#------------------------------------------------------------------------------
#$Date: 2024-12-06 17:29:12 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296319 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/35/7133508.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_7133508
loop_
_publ_author_name
'Blanes-Díaz, Anamar'
'Wacker, Jennifer N.'
'Szymanowski, Jennifer E. S.'
'Bertke, Jeffery A.'
'Knope, Karah E.'
_publ_section_title
;
 Isolation of a chloride-capped cerium polyoxo nanocluster built from 52
 metal ions.
;
_journal_issue                   84
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              12185
_journal_page_last               12188
_journal_paper_doi               10.1039/d4cc03144j
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'Ce Cl6, 4(C5 H6 N), 2(Cl)'
_chemical_formula_sum            'C20 H24 Ce Cl8 N4'
_chemical_formula_weight         744.15
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     intrinsic
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2024-08-08 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                100.578(2)
_cell_angle_beta                 104.990(3)
_cell_angle_gamma                107.349(2)
_cell_formula_units_Z            1
_cell_length_a                   7.5899(6)
_cell_length_b                   9.2556(8)
_cell_length_c                   11.8931(9)
_cell_measurement_reflns_used    9870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.31
_cell_measurement_theta_min      2.40
_cell_volume                     738.90(11)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2005)'
_computing_data_collection       'APEX3 V2016.5-0 (Bruker, 2016)'
_computing_data_reduction
; 
SAINT V8.37A, XPREP v2014/2, SADABS V2016/2 (Bruker, 2016) 
;
_computing_molecular_graphics    'SHELXLE v932 (Hubschle, 2011)'
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'Bruker D8 Quest/Photon 100'
_diffrn_measurement_method       'profile data from φ and ω scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0462
_diffrn_reflns_av_unetI/netI     0.0177
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            36075
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.375
_diffrn_reflns_theta_min         2.403
_diffrn_source                   'microfocus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.280
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6942
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.672
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             366
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.170
_exptl_crystal_size_min          0.038
_refine_diff_density_max         0.644
_refine_diff_density_min         -1.825
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         2710
_refine_ls_number_restraints     637
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0343
_refine_ls_R_factor_gt           0.0267
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0142P)²+1.7211P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0560
_refine_ls_wR_factor_ref         0.0600
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2475
_reflns_number_total             2710
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03144j2.cif
_cod_data_source_block           pbar1b_a
_cod_depositor_comments
'Adding full bibliography for 7133508--7133511.cif.'
_cod_original_cell_volume        738.90(10)
_cod_database_code               7133508
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ce1 Ce 0.500000 0.500000 0.000000 0.02631(10) Uani 1 2 d DS . P . .
Cl1 Cl 0.6917(18) 0.7904(3) 0.1403(7) 0.0338(14) Uani 0.82(4) 1 d D U P A 1
Cl1B Cl 0.637(3) 0.7965(9) 0.1183(14) 0.017(2) Uani 0.18(4) 1 d D U P A 2
Cl2 Cl 0.287(2) 0.4425(6) 0.1399(11) 0.0272(13) Uani 0.72(4) 1 d D U P A 1
Cl2B Cl 0.343(3) 0.4517(13) 0.1669(13) 0.0155(17) Uani 0.28(4) 1 d D U P A 2
Cl3 Cl 0.773(2) 0.421(2) 0.127(2) 0.034(2) Uani 0.43(9) 1 d D U P A 1
