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#$Date: 2024-12-06 17:29:12 +0200 (Fri, 06 Dec 2024) $
#$Revision: 296319 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/13/35/7133509.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_7133509
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         'C10 H12 Ce Cl6 N2'
_chemical_formula_sum            'C10 H12 Ce Cl6 N2'
_chemical_formula_weight         513.04
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2017/1
_audit_update_record
;
2024-08-08 deposited with the CCDC.	2024-08-14 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.8270(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.9930(6)
_cell_length_b                   8.6538(4)
_cell_length_c                   7.9621(3)
_cell_measurement_reflns_used    9881
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.99
_cell_measurement_theta_min      2.58
_cell_volume                     886.91(7)
_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  'SHELX-2018-1 (Sheldrick, 2015)'
_computing_structure_solution    'SHELX-2014-5 (Sheldrick, 2015)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0095
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            25090
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.255
_diffrn_reflns_theta_min         2.582
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.457
_exptl_absorpt_correction_T_max  0.91599
_exptl_absorpt_correction_T_min  0.73862
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2016/2 (Bruker, 2016)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.921
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             492
_exptl_crystal_size_max          0.129
_exptl_crystal_size_mid          0.106
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.698
_refine_diff_density_min         -0.484
_refine_diff_density_rms         0.082
_refine_ls_extinction_coef       0.0048(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2017/1 (Sheldrick 2017)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     107
_refine_ls_number_reflns         1179
_refine_ls_number_restraints     180
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0217
_refine_ls_R_factor_gt           0.0217
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0412P)²+0.8068P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0607
_refine_ls_wR_factor_ref         0.0607
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1179
_reflns_number_total             1179
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d4cc03144j2.cif
_cod_data_source_block           c2overm_a_save2
_cod_depositor_comments
'Adding full bibliography for 7133508--7133511.cif.'
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7133509
_shelx_shelxl_version_number     2017/1
_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.
;
_shelx_estimated_absorpt_t_min   0.664
_shelx_estimated_absorpt_t_max   0.889
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.04225(13) Uani 1 4 d S T P . .
Cl1 Cl 0.58407(9) 0.500000 0.31320(12) 0.0656(3) Uani 1 2 d S T P . .
Cl2 Cl 0.500000 0.79920(14) 0.000000 0.0768(3) Uani 1 2 d S T P . .
Cl3 Cl 0.31704(9) 0.500000 0.10483(15) 0.0818(4) Uani 1 2 d S T P . .
N1 N 0.3717(14) 0.8814(11) 0.5476(11) 0.058(2) Uani 0.25 1 d G U P A -1
H1A H 0.379564 0.809081 0.622324 0.069 Uiso 0.25 1 calc R U P A -1
C1 C 0.3591(14) 0.8447(11) 0.3761(12) 0.049(2) Uani 0.25 1 d G U P A -1
