calc R
H9B H 0.3514 0.1704 0.6510 0.041 Uiso 1 1 calc R
H9C H 0.3188 0.1583 0.5620 0.041 Uiso 1 1 calc R
C10 C 0.35387(8) 0.40477(11) 0.55468(9) 0.0248(3) Uani 1 1 d .
H10A H 0.3749 0.4634 0.5738 0.037 Uiso 1 1 calc R
H10B H 0.3190 0.3927 0.5691 0.037 Uiso 1 1 calc R
H10C H 0.3311 0.4040 0.4995 0.037 Uiso 1 1 calc R
C11 C 0.51056(8) 0.42884(10) 0.58783(9) 0.0237(3) Uani 1 1 d .
H11A H 0.4749 0.4565 0.5404 0.036 Uiso 1 1 calc R
H11B H 0.5520 0.4146 0.5848 0.036 Uiso 1 1 calc R
H11C H 0.5236 0.4703 0.6297 0.036 Uiso 1 1 calc R
C12 C 0.58955(8) 0.23341(11) 0.64227(9) 0.0265(3) Uani 1 1 d .
H12A H 0.6153 0.1978 0.6885 0.040 Uiso 1 1 calc R
H12B H 0.6160 0.2877 0.6472 0.040 Uiso 1 1 calc R
H12C H 0.5832 0.1986 0.5990 0.040 Uiso 1 1 calc R
C13 C 0.33951(8) 0.74863(10) 0.87483(8) 0.0203(3) Uani 1 1 d .
H13A H 0.2899 0.7459 0.8609 0.024 Uiso 1 1 calc R
H13B H 0.3684 0.7284 0.9279 0.024 Uiso 1 1 calc R
C14 C 0.35822(8) 0.84722(10) 0.87030(9) 0.0225(3) Uani 1 1 d .
H14A H 0.3221 0.8735 0.8216 0.027 Uiso 1 1 calc R
H14B H 0.4038 0.8500 0.8728 0.027 Uiso 1 1 calc R
C15 C 0.36242(9) 0.90123(11) 0.93673(9) 0.0269(3) Uani 1 1 d .
H15A H 0.3963 0.8724 0.9852 0.032 Uiso 1 1 calc R
H15B H 0.3160 0.9010 0.9323 0.032 Uiso 1 1 calc R
C16 C 0.38541(9) 0.99908(11) 0.93684(10) 0.0327(4) Uani 1 1 d .
H16A H 0.4312 0.9995 0.9409 0.049 Uiso 1 1 calc R
H16B H 0.3886 1.0310 0.9799 0.049 Uiso 1 1 calc R
H16C H 0.3509 1.0284 0.8898 0.049 Uiso 1 1 calc R
C17 C 0.29879(7) 0.70681(10) 0.73966(8) 0.0200(3) Uani 1 1 d .
H17A H 0.3085 0.7686 0.7309 0.024 Uiso 1 1 calc R
H17B H 0.2505 0.7054 0.7303 0.024 Uiso 1 1 calc R
C18 C 0.30228(8) 0.64465(11) 0.68136(8) 0.0223(3) Uani 1 1 d .
H18A H 0.2914 0.5827 0.6885 0.027 Uiso 1 1 calc R
H18B H 0.3502 0.6456 0.6898 0.027 Uiso 1 1 calc R
C19 C 0.24906(8) 0.67566(10) 0.59915(9) 0.0224(3) Uani 1 1 d .
H19A H 0.2011 0.6742 0.5907 0.027 Uiso 1 1 calc R
H19B H 0.2596 0.7379 0.5923 0.027 Uiso 1 1 calc R
C20 C 0.25265(8) 0.61454(11) 0.54022(9) 0.0278(3) Uani 1 1 d .
H20A H 0.2993 0.6187 0.5467 0.042 Uiso 1 1 calc R
H20B H 0.2174 0.6337 0.4891 0.042 Uiso 1 1 calc R
H20C H 0.2435 0.5527 0.5478 0.042 Uiso 1 1 calc R
C21 C 0.42623(7) 0.68874(11) 0.83852(8) 0.0205(3) Uani 1 1 d .
H21A H 0.4338 0.6382 0.8127 0.025 Uiso 1 1 calc R
H21B H 0.4304 0.7444 0.8153 0.025 Uiso 1 1 calc R
C22 C 0.48531(8) 0.68763(12) 0.92313(9) 0.0251(3) Uani 1 1 d .
H22A H 0.4801 0.6343 0.9481 0.030 Uiso 1 1 calc R
H22B H 0.4814 0.7412 0.9488 0.030 Uiso 1 1 calc R
C23 C 0.55880(8) 0.68612(12) 0.93053(10) 0.0291(3) Uani 1 1 d .
H23A H 0.5954 0.6830 0.9848 0.035 Uiso 1 1 calc R
H23B H 0.5625 0.6314 0.9060 0.035 Uiso 1 1 calc R
C24 C 0.57342(10) 0.76791(13) 0.89501(12) 0.0405(4) Uani 1 1 d .