Cl3B Cl 0.7607(19) 0.4273(16) 0.1453(17) 0.0339(17) Uani 0.57(9) 1 d D U P A 2
Cl4 Cl 0.2443(7) 0.7481(4) 0.4658(12) 0.0556(13) Uani 0.57(3) 1 d . U P B 1
Cl4B Cl 0.2453(8) 0.7552(6) 0.5112(15) 0.0553(17) Uani 0.43(3) 1 d . U P B 2
N1 N 0.8707(15) 1.1766(14) 0.9277(10) 0.039(2) Uani 0.395(7) 1 d D U P C 1
HN1A H 0.974(10) 1.240(12) 0.990(7) 0.059 Uiso 0.395(7) 1 d D U P C 1
C1 C 0.755(2) 1.0308(19) 0.9403(10) 0.036(2) Uani 0.395(7) 1 d D U P C 1
H1 H 0.787306 1.004134 1.014513 0.043 Uiso 0.395(7) 1 calc R U P C 1
C2 C 0.5972(18) 0.9309(12) 0.8423(15) 0.027(2) Uani 0.395(7) 1 d D U P C 1
H2 H 0.519121 0.832223 0.847073 0.032 Uiso 0.395(7) 1 calc R U P C 1
C3 C 0.5535(15) 0.9719(15) 0.7413(10) 0.026(2) Uani 0.395(7) 1 d D U P C 1
H3 H 0.436290 0.905191 0.677159 0.031 Uiso 0.395(7) 1 calc R U P C 1
C4 C 0.660(2) 1.096(2) 0.7250(10) 0.035(2) Uani 0.395(7) 1 d D U P C 1
H4 H 0.624958 1.111682 0.646625 0.041 Uiso 0.395(7) 1 calc R U P C 1
C5 C 0.8111(19) 1.2014(12) 0.8079(13) 0.024(2) Uani 0.395(7) 1 d D U P C 1
H5 H 0.883345 1.293949 0.792019 0.029 Uiso 0.395(7) 1 calc R U P C 1
N1B N 0.8479(10) 1.2166(7) 0.8843(9) 0.0374(15) Uani 0.605(7) 1 d D U P C 2
HN1B H 0.940(8) 1.313(4) 0.918(6) 0.056 Uiso 0.605(7) 1 d D U P C 2
C1B C 0.8039(12) 1.1081(11) 0.9560(5) 0.0272(14) Uani 0.605(7) 1 d D U P C 2
H1B H 0.877186 1.134674 1.039711 0.033 Uiso 0.605(7) 1 calc R U P C 2
C2B C 0.6527(14) 0.9656(9) 0.8984(9) 0.0282(15) Uani 0.605(7) 1 d D U P C 2
H2B H 0.618352 0.892077 0.942495 0.034 Uiso 0.605(7) 1 calc R U P C 2
C3B C 0.5534(10) 0.9304(9) 0.7799(9) 0.0307(16) Uani 0.605(7) 1 d D U P C 2
H3B H 0.451485 0.830147 0.740939 0.037 Uiso 0.605(7) 1 calc R U P C 2
C4B C 0.5905(16) 1.0259(13) 0.7180(6) 0.0372(18) Uani 0.605(7) 1 d D U P C 2
H4B H 0.515808 0.993487 0.634146 0.045 Uiso 0.605(7) 1 calc R U P C 2
C5B C 0.7258(17) 1.1663(10) 0.7633(8) 0.0283(15) Uani 0.605(7) 1 d D U P C 2
H5B H 0.741699 1.235368 0.713549 0.034 Uiso 0.605(7) 1 calc R U P C 2
N2 N 0.190(2) 0.4064(11) 0.4815(8) 0.034(2) Uani 0.437(7) 1 d D U P D 1
HN2A H 0.229(19) 0.507(3) 0.498(10) 0.052 Uiso 0.437(7) 1 d D U P D 1
C6 C 0.2364(17) 0.3271(12) 0.5616(7) 0.0367(18) Uani 0.437(7) 1 d D U P D 1
H6 H 0.310815 0.382637 0.644157 0.044 Uiso 0.437(7) 1 calc R U P D 1
C7 C 0.1758(16) 0.1667(10) 0.5238(8) 0.0385(18) Uani 0.437(7) 1 d D U P D 1
H7 H 0.207227 0.109505 0.579772 0.046 Uiso 0.437(7) 1 calc R U P D 1
C8 C 0.0684(16) 0.0885(10) 0.4036(8) 0.042(2) Uani 0.437(7) 1 d D U P D 1
H8 H 0.025945 -0.023211 0.376017 0.050 Uiso 0.437(7) 1 calc R U P D 1
C9 C 0.0232(17) 0.1720(10) 0.3240(8) 0.037(2) Uani 0.437(7) 1 d D U P D 1
H9 H -0.049777 0.118458 0.240885 0.045 Uiso 0.437(7) 1 calc R U P D 1
C10 C 0.083(2) 0.3332(11) 0.3644(9) 0.034(2) Uani 0.437(7) 1 d D U P D 1
H10 H 0.049640 0.392013 0.310326 0.040 Uiso 0.437(7) 1 calc R U P D 1
N2B N 0.2096(17) 0.4186(8) 0.4563(7) 0.034(2) Uani 0.563(7) 1 d D U P D 2
HN2B H 0.214(15) 0.513(5) 0.459(7) 0.050 Uiso 0.563(7) 1 d D U P D 2
C6B C 0.3080(12) 0.4054(9) 0.5633(6) 0.0357(16) Uani 0.563(7) 1 d D U P D 2
H6B H 0.371866 0.494668 0.632699 0.043 Uiso 0.563(7) 1 calc R U P D 2
C7B C 0.3145(13) 0.2612(8) 0.5703(6) 0.0406(16) Uani 0.563(7) 1 d D U P D 2
H7B H 0.384906 0.249425 0.644507 0.049 Uiso 0.563(7) 1 calc R U P D 2
C8B C 0.2180(13) 0.1330(8) 0.4687(7) 0.0411(16) Uani 0.563(7) 1 d D U P D 2
H8B H 0.219665 0.032072 0.473386 0.049 Uiso 0.563(7) 1 calc R U P D 2
C9B C 0.1196(14) 0.1505(8) 0.3610(7) 0.0406(16) Uani 0.563(7) 1 d D U P D 2
H9B H 0.054461 0.062540 0.290658 0.049 Uiso 0.563(7) 1 calc R U P D 2
C10B C 0.1166(15) 0.2967(9) 0.3561(7) 0.034(2) Uani 0.563(7) 1 d D U P D 2
H10B H 0.049056 0.311230 0.282327 0.041 Uiso 0.563(7) 1 calc R U P D 2
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'
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'
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
Cl1B Ce1 Cl2B 86.1(4) . . ?
