#------------------------------------------------------------------------------
#$Date: 2016-03-23 20:59:17 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179434 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/31/4333136.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided the Crystal Eye server at
# http://wwmm.ch.cam.ac.uk/crystaleye/, created by Nick Day at the
# Peter Murray-Rust laboratory.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_4333136
loop_
_publ_author_name
'Evans, William J.'
'Rego, Daniel B.'
'Ziller, Joseph W.'
_publ_section_title
;
 Synthesis, Structure, and15N NMR Studies of Paramagnetic Lanthanide
 Complexes Obtained by Reduction of Dinitrogen
;
_journal_issue                   26
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10790
_journal_page_last               10798
_journal_paper_doi               10.1021/ic061485g
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C27 H39 Ce'
_chemical_formula_weight         503.70
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            6
_cell_length_a                   15.7088(6)
_cell_length_b                   15.7088(6)
_cell_length_c                   16.4763(12)
_cell_measurement_temperature    163(2)
_cell_volume                     3521.1(3)
_computing_cell_refinement       'Bruker SMART/SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      163(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15131
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.94
_diffrn_standards_decay_%        '< 1.0'
_diffrn_standards_interval_count 'initial 50 frames recollected'
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    1.949
_exptl_absorpt_correction_T_max  0.8920
_exptl_absorpt_correction_T_min  0.6738
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            aquablue
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1554
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.605
_refine_diff_density_min         -0.271
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.121
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     138
_refine_ls_number_reflns         1941
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.121
_refine_ls_R_factor_all          0.0193
_refine_ls_R_factor_gt           0.0161
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0162P)²+5.4617P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0379
_refine_ls_wR_factor_ref         0.0395
_reflns_number_gt                1775
_reflns_number_total             1941
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061485gsup3.cif
_cod_data_source_block           dbr26
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Rhombohedral' changed to
'rhombohedral' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/a' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      R-3
_cod_database_code               4333136
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'x+2/3, y+1/3, z+1/3'
'-y+2/3, x-y+1/3, z+1/3'
'-x+y+2/3, -x+1/3, z+1/3'
'x+1/3, y+2/3, z+2/3'
'-y+1/3, x-y+2/3, z+2/3'
'-x+y+1/3, -x+2/3, z+2/3'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'-x+2/3, -y+1/3, -z+1/3'
'y+2/3, -x+y+1/3, -z+1/3'
'x-y+2/3, x+1/3, -z+1/3'
'-x+1/3, -y+2/3, -z+2/3'
'y+1/3, -x+y+2/3, -z+2/3'
'x-y+1/3, x+2/3, -z+2/3'
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
Ce1 Ce 0.0000 0.0000 0.751752(9) 0.01200(5) Uani 1 3 d S
C1 C 0.12547(14) -0.05702(14) 0.68099(11) 0.0163(3) Uani 1 1 d .
C2 C 0.04805(14) -0.14889(14) 0.70781(11) 0.0160(3) Uani 1 1 d .
C3 C 0.04824(14) -0.14883(14) 0.79408(11) 0.0166(4) Uani 1 1 d .
C4 C 0.12614(14) -0.05733(14) 0.82052(11) 0.0169(3) Uani 1 1 d .
C5 C 0.17402(13) -0.00185(16) 0.75098(12) 0.0162(3) Uani 1 1 d .
C6 C 0.15473(18) -0.02876(18) 0.59389(13) 0.0251(4) Uani 1 1 d .
C7 C -0.01290(17) -0.23624(16) 0.65474(13) 0.0223(4) Uani 1 1 d .
C8 C -0.01173(17) -0.23593(16) 0.84793(13) 0.0228(4) Uani 1 1 d .
C9 C 0.15657(18) -0.03051(18) 0.90762(12) 0.0255(4) Uani 1 1 d .
H5A H 0.2279(19) 0.0583(19) 0.7505(14) 0.027(6) Uiso 1 1 d .
H6A H 0.206(2) 0.032(2) 0.5880(17) 0.038(8) Uiso 1 1 d .
H6B H 0.176(3) -0.065(3) 0.571(2) 0.066(11) Uiso 1 1 d .
H6C H 0.111(3) -0.029(2) 0.5630(19) 0.057(9) Uiso 1 1 d .
H7A H -0.011(2) -0.220(2) 0.5998(18) 0.036(8) Uiso 1 1 d .
H7B H 0.011(3) -0.276(2) 0.660(2) 0.061(10) Uiso 1 1 d .
