#------------------------------------------------------------------------------
#$Date: 2016-03-23 22:43:03 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179489 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/86/4338670.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_4338670
loop_
_publ_author_name
'Williams, Ursula J.'
'Carroll, Patrick J.'
'Schelter, Eric J.'
_publ_section_title
;
 Synthesis and Analysis of a Family of Cerium(IV) Halide and Pseudohalide
 Compounds.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6338
_journal_page_last               6345
_journal_paper_doi               10.1021/ic500969r
_journal_volume                  53
_journal_year                    2014
_chemical_formula_sum            'C36 H108 Ce2 N12 Si12'
_chemical_formula_weight         1326.66
_space_group_IT_number           146
_symmetry_cell_setting           rhombohedral
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   18.5150(10)
_cell_length_b                   18.5150(10)
_cell_length_c                   16.7999(9)
_cell_measurement_temperature    100(1)
_cell_volume                     4987.5(5)
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'CCD Area Detector'
_diffrn_measurement_device_type  'Bruker APEXII'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0177
_diffrn_reflns_av_sigmaI/netI    0.0113
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45090
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.76
_exptl_absorpt_coefficient_mu    1.602
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6820
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.325
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2076
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.185
_refine_diff_density_min         -0.839
_refine_diff_density_rms         0.249
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.257
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     203
_refine_ls_number_reflns         5029
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.257
_refine_ls_R_factor_all          0.0126
_refine_ls_R_factor_gt           0.0116
_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)+(0.0274P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0309
_refine_ls_wR_factor_ref         0.0398
_reflns_number_gt                5022
_reflns_number_total             5029
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic500969r_si_002.cif
_cod_data_source_block           compound_2-N3
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

 Adding full bibliography for 4338669--4338671.cif.
;
_cod_original_sg_symbol_H-M      'R 3     '
_cod_database_code               4338670
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'
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 0.6667 0.3333 0.859836(8) 0.01240(4) Uani 1 3 d S
Ce2 Ce 0.6667 0.3333 0.419544(8) 0.01380(5) Uani 1 3 d S
Si1 Si 0.84502(4) 0.33963(4) 0.93517(4) 0.01422(11) Uani 1 1 d .
Si2 Si 0.75568(4) 0.21838(4) 0.80171(4) 0.01447(14) Uani 1 1 d .
Si3 Si 0.85016(4) 0.50686(4) 0.45068(4) 0.01530(12) Uani 1 1 d .
Si4 Si 0.75037(4) 0.52394(4) 0.31604(4) 0.01418(13) Uani 1 1 d .
N1 N 0.76435(11) 0.29614(11) 0.86589(11) 0.0125(3) Uani 1 1 d .
N2 N 0.76082(11) 0.46265(11) 0.39026(11) 0.0147(3) Uani 1 1 d .
N3 N 0.6667 0.3333 0.7012(3) 0.0188(8) Uani 1 3 d S
N4 N 0.6667 0.3333 0.6334(3) 0.0207(6) Uani 1 3 d S
N5 N 0.6667 0.3333 0.5611(3) 0.0254(10) Uani 1 3 d S
N6 N 0.6667 0.3333 0.9938(2) 0.0207(6) Uani 1 3 d S
N7 N 0.6667 0.3333 1.06609(19) 0.0221(7) Uani 1 3 d S
N8 N 0.6667 0.3333 1.1335(5) 0.0422(10) Uani 1 3 d S
C1 C 0.94462(15) 0.35192(16) 0.89438(15) 0.0209(5) Uani 1 1 d .
H1a H 0.9370 0.2981 0.8813 0.031 Uiso 1 1 calc R
H1b H 0.9879 0.3781 0.9336 0.031 Uiso 1 1 calc R
H1c H 0.9601 0.3859 0.8474 0.031 Uiso 1 1 calc R
C2 C 0.81981(16) 0.27414(16) 1.02667(15) 0.0241(5) Uani 1 1 d .
H2a H 0.7773 0.2775 1.0564 0.036 Uiso 1 1 calc R
H2b H 0.8690 0.2940 1.0588 0.036 Uiso 1 1 calc R
H2c H 0.8002 0.2172 1.0118 0.036 Uiso 1 1 calc R
C3 C 0.86978(17) 0.44758(17) 0.96667(16) 0.0211(5) Uani 1 1 d .