Cl1B Ce1 Cl2B 93.9(4) 2_665 . ?
Cl2B Ce1 Cl2B 180.0(7) 2_665 . ?
Cl3 Ce1 Cl3 180.0 . 2_665 ?
Cl1B Ce1 Cl3B 84.5(6) . 2_665 ?
Cl1B Ce1 Cl3B 95.5(6) 2_665 2_665 ?
Cl2B Ce1 Cl3B 78.9(7) 2_665 2_665 ?
Cl2B Ce1 Cl3B 101.1(7) . 2_665 ?
Cl3 Ce1 Cl3B 174.3(7) . 2_665 ?
Cl3 Ce1 Cl3B 5.7(7) 2_665 2_665 ?
Cl1B Ce1 Cl3B 95.5(6) . . ?
Cl1B Ce1 Cl3B 84.5(6) 2_665 . ?
Cl2B Ce1 Cl3B 101.1(7) 2_665 . ?
Cl2B Ce1 Cl3B 78.9(7) . . ?
Cl3B Ce1 Cl3B 180.0 2_665 . ?
Cl3 Ce1 Cl2 87.1(7) . 2_665 ?
Cl3 Ce1 Cl2 92.9(7) 2_665 2_665 ?
Cl3 Ce1 Cl2 92.9(7) . . ?
Cl3 Ce1 Cl2 87.1(7) 2_665 . ?
Cl2 Ce1 Cl2 180.0 2_665 . ?
Cl3 Ce1 Cl1 92.1(6) . 2_665 ?
Cl3 Ce1 Cl1 87.9(6) 2_665 2_665 ?
Cl2 Ce1 Cl1 90.5(2) 2_665 2_665 ?
Cl2 Ce1 Cl1 89.5(2) . 2_665 ?
Cl3 Ce1 Cl1 87.9(6) . . ?
Cl3 Ce1 Cl1 92.1(6) 2_665 . ?
Cl2 Ce1 Cl1 89.5(2) 2_665 . ?
Cl2 Ce1 Cl1 90.5(2) . . ?
Cl1 Ce1 Cl1 180.00(8) 2_665 . ?
C1 N1 C5 115.9(7) . . ?
C1 N1 HN1A 118(8) . . ?
C5 N1 HN1A 125(9) . . ?
C2 C1 N1 117.9(8) . . ?
C2 C1 H1 121.0 . . ?
N1 C1 H1 121.0 . . ?
C3 C2 C1 119.9(8) . . ?
C3 C2 H2 120.1 . . ?
C1 C2 H2 120.1 . . ?
C4 C3 C2 123.5(9) . . ?
C4 C3 H3 118.3 . . ?
C2 C3 H3 118.3 . . ?
C3 C4 C5 123.8(9) . . ?
C3 C4 H4 118.1 . . ?
C5 C4 H4 118.1 . . ?
C4 C5 N1 118.7(8) . . ?
C4 C5 H5 120.6 . . ?
N1 C5 H5 120.6 . . ?
C5B N1B C1B 115.9(5) . . ?
C5B N1B HN1B 122(5) . . ?
C1B N1B HN1B 121(5) . . ?
C2B C1B N1B 117.5(6) . . ?
C2B C1B H1B 121.2 . . ?
N1B C1B H1B 121.2 . . ?
C3B C2B C1B 120.0(6) . . ?
C3B C2B H2B 120.0 . . ?
C1B C2B H2B 120.0 . . ?
C4B C3B C2B 122.3(7) . . ?
C4B C3B H3B 118.8 . . ?
C2B C3B H3B 118.8 . . ?
C3B C4B C5B 123.4(7) . . ?
C3B C4B H4B 118.3 . . ?
C5B C4B H4B 118.3 . . ?
C4B C5B N1B 120.7(6) . . ?
C4B C5B H5B 119.6 . . ?
N1B C5B H5B 119.6 . . ?