H7C H -0.076(2) -0.274(2) 0.6706(16) 0.034(7) Uiso 1 1 d .
H8A H 0.0215(19) -0.2703(19) 0.8571(15) 0.030(7) Uiso 1 1 d .
H8B H -0.072(2) -0.278(2) 0.8246(16) 0.035(7) Uiso 1 1 d .
H8C H -0.026(2) -0.219(2) 0.8981(18) 0.039(8) Uiso 1 1 d .
H9A H 0.209(2) 0.026(2) 0.9116(18) 0.044(9) Uiso 1 1 d .
H9B H 0.163(2) -0.078(2) 0.9349(17) 0.044(8) Uiso 1 1 d .
H9C H 0.111(2) -0.0260(19) 0.9368(16) 0.035(7) Uiso 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 0.0000 0.0000 '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
Cnt Ce1 Cnt 120.00 . .
C5 Ce1 C5 119.997(1) . 3
C5 Ce1 C5 119.998(1) . 2
C5 Ce1 C5 119.998(1) 3 2
C5 Ce1 C4 101.74(6) . 2
C5 Ce1 C4 132.32(6) 3 2
C5 Ce1 C4 29.42(6) 2 2
C5 Ce1 C4 29.42(6) . .
C5 Ce1 C4 101.74(6) 3 .
C5 Ce1 C4 132.31(6) 2 .
C4 Ce1 C4 104.67(4) 2 .
C5 Ce1 C4 132.31(6) . 3
C5 Ce1 C4 29.42(6) 3 3
C5 Ce1 C4 101.74(6) 2 3
C4 Ce1 C4 104.67(4) 2 3
C4 Ce1 C4 104.67(4) . 3
C5 Ce1 C1 101.45(6) . 2
C5 Ce1 C1 131.72(6) 3 2
C5 Ce1 C1 29.56(6) 2 2
C4 Ce1 C1 48.58(5) 2 2
C4 Ce1 C1 125.77(6) . 2
C4 Ce1 C1 125.77(6) 3 2
C5 Ce1 C1 29.56(6) . .
C5 Ce1 C1 101.45(6) 3 .
C5 Ce1 C1 131.72(6) 2 .
C4 Ce1 C1 125.77(6) 2 .
C4 Ce1 C1 48.58(5) . .
C4 Ce1 C1 125.77(6) 3 .
C1 Ce1 C1 103.83(4) 2 .
C5 Ce1 C1 131.72(6) . 3
C5 Ce1 C1 29.56(6) 3 3
C5 Ce1 C1 101.45(6) 2 3
C4 Ce1 C1 125.77(6) 2 3
C4 Ce1 C1 125.77(6) . 3
C4 Ce1 C1 48.58(5) 3 3
C1 Ce1 C1 103.83(4) 2 3
C1 Ce1 C1 103.83(4) . 3
C5 Ce1 C3 47.61(6) . .
C5 Ce1 C3 74.66(6) 3 .
C5 Ce1 C3 160.41(6) 2 .
C4 Ce1 C3 131.23(6) 2 .
C4 Ce1 C3 28.77(5) . .
C4 Ce1 C3 85.58(5) 3 .
C1 Ce1 C3 148.64(5) 2 .
C1 Ce1 C3 47.71(5) . .
C1 Ce1 C3 97.01(5) 3 .
C5 Ce1 C3 160.41(6) . 3
C5 Ce1 C3 47.61(6) 3 3
C5 Ce1 C3 74.66(6) 2 3
C4 Ce1 C3 85.58(5) 2 3
C4 Ce1 C3 131.23(6) . 3
C4 Ce1 C3 28.77(5) 3 3
C1 Ce1 C3 97.01(5) 2 3
C1 Ce1 C3 148.65(5) . 3
C1 Ce1 C3 47.71(5) 3 3
C3 Ce1 C3 114.34(3) . 3
C5 Ce1 C3 74.66(6) . 2
C5 Ce1 C3 160.41(6) 3 2
C5 Ce1 C3 47.61(6) 2 2
C4 Ce1 C3 28.77(5) 2 2
C4 Ce1 C3 85.58(5) . 2
C4 Ce1 C3 131.23(6) 3 2
C1 Ce1 C3 47.71(5) 2 2
C1 Ce1 C3 97.01(5) . 2
C1 Ce1 C3 148.64(5) 3 2
C3 Ce1 C3 114.34(3) . 2
C3 Ce1 C3 114.33(3) 3 2
C5 Ce1 C2 159.70(6) . 3
C5 Ce1 C2 47.60(6) 3 3
C5 Ce1 C2 74.51(6) 2 3
C4 Ce1 C2 97.01(5) 2 3
C4 Ce1 C2 149.06(5) . 3
C4 Ce1 C2 47.58(5) 3 3
C1 Ce1 C2 85.15(5) 2 3
C1 Ce1 C2 130.32(6) . 3
C1 Ce1 C2 28.79(5) 3 3
C3 Ce1 C2 122.08(5) . 3
C3 Ce1 C2 28.54(5) 3 3
C3 Ce1 C2 121.98(5) 2 3
C5 Ce1 C2 47.60(6) . .
