#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:49:05 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179457 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/54/4335498.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_4335498
loop_
_publ_author_name
'Haolin Yin'
'Andrew J. Lewis'
'Patrick Carroll'
'Eric J. Schelter'
_publ_section_title
;
 Electrophilic Ln(III) Cations Protected by C-F → Ln
 Interactions and Their Coordination Chemistry with Weak σ- and π-Donors
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8234
_journal_page_last               8243
_journal_paper_doi               10.1021/ic401130e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C44 H20 Ce F30 N3 O2'
_chemical_formula_weight         1332.75
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_Int_Tables_number      88
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   20.0824(9)
_cell_length_b                   20.0824(9)
_cell_length_c                   22.9594(12)
_cell_measurement_temperature    143(1)
_cell_volume                     9259.6(8)
_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      143(1)
_diffrn_measured_fraction_theta_full 0.966
_diffrn_measured_fraction_theta_max 0.966
_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  0.0604
_diffrn_reflns_av_sigmaI/netI    0.0702
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            15842
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.35
_exptl_absorpt_coefficient_mu    1.148
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 2007)'
_exptl_crystal_density_diffrn    1.912
_exptl_crystal_F_000             5192
_exptl_crystal_size_max          0.68
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.002
_refine_diff_density_min         -0.493
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         5136
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.015
_refine_ls_R_factor_all          0.0581
_refine_ls_R_factor_gt           0.0299
_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)+(0.0372P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0633
_refine_ls_wR_factor_ref         0.0675
_reflns_number_gt                3807
_reflns_number_total             5136
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic401130e_si_002_3.cif
_cod_data_source_block           UP4327(1-Ce(Et2O)2)
_cod_original_sg_symbol_H-M      'I 41/a '
_cod_database_code               4335498
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y+3/4, x+1/4, z+1/4'
'-x+1/2, -y, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-y+5/4, x+3/4, z+3/4'
'-x+1, -y+1/2, z+1'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'y-3/4, -x-1/4, -z-1/4'
'x-1/2, y, -z-1/2'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'y-1/4, -x+1/4, -z+1/4'
'x, y+1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
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 0.7500 0.101284(8) 0.01995(6) Uani 1 2 d S
F1 F 0.17703(8) 0.77670(7) 0.16787(7) 0.0368(4) Uani 1 1 d .
F2 F 0.21213(9) 0.82015(9) 0.27426(8) 0.0528(5) Uani 1 1 d .
F3 F 0.15646(11) 0.93294(12) 0.31833(9) 0.0725(7) Uani 1 1 d .
F4 F 0.06570(10) 1.00200(10) 0.25387(11) 0.0807(8) Uani 1 1 d .
F5 F 0.03662(8) 0.96295(8) 0.14487(10) 0.0586(6) Uani 1 1 d .
F6 F 0.18097(8) 0.95324(8) 0.09300(9) 0.0486(5) Uani 1 1 d .
F7 F 0.21530(9) 1.00375(8) -0.00901(10) 0.0605(5) Uani 1 1 d .
F8 F 0.16068(11) 0.95887(10) -0.11073(9) 0.0670(6) Uani 1 1 d .
F9 F 0.07138(11) 0.85522(10) -0.10600(8) 0.0580(5) Uani 1 1 d .
F10 F 0.03916(7) 0.80018(7) -0.00307(7) 0.0327(3) Uani 1 1 d .
F11 F -0.05827(7) 0.71016(7) 0.32071(6) 0.0309(3) Uani 1 1 d .
F12 F -0.15740(7) 0.78025(8) 0.36805(7) 0.0368(4) Uani 1 1 d .
F13 F -0.20538(7) 0.89261(8) 0.31491(7) 0.0405(4) Uani 1 1 d .
F14 F -0.15096(8) 0.93163(8) 0.21149(7) 0.0424(4) Uani 1 1 d .
F15 F -0.05150(7) 0.85998(7) 0.16286(6) 0.0300(3) Uani 1 1 d .
O1 O 0.08968(8) 0.67959(8) 0.05522(8) 0.0283(4) Uani 1 1 d .
N1 N 0.08444(10) 0.84216(9) 0.09899(10) 0.0265(5) Uani 1 1 d .
N2 N 0.0000 0.7500 0.20850(12) 0.0196(5) Uani 1 2 d S
C1 C 0.10451(12) 0.86716(12) 0.15372(13) 0.0282(6) Uani 1 1 d .
C2 C 0.14932(12) 0.83307(12) 0.18837(12) 0.0292(6) Uani 1 1 d .
C3 C 0.16758(14) 0.85433(14) 0.24290(13) 0.0370(7) Uani 1 1 d .
C4 C 0.13938(16) 0.91184(16) 0.26527(14) 0.0482(9) Uani 1 1 d .
C5 C 0.09423(15) 0.94668(15) 0.23226(17) 0.0524(9) Uani 1 1 d .
C6 C 0.07850(13) 0.92551(13) 0.17746(14) 0.0398(7) Uani 1 1 d .