H3a H 0.9032 0.4871 0.9265 0.032 Uiso 1 1 calc R
H3b H 0.8999 0.4618 1.0160 0.032 Uiso 1 1 calc R
H3c H 0.8188 0.4486 0.9735 0.032 Uiso 1 1 calc R
C4 C 0.77134(16) 0.13695(16) 0.85262(16) 0.0239(5) Uani 1 1 d .
H4a H 0.8261 0.1627 0.8757 0.036 Uiso 1 1 calc R
H4b H 0.7657 0.0958 0.8145 0.036 Uiso 1 1 calc R
H4c H 0.7303 0.1107 0.8937 0.036 Uiso 1 1 calc R
C5 C 0.83225(15) 0.26384(16) 0.71828(14) 0.0224(5) Uani 1 1 d .
H5a H 0.8229 0.3033 0.6897 0.034 Uiso 1 1 calc R
H5b H 0.8253 0.2201 0.6829 0.034 Uiso 1 1 calc R
H5c H 0.8879 0.2914 0.7394 0.034 Uiso 1 1 calc R
C6 C 0.64812(15) 0.15813(14) 0.75761(15) 0.0205(5) Uani 1 1 d .
H6a H 0.6076 0.1365 0.7996 0.031 Uiso 1 1 calc R
H6b H 0.6439 0.1128 0.7263 0.031 Uiso 1 1 calc R
H6c H 0.6380 0.1943 0.7244 0.031 Uiso 1 1 calc R
C7 C 0.94763(14) 0.58145(16) 0.39645(15) 0.0228(5) Uani 1 1 d .
H7a H 0.9531 0.5551 0.3495 0.034 Uiso 1 1 calc R
H7b H 0.9950 0.5975 0.4304 0.034 Uiso 1 1 calc R
H7c H 0.9448 0.6300 0.3816 0.034 Uiso 1 1 calc R
C8 C 0.86757(18) 0.42206(19) 0.49149(16) 0.0240(6) Uani 1 1 d .
H8a H 0.8161 0.3778 0.5123 0.036 Uiso 1 1 calc R
H8b H 0.9084 0.4444 0.5332 0.036 Uiso 1 1 calc R
H8c H 0.8871 0.4007 0.4497 0.036 Uiso 1 1 calc R
C9 C 0.83742(18) 0.56383(18) 0.53622(15) 0.0270(5) Uani 1 1 d .
H9a H 0.8268 0.6063 0.5165 0.041 Uiso 1 1 calc R
H9b H 0.8875 0.5891 0.5675 0.041 Uiso 1 1 calc R
H9c H 0.7914 0.5254 0.5686 0.041 Uiso 1 1 calc R
C10 C 0.82705(15) 0.55382(16) 0.23229(14) 0.0217(5) Uani 1 1 d .
H10a H 0.8827 0.5819 0.2533 0.033 Uiso 1 1 calc R
H10b H 0.8203 0.5903 0.1964 0.033 Uiso 1 1 calc R
H10c H 0.8174 0.5046 0.2043 0.033 Uiso 1 1 calc R
C11 C 0.64539(14) 0.46427(16) 0.26871(14) 0.0229(5) Uani 1 1 d .
H11a H 0.6390 0.4140 0.2456 0.034 Uiso 1 1 calc R
H11b H 0.6401 0.4977 0.2280 0.034 Uiso 1 1 calc R
H11c H 0.6030 0.4504 0.3083 0.034 Uiso 1 1 calc R
C12 C 0.76132(16) 0.62245(15) 0.35833(16) 0.0236(5) Uani 1 1 d .
H12a H 0.7222 0.6091 0.4010 0.035 Uiso 1 1 calc R
H12b H 0.7504 0.6520 0.3175 0.035 Uiso 1 1 calc R
H12c H 0.8170 0.6567 0.3782 0.035 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'
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
N1 Ce1 N1 119.795(8) . 3_665
N1 Ce1 N1 119.795(8) . 2_655
N1 Ce1 N1 119.795(8) 3_665 2_655
N1 Ce1 N6 87.39(5) . .