C10 N2 C6 122.3(8) . . ?
C10 N2 HN2A 113(7) . . ?
C6 N2 HN2A 125(7) . . ?
N2 C6 C7 119.7(8) . . ?
N2 C6 H6 120.1 . . ?
C7 C6 H6 120.1 . . ?
C6 C7 C8 119.2(7) . . ?
C6 C7 H7 120.4 . . ?
C8 C7 H7 120.4 . . ?
C9 C8 C7 119.9(7) . . ?
C9 C8 H8 120.1 . . ?
C7 C8 H8 120.1 . . ?
C8 C9 C10 119.9(8) . . ?
C8 C9 H9 120.1 . . ?
C10 C9 H9 120.1 . . ?
N2 C10 C9 119.0(9) . . ?
N2 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10B N2B C6B 123.0(7) . . ?
C10B N2B HN2B 124(6) . . ?
C6B N2B HN2B 113(6) . . ?
N2B C6B C7B 118.8(7) . . ?
N2B C6B H6B 120.6 . . ?
C7B C6B H6B 120.6 . . ?
C6B C7B C8B 119.4(6) . . ?
C6B C7B H7B 120.3 . . ?
C8B C7B H7B 120.3 . . ?
C9B C8B C7B 120.4(6) . . ?
C9B C8B H8B 119.8 . . ?
C7B C8B H8B 119.8 . . ?
C8B C9B C10B 119.1(6) . . ?
C8B C9B H9B 120.5 . . ?
C10B C9B H9B 120.5 . . ?
N2B C10B C9B 119.3(7) . . ?
N2B C10B H10B 120.3 . . ?
C9B C10B H10B 120.3 . . ?
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
Ce1 Cl1B 2.592(7) . ?
Ce1 Cl1B 2.592(7) 2_665 ?
Ce1 Cl2B 2.605(6) 2_665 ?
Ce1 Cl2B 2.605(6) . ?
Ce1 Cl3 2.608(6) . ?
Ce1 Cl3 2.608(6) 2_665 ?
Ce1 Cl3B 2.609(5) 2_665 ?
Ce1 Cl3B 2.609(5) . ?
Ce1 Cl2 2.620(3) 2_665 ?
Ce1 Cl2 2.620(3) . ?
Ce1 Cl1 2.625(3) 2_665 ?
Ce1 Cl1 2.625(3) . ?
N1 C1 1.432(11) . ?
N1 C5 1.461(11) . ?
N1 HN1A 0.88(2) . ?
C1 C2 1.368(11) . ?
C1 H1 0.9500 . ?
C2 C3 1.316(11) . ?
C2 H2 0.9500 . ?
C3 C4 1.275(11) . ?
C3 H3 0.9500 . ?
C4 C5 1.278(12) . ?
C4 H4 0.9500 . ?
C5 H5 0.9500 . ?
N1B C5B 1.397(9) . ?
N1B C1B 1.453(9) . ?
N1B HN1B 0.90(2) . ?
C1B C2B 1.373(9) . ?
C1B H1B 0.9500 . ?
C2B C3B 1.340(9) . ?
C2B H2B 0.9500 . ?
C3B C4B 1.265(10) . ?
C3B H3B 0.9500 . ?
C4B C5B 1.302(10) . ?
C4B H4B 0.9500 . ?
C5B H5B 0.9500 . ?
N2 C10 1.341(8) . ?
N2 C6 1.343(9) . ?
N2 HN2A 0.86(2) . ?
C6 C7 1.364(11) . ?
C6 H6 0.9500 . ?
C7 C8 1.378(11) . ?
C7 H7 0.9500 . ?
C8 C9 1.367(11) . ?
C8 H8 0.9500 . ?
C9 C10 1.372(10) . ?
C9 H9 0.9500 . ?
C10 H10 0.9500 . ?
N2B C10B 1.337(7) . ?
N2B C6B 1.346(8) . ?
N2B HN2B 0.86(2) . ?
C6B C7B 1.366(9) . ?
C6B H6B 0.9500 . ?
C7B C8B 1.379(10) . ?
C7B H7B 0.9500 . ?
C8B C9B 1.370(11) . ?
C8B H8B 0.9500 . ?
C9B C10B 1.372(9) . ?
C9B H9B 0.9500 . ?
C10B H10B 0.9500 . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
N1^a HN1A^a Cl2^a 0.88(2) 2.50(3) 3.373(17) 170(11) 1_666 yes
N2^a HN2A^a Cl4^a 0.86(2) 2.31(5) 3.113(10) 157(10) . yes
N2B^b HN2B^b Cl4B^b 0.86(2) 2.13(3) 2.977(9) 167(8) . yes