C5 Ce1 C2 74.51(6) 3 .
C5 Ce1 C2 159.70(6) 2 .
C4 Ce1 C2 149.06(5) 2 .
C4 Ce1 C2 47.58(5) . .
C4 Ce1 C2 97.01(5) 3 .
C1 Ce1 C2 130.32(6) 2 .
C1 Ce1 C2 28.79(5) . .
C1 Ce1 C2 85.15(5) 3 .
C3 Ce1 C2 28.54(5) . .
C3 Ce1 C2 121.98(5) 3 .
C3 Ce1 C2 122.08(5) 2 .
C2 Ce1 C2 113.93(3) 3 .
C5 Ce1 C2 74.51(6) . 2
C5 Ce1 C2 159.70(6) 3 2
C5 Ce1 C2 47.60(6) 2 2
C4 Ce1 C2 47.58(5) 2 2
C4 Ce1 C2 97.01(5) . 2
C4 Ce1 C2 149.06(5) 3 2
C1 Ce1 C2 28.78(5) 2 2
C1 Ce1 C2 85.15(5) . 2
C1 Ce1 C2 130.32(6) 3 2
C3 Ce1 C2 121.98(5) . 2
C3 Ce1 C2 122.08(5) 3 2
C3 Ce1 C2 28.54(5) 2 2
C2 Ce1 C2 113.93(3) 3 2
C2 Ce1 C2 113.93(3) . 2
C5 C1 C2 107.18(16) . .
C5 C1 C6 127.23(19) . .
C2 C1 C6 125.37(17) . .
C5 C1 Ce1 73.40(10) . .
C2 C1 Ce1 79.19(11) . .
C6 C1 Ce1 117.63(13) . .
C1 C2 C3 108.13(16) . .
C1 C2 C7 125.52(16) . .
C3 C2 C7 125.71(17) . .
C1 C2 Ce1 72.02(10) . .
C3 C2 Ce1 75.52(11) . .
C7 C2 Ce1 125.56(13) . .
C4 C3 C2 108.04(16) . .
C4 C3 C8 125.06(17) . .
C2 C3 C8 126.13(18) . .
C4 C3 Ce1 72.20(11) . .
C2 C3 Ce1 75.94(11) . .
C8 C3 Ce1 125.62(13) . .
C5 C4 C3 107.57(16) . .
C5 C4 C9 127.31(19) . .
C3 C4 C9 124.85(17) . .
C5 C4 Ce1 73.50(10) . .
C3 C4 Ce1 79.03(11) . .
C9 C4 Ce1 118.28(13) . .
C4 C5 C1 109.06(17) . .
C4 C5 Ce1 77.08(10) . .
C1 C5 Ce1 77.04(10) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 Cnt 2.552 .
Ce1 C5 2.7483(17) .
Ce1 C5 2.7484(17) 3
Ce1 C5 2.7484(17) 2
Ce1 C4 2.7939(18) 2
Ce1 C4 2.7939(18) .
Ce1 C4 2.7939(18) 3
Ce1 C1 2.7948(18) 2
Ce1 C1 2.7949(18) .
Ce1 C1 2.7949(18) 3
Ce1 C3 2.8807(18) .
Ce1 C3 2.8807(19) 3
Ce1 C3 2.8807(19) 2
Ce1 C2 2.8861(18) 3
Ce1 C2 2.8861(18) .
Ce1 C2 2.8862(18) 2
C1 C5 1.415(3) .
C1 C2 1.415(3) .
C1 C6 1.505(3) .
C2 C3 1.421(2) .
C2 C7 1.500(3) .
C3 C4 1.412(3) .
C3 C8 1.503(3) .
C4 C5 1.408(3) .
C4 C9 1.505(3) .