N1 Ce1 N6 87.39(5) 3_665 .
N1 Ce1 N6 87.39(5) 2_655 .
N1 Ce1 N3 92.61(5) . .
N1 Ce1 N3 92.61(5) 3_665 .
N1 Ce1 N3 92.61(5) 2_655 .
N6 Ce1 N3 180.000(2) . .
N1 Ce1 Si2 26.64(5) . .
N1 Ce1 Si2 101.56(5) 3_665 .
N1 Ce1 Si2 137.09(5) 2_655 .
N6 Ce1 Si2 106.583(12) . .
N3 Ce1 Si2 73.417(12) . .
N1 Ce1 Si2 101.56(5) . 2_655
N1 Ce1 Si2 137.09(5) 3_665 2_655
N1 Ce1 Si2 26.64(5) 2_655 2_655
N6 Ce1 Si2 106.583(12) . 2_655
N3 Ce1 Si2 73.417(12) . 2_655
Si2 Ce1 Si2 112.199(10) . 2_655
N1 Ce1 Si2 137.09(5) . 3_665
N1 Ce1 Si2 26.64(5) 3_665 3_665
N1 Ce1 Si2 101.56(5) 2_655 3_665
N6 Ce1 Si2 106.583(12) . 3_665
N3 Ce1 Si2 73.417(12) . 3_665
Si2 Ce1 Si2 112.199(10) . 3_665
Si2 Ce1 Si2 112.199(10) 2_655 3_665
N1 Ce1 Si1 25.14(5) . .
N1 Ce1 Si1 131.84(5) 3_665 .
N1 Ce1 Si1 100.87(5) 2_655 .
N6 Ce1 Si1 68.696(12) . .
N3 Ce1 Si1 111.304(12) . .
Si2 Ce1 Si1 51.767(15) . .
Si2 Ce1 Si1 90.609(16) 2_655 .
Si2 Ce1 Si1 156.823(16) 3_665 .
N1 Ce1 Si1 100.87(5) . 3_665
N1 Ce1 Si1 25.14(5) 3_665 3_665
N1 Ce1 Si1 131.84(5) 2_655 3_665
N6 Ce1 Si1 68.696(12) . 3_665
N3 Ce1 Si1 111.304(12) . 3_665
Si2 Ce1 Si1 90.609(16) . 3_665
Si2 Ce1 Si1 156.823(15) 2_655 3_665
Si2 Ce1 Si1 51.767(15) 3_665 3_665
Si1 Ce1 Si1 107.578(12) . 3_665
N1 Ce1 Si1 131.84(5) . 2_655
N1 Ce1 Si1 100.87(5) 3_665 2_655
N1 Ce1 Si1 25.14(5) 2_655 2_655
N6 Ce1 Si1 68.696(12) . 2_655
N3 Ce1 Si1 111.304(12) . 2_655
Si2 Ce1 Si1 156.823(16) . 2_655
Si2 Ce1 Si1 51.767(15) 2_655 2_655
Si2 Ce1 Si1 90.609(16) 3_665 2_655
Si1 Ce1 Si1 107.578(13) . 2_655
Si1 Ce1 Si1 107.578(12) 3_665 2_655
N2 Ce2 N2 115.15(4) 3_665 .
N2 Ce2 N2 115.15(4) 3_665 2_655
N2 Ce2 N2 115.15(4) . 2_655
N2 Ce2 N5 102.92(5) 3_665 .
N2 Ce2 N5 102.92(5) . .
N2 Ce2 N5 102.92(5) 2_655 .
N2 Ce2 Si3 28.29(5) 3_665 3_665
N2 Ce2 Si3 138.64(5) . 3_665
N2 Ce2 Si3 103.58(5) 2_655 3_665
N5 Ce2 Si3 81.016(11) . 3_665
N2 Ce2 Si3 103.58(5) 3_665 .
N2 Ce2 Si3 28.29(5) . .
N2 Ce2 Si3 138.64(5) 2_655 .
N5 Ce2 Si3 81.016(11) . .
Si3 Ce2 Si3 117.608(6) 3_665 .