C7 C 0.10628(11) 0.87438(11) 0.04950(13) 0.0275(6) Uani 1 1 d .
C8 C 0.15223(13) 0.92736(12) 0.04505(14) 0.0367(7) Uani 1 1 d .
C9 C 0.17028(14) 0.95396(13) -0.00803(16) 0.0445(8) Uani 1 1 d .
C10 C 0.14419(16) 0.93147(14) -0.05933(16) 0.0469(8) Uani 1 1 d .
C11 C 0.09905(15) 0.87938(14) -0.05721(14) 0.0412(7) Uani 1 1 d .
C12 C 0.08292(13) 0.85286(12) -0.00380(13) 0.0321(6) Uani 1 1 d .
C13 C -0.04874(11) 0.78441(11) 0.24074(11) 0.0232(5) Uani 1 1 d .
C14 C -0.07815(11) 0.76644(11) 0.29344(11) 0.0244(5) Uani 1 1 d .
C15 C -0.12981(12) 0.80202(13) 0.31846(11) 0.0280(6) Uani 1 1 d .
C16 C -0.15469(12) 0.85820(13) 0.29171(12) 0.0301(6) Uani 1 1 d .
C17 C -0.12754(12) 0.87772(12) 0.23909(12) 0.0282(6) Uani 1 1 d .
C18 C -0.07620(12) 0.84134(12) 0.21583(11) 0.0242(5) Uani 1 1 d .
C20 C 0.07654(13) 0.61023(12) 0.04100(12) 0.0301(6) Uani 1 1 d .
H20a H 0.0320 0.5988 0.0540 0.040 Uiso 1 1 calc R
H20b H 0.1077 0.5823 0.0621 0.040 Uiso 1 1 calc R
C21 C 0.08229(16) 0.59553(15) -0.02315(13) 0.0431(7) Uani 1 1 d .
H21a H 0.0582 0.6285 -0.0448 0.065 Uiso 1 1 calc R
H21b H 0.0640 0.5523 -0.0311 0.065 Uiso 1 1 calc R
H21c H 0.1283 0.5964 -0.0344 0.065 Uiso 1 1 calc R
C22 C 0.15742(13) 0.70109(13) 0.04259(14) 0.0370(7) Uani 1 1 d .
H22a H 0.1616 0.7479 0.0523 0.049 Uiso 1 1 calc R
H22b H 0.1654 0.6965 0.0011 0.049 Uiso 1 1 calc R
C23 C 0.20988(14) 0.66271(14) 0.07503(15) 0.0471(8) Uani 1 1 d .
H23a H 0.1979 0.6599 0.1154 0.071 Uiso 1 1 calc R
H23b H 0.2519 0.6850 0.0713 0.071 Uiso 1 1 calc R
H23c H 0.2133 0.6187 0.0591 0.071 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'
Ce Ce -0.2486 2.6331 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
O O 0.0106 0.0060 '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
N2 Ce1 N1 91.20(5) . 7_464
N2 Ce1 N1 91.20(5) . .
N1 Ce1 N1 177.59(10) 7_464 .
N2 Ce1 O1 114.79(4) . .
N1 Ce1 O1 93.45(6) 7_464 .
N1 Ce1 O1 85.54(6) . .
N2 Ce1 O1 114.79(4) . 7_464
N1 Ce1 O1 85.54(6) 7_464 7_464
N1 Ce1 O1 93.45(6) . 7_464
O1 Ce1 O1 130.42(8) . 7_464
N2 Ce1 F10 151.92(3) . 7_464
N1 Ce1 F10 60.81(6) 7_464 7_464
N1 Ce1 F10 116.78(6) . 7_464
O1 Ce1 F10 68.21(5) . 7_464
O1 Ce1 F10 68.37(5) 7_464 7_464
N2 Ce1 F10 151.92(3) . .
N1 Ce1 F10 116.78(6) 7_464 .
N1 Ce1 F10 60.81(6) . .
O1 Ce1 F10 68.37(5) . .
O1 Ce1 F10 68.21(5) 7_464 .
F10 Ce1 F10 56.16(6) 7_464 .
N2 Ce1 F15 59.90(3) . 7_464
N1 Ce1 F15 71.39(5) 7_464 7_464
N1 Ce1 F15 109.89(6) . 7_464
O1 Ce1 F15 60.60(5) . 7_464
O1 Ce1 F15 155.72(5) 7_464 7_464
F10 Ce1 F15 104.95(4) 7_464 7_464
F10 Ce1 F15 128.83(4) . 7_464
N2 Ce1 F15 59.90(3) . .
N1 Ce1 F15 109.89(6) 7_464 .
N1 Ce1 F15 71.39(5) . .
O1 Ce1 F15 155.72(5) . .
O1 Ce1 F15 60.60(5) 7_464 .
F10 Ce1 F15 128.83(4) 7_464 .
F10 Ce1 F15 104.95(4) . .