H24A H 0.5426 0.7660 0.8400 0.061 Uiso 1 1 calc R
H24B H 0.6224 0.7668 0.9080 0.061 Uiso 1 1 calc R
H24C H 0.5645 0.8227 0.9146 0.061 Uiso 1 1 calc R
C25 C 0.33784(8) 0.58558(10) 0.84089(8) 0.0201(3) Uani 1 1 d .
H25A H 0.3508 0.5439 0.8129 0.024 Uiso 1 1 calc R
H25B H 0.3696 0.5740 0.8955 0.024 Uiso 1 1 calc R
C26 C 0.26184(8) 0.56464(10) 0.82027(9) 0.0234(3) Uani 1 1 d .
H26A H 0.2300 0.5701 0.7649 0.028 Uiso 1 1 calc R
H26B H 0.2469 0.6085 0.8450 0.028 Uiso 1 1 calc R
C27 C 0.25635(8) 0.46881(10) 0.84592(9) 0.0233(3) Uani 1 1 d .
H27A H 0.2697 0.4248 0.8198 0.028 Uiso 1 1 calc R
H27B H 0.2895 0.4628 0.9010 0.028 Uiso 1 1 calc R
C28 C 0.18080(9) 0.44858(11) 0.82794(10) 0.0282(3) Uani 1 1 d .
H28A H 0.1685 0.4900 0.8560 0.042 Uiso 1 1 calc R
H28B H 0.1785 0.3873 0.8429 0.042 Uiso 1 1 calc R
H28C H 0.1478 0.4557 0.7736 0.042 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'
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
C2 Ce C2 149.78(6) 2_656
C2 Ce C1 74.89(3) 2_656
C2 Ce C1 74.89(3) .
C17 N3 C13 109.00(11) .
C17 N3 C25 111.02(11) .
C13 N3 C25 109.34(11) .
C17 N3 C21 108.11(11) .
C13 N3 C21 111.08(11) .
C25 N3 C21 108.28(11) .
N1 C1 Ce 180.000(1) .
N2 C2 Ce 177.46(12) .
C7 C3 C4 108.03(13) .
C7 C3 C8 125.16(13) .
C4 C3 C8 126.25(14) .
C5 C4 C3 107.88(12) .
C5 C4 C9 126.68(13) .
C3 C4 C9 125.34(14) .
C6 C5 C4 108.02(12) .
C6 C5 C10 125.02(13) .
C4 C5 C10 126.91(13) .
C5 C6 C7 108.00(12) .
C5 C6 C11 125.05(13) .
C7 C6 C11 126.94(13) .
C3 C7 C6 108.06(12) .
C3 C7 C12 124.62(14) .
C6 C7 C12 126.90(13) .
C14 C13 N3 115.19(12) .
C13 C14 C15 109.87(12) .
C14 C15 C16 111.35(13) .
N3 C17 C18 114.87(11) .
C17 C18 C19 110.49(12) .
C20 C19 C18 110.99(12) .
C22 C21 N3 115.26(12) .
C21 C22 C23 110.38(13) .
C24 C23 C22 114.02(14) .
C26 C25 N3 115.14(11) .
C25 C26 C27 111.05(12) .
C28 C27 C26 111.31(13) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce C2 2.6630(14) 2_656
Ce C2 2.6630(14) .
Ce C1 2.674(2) .
Ce C5 2.8080(14) 2_656
Ce C5 2.8080(14) .
Ce C6 2.8202(14) 2_656
Ce C6 2.8202(14) .
Ce C4 2.8217(14) .
Ce C4 2.8217(14) 2_656
Ce C3 2.8514(14) .
Ce C3 2.8514(14) 2_656
Ce C7 2.8598(14) .
Ce C7 2.8598(14) 2_656
N1 C1 1.154(3) .
N2 C2 1.161(2) .
N3 C17 1.5189(18) .
N3 C13 1.5244(18) .
N3 C25 1.5257(18) .
N3 C21 1.5268(18) .
C3 C7 1.414(2) .
C3 C4 1.423(2) .
C3 C8 1.507(2) .
C4 C5 1.419(2) .
C4 C9 1.505(2) .
C5 C6 1.417(2) .
C5 C10 1.506(2) .
C6 C7 1.421(2) .
C6 C11 1.507(2) .
C7 C12 1.508(2) .
C13 C14 1.521(2) .
C14 C15 1.522(2) .
C15 C16 1.523(2) .
C17 C18 1.524(2) .
C18 C19 1.527(2) .
C19 C20 1.526(2) .
C21 C22 1.523(2) .
C22 C23 1.533(2) .
C23 C24 1.517(3) .
C25 C26 1.520(2) .
C26 C27 1.527(2) .
C27 C28 1.524(2) .