N2 Ce2 Si3 138.64(5) 3_665 2_655
N2 Ce2 Si3 103.58(5) . 2_655
N2 Ce2 Si3 28.29(5) 2_655 2_655
N5 Ce2 Si3 81.016(11) . 2_655
Si3 Ce2 Si3 117.608(6) 3_665 2_655
Si3 Ce2 Si3 117.608(6) . 2_655
N1 Si1 C2 111.84(10) . .
N1 Si1 C1 112.14(10) . .
C2 Si1 C1 106.95(12) . .
N1 Si1 C3 112.01(10) . .
C2 Si1 C3 107.83(12) . .
C1 Si1 C3 105.71(12) . .
N1 Si1 Ce1 33.07(6) . .
C2 Si1 Ce1 110.64(8) . .
C1 Si1 Ce1 136.97(8) . .
C3 Si1 Ce1 82.05(8) . .
N1 Si2 C5 110.90(11) . .
N1 Si2 C4 113.24(10) . .
C5 Si2 C4 108.44(12) . .
N1 Si2 C6 111.53(11) . .
C5 Si2 C6 108.16(12) . .
C4 Si2 C6 104.24(11) . .
N1 Si2 Ce1 35.18(6) . .
C5 Si2 Ce1 115.27(9) . .
C4 Si2 Ce1 133.26(9) . .
C6 Si2 Ce1 77.58(8) . .
N2 Si3 C9 110.66(11) . .
N2 Si3 C7 113.50(10) . .
C9 Si3 C7 107.79(12) . .
N2 Si3 C8 109.63(11) . .
C9 Si3 C8 108.28(13) . .
C7 Si3 C8 106.78(13) . .
N2 Si3 Ce2 36.42(6) . .
C9 Si3 Ce2 107.95(9) . .
C7 Si3 Ce2 140.63(8) . .
C8 Si3 Ce2 76.79(9) . .
N2 Si4 C11 109.74(10) . .
N2 Si4 C12 111.47(10) . .
C11 Si4 C12 108.18(11) . .
N2 Si4 C10 114.24(10) . .
C11 Si4 C10 105.41(11) . .
C12 Si4 C10 107.47(12) . .
Si2 N1 Si1 119.97(11) . .
Si2 N1 Ce1 118.18(10) . .
Si1 N1 Ce1 121.80(9) . .
Si3 N2 Si4 119.38(11) . .
Si3 N2 Ce2 115.29(10) . .
Si4 N2 Ce2 125.26(10) . .
N4 N3 Ce1 180.000(1) . .
N3 N4 N5 180.000(3) . .
N4 N5 Ce2 180.000(1) . .
N7 N6 Ce1 180.000(1) . .
N8 N7 N6 180.000(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 N1 2.2362(18) .
Ce1 N1 2.2362(19) 3_665
Ce1 N1 2.2362(18) 2_655
Ce1 N6 2.250(4) .
Ce1 N3 2.665(4) .
Ce1 Si2 3.4215(7) .
Ce1 Si2 3.4215(7) 2_655
Ce1 Si2 3.4215(7) 3_665
Ce1 Si1 3.4835(6) .
Ce1 Si1 3.4835(6) 3_665
Ce1 Si1 3.4835(6) 2_655
Ce2 N2 2.2000(18) 3_665
Ce2 N2 2.2000(18) .
Ce2 N2 2.2000(18) 2_655
Ce2 N5 2.379(4) .
Ce2 Si3 3.3500(6) 3_665
Ce2 Si3 3.3500(6) .
Ce2 Si3 3.3500(6) 2_655
Si1 N1 1.7411(19) .
Si1 C2 1.867(3) .
Si1 C1 1.872(3) .
Si1 C3 1.889(3) .
Si2 N1 1.7407(19) .
Si2 C5 1.868(2) .
Si2 C4 1.878(3) .
Si2 C6 1.881(2) .
Si3 N2 1.756(2) .
Si3 C9 1.866(3) .
Si3 C7 1.871(2) .
Si3 C8 1.883(3) .
Si4 N2 1.761(2) .
Si4 C11 1.866(2) .
Si4 C12 1.871(3) .
Si4 C10 1.875(2) .
N3 N4 1.139(8) .
N4 N5 1.214(7) .
N6 N7 1.215(5) .
N7 N8 1.132(9) .