F15 Ce1 F15 119.80(6) 7_464 .
C12 F10 Ce1 118.77(15) . .
C18 F15 Ce1 111.41(12) . .
C20 O1 C22 114.11(18) . .
C20 O1 Ce1 120.09(14) . .
C22 O1 Ce1 125.75(14) . .
C7 N1 C1 118.4(2) . .
C7 N1 Ce1 125.31(17) . .
C1 N1 Ce1 115.86(15) . .
C13 N2 C13 116.6(3) 7_464 .
C13 N2 Ce1 121.70(14) 7_464 .
C13 N2 Ce1 121.70(14) . .
C2 C1 C6 115.8(3) . .
C2 C1 N1 121.5(2) . .
C6 C1 N1 122.7(2) . .
F1 C2 C3 118.0(2) . .
F1 C2 C1 119.0(2) . .
C3 C2 C1 123.0(2) . .
F2 C3 C2 120.7(3) . .
F2 C3 C4 120.1(3) . .
C2 C3 C4 119.2(3) . .
F3 C4 C5 120.8(3) . .
F3 C4 C3 119.9(3) . .
C5 C4 C3 119.3(3) . .
F4 C5 C6 119.9(3) . .
F4 C5 C4 119.9(3) . .
C6 C5 C4 120.2(3) . .
F5 C6 C5 118.7(3) . .
F5 C6 C1 118.9(3) . .
C5 C6 C1 122.4(3) . .
N1 C7 C12 118.4(2) . .
N1 C7 C8 128.4(3) . .
C12 C7 C8 113.2(3) . .
F6 C8 C9 117.4(2) . .
F6 C8 C7 120.8(3) . .
C9 C8 C7 121.8(3) . .
F7 C9 C10 119.2(3) . .
F7 C9 C8 118.6(3) . .
C10 C9 C8 122.2(3) . .
F8 C10 C9 121.8(3) . .
F8 C10 C11 120.1(3) . .
C9 C10 C11 118.1(3) . .
F9 C11 C12 120.5(3) . .
F9 C11 C10 121.0(3) . .
C12 C11 C10 118.5(3) . .
F10 C12 C11 117.3(3) . .
F10 C12 C7 116.6(2) . .
C11 C12 C7 126.1(3) . .
C18 C13 C14 113.7(2) . .
C18 C13 N2 117.5(2) . .
C14 C13 N2 128.6(2) . .
F11 C14 C15 117.4(2) . .
F11 C14 C13 119.5(2) . .
C15 C14 C13 123.0(2) . .
F12 C15 C16 119.7(2) . .
F12 C15 C14 119.6(2) . .
C16 C15 C14 120.6(2) . .
F13 C16 C15 121.3(3) . .
F13 C16 C17 120.0(2) . .
C15 C16 C17 118.6(2) . .
F14 C17 C18 120.7(2) . .
F14 C17 C16 120.3(2) . .
C18 C17 C16 119.1(2) . .
F15 C18 C17 118.3(2) . .
F15 C18 C13 116.6(2) . .
C17 C18 C13 125.1(2) . .
O1 C20 C21 113.1(2) . .
O1 C22 C23 113.8(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ce1 N2 2.462(3) .
Ce1 N1 2.5108(19) 7_464
Ce1 N1 2.5108(19) .
Ce1 O1 2.5222(16) .
Ce1 O1 2.5222(16) 7_464
Ce1 F10 2.7155(15) 7_464
Ce1 F10 2.7155(15) .
Ce1 F15 2.8190(14) 7_464
Ce1 F15 2.8190(14) .
F1 C2 1.346(3) .
F2 C3 1.338(3) .
F3 C4 1.335(3) .
F4 C5 1.345(3) .
F5 C6 1.354(3) .
F6 C8 1.347(4) .
F7 C9 1.348(3) .
F8 C10 1.343(3) .
F9 C11 1.341(4) .
F10 C12 1.375(3) .
F11 C14 1.352(3) .
F12 C15 1.340(3) .
F13 C16 1.341(3) .
F14 C17 1.340(3) .
F15 C18 1.366(3) .
O1 C20 1.455(3) .
O1 C22 1.456(3) .
N1 C7 1.379(3) .
N1 C1 1.412(3) .
N2 C13 1.408(3) 7_464
N2 C13 1.408(3) .
C1 C2 1.382(4) .
C1 C6 1.394(3) .
C2 C3 1.373(4) .
C3 C4 1.385(4) .
C4 C5 1.373(5) .
C5 C6 1.365(5) .
C7 C12 1.380(4) .
C7 C8 1.412(3) .
C8 C9 1.379(4) .
C9 C10 1.366(5) .
C10 C11 1.385(4) .
C11 C12 1.376(4) .
C13 C18 1.392(3) .
C13 C14 1.394(3) .
C14 C15 1.385(3) .
C15 C16 1.378(4) .
C16 C17 1.382(4) .
C17 C18 1.372(3) .
C20 C21 1.507(4) .
C22 C23 1.503(4) .