H1B H 0.359147 0.741852 0.342125 0.058 Uiso 0.25 1 calc R U P A -1
C2 C 0.3465(13) 0.9616(13) 0.2553(9) 0.047(2) Uani 0.25 1 d G U P A -1
H2 H 0.338013 0.937005 0.140591 0.057 Uiso 0.25 1 calc R U P A -1
C3 C 0.3464(13) 1.1153(12) 0.3061(10) 0.045(2) Uani 0.25 1 d G U P A -1
H3 H 0.337934 1.193501 0.225334 0.054 Uiso 0.25 1 calc R U P A -1
C4 C 0.3590(12) 1.1520(10) 0.4776(11) 0.053(2) Uani 0.25 1 d G U P A -1
H4 H 0.358988 1.254845 0.511612 0.064 Uiso 0.25 1 calc R U P A -1
C5 C 0.3717(12) 1.0351(12) 0.5984(9) 0.060(3) Uani 0.25 1 d G U P A -1
H5 H 0.380122 1.059693 0.713149 0.072 Uiso 0.25 1 calc R U P A -1
N1B N 0.3738(13) 0.930(3) 0.5728(14) 0.053(2) Uani 0.25 1 d G U P B -2
H1C H 0.384461 0.879983 0.667111 0.063 Uiso 0.25 1 calc R U P B -2
C1B C 0.3644(17) 0.850(2) 0.420(3) 0.045(2) Uani 0.25 1 d G U P B -2
H1D H 0.369641 0.742793 0.419664 0.054 Uiso 0.25 1 calc R U P B -2
C2B C 0.3470(15) 0.930(3) 0.2676(14) 0.047(2) Uani 0.25 1 d G U P B -2
H2B H 0.340752 0.876999 0.165365 0.057 Uiso 0.25 1 calc R U P B -2
C3B C 0.3391(13) 1.091(3) 0.2681(14) 0.048(2) Uani 0.25 1 d G U P B -2
H3B H 0.327556 1.144347 0.166184 0.057 Uiso 0.25 1 calc R U P B -2
C4B C 0.3485(16) 1.170(2) 0.421(3) 0.051(3) Uani 0.25 1 d G U P B -2
H4B H 0.343247 1.277490 0.421301 0.061 Uiso 0.25 1 calc R U P B -2
C5B C 0.3658(13) 1.090(3) 0.5733(14) 0.058(3) Uani 0.25 1 d G U P B -2
H5B H 0.372136 1.143286 0.675602 0.069 Uiso 0.25 1 calc R U P B -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_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0.00 0.00 1.00 0.0100
0.00 0.00 -1.00 0.0170
2.00 0.00 1.00 0.0360
-2.00 1.00 2.00 0.0290
2.00 -1.00 -2.00 0.0430
-2.00 1.00 1.00 0.0350
-1.00 1.00 0.00 0.0420
2.00 -1.00 0.00 0.0560
-2.00 -2.00 1.00 0.0390
2.00 1.00 -1.00 0.0480
2.00 1.00 1.00 0.0470
1.00 0.00 0.00 0.0480
-1.00 0.00 0.00 0.0280
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
Cl1 Ce1 Cl1 180.0 5_665 . ?
Cl1 Ce1 Cl2 90.0 5_665 5_665 ?
Cl1 Ce1 Cl2 90.0 . 5_665 ?
Cl1 Ce1 Cl2 90.0 5_665 . ?
Cl1 Ce1 Cl2 90.0 . . ?
Cl2 Ce1 Cl2 180.0 5_665 . ?
Cl1 Ce1 Cl3 88.58(4) 5_665 5_665 ?
Cl1 Ce1 Cl3 91.42(4) . 5_665 ?
Cl2 Ce1 Cl3 90.0 5_665 5_665 ?
Cl2 Ce1 Cl3 90.0 . 5_665 ?
Cl1 Ce1 Cl3 91.42(4) 5_665 . ?
Cl1 Ce1 Cl3 88.58(4) . . ?
Cl2 Ce1 Cl3 90.0 5_665 . ?
Cl2 Ce1 Cl3 90.0 . . ?
Cl3 Ce1 Cl3 180.0 5_665 . ?
C1 N1 C5 120.0 . . ?
C1 N1 H1A 120.0 . . ?
C5 N1 H1A 120.0 . . ?
N1 C1 C2 120.0 . . ?
N1 C1 H1B 120.0 . . ?
C2 C1 H1B 120.0 . . ?
C1 C2 C3 120.0 . . ?
C1 C2 H2 120.0 . . ?
C3 C2 H2 120.0 . . ?
C2 C3 C4 120.0 . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C3 C4 C5 120.0 . . ?
C3 C4 H4 120.0 . . ?
C5 C4 H4 120.0 . . ?
C4 C5 N1 120.0 . . ?
C4 C5 H5 120.0 . . ?
N1 C5 H5 120.0 . . ?
C1B N1B C5B 120.0 . . ?
C1B N1B H1C 120.0 . . ?
C5B N1B H1C 120.0 . . ?
C2B C1B N1B 120.0 . . ?
C2B C1B H1D 120.0 . . ?
N1B C1B H1D 120.0 . . ?
C1B C2B C3B 120.0 . . ?
C1B C2B H2B 120.0 . . ?
C3B C2B H2B 120.0 . . ?
C4B C3B C2B 120.0 . . ?
C4B C3B H3B 120.0 . . ?
C2B C3B H3B 120.0 . . ?
C3B C4B C5B 120.0 . . ?
C3B C4B H4B 120.0 . . ?
C5B C4B H4B 120.0 . . ?
C4B C5B N1B 120.0 . . ?
C4B C5B H5B 120.0 . . ?
N1B C5B H5B 120.0 . . ?
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 Cl1 2.5826(9) 5_665 ?
Ce1 Cl1 2.5826(9) . ?
Ce1 Cl2 2.5892(12) 5_665 ?
Ce1 Cl2 2.5893(12) . ?
Ce1 Cl3 2.6244(11) 5_665 ?
Ce1 Cl3 2.6245(11) . ?
N1 C1 1.3900 . ?
N1 C5 1.3900 . ?
N1 H1A 0.8600 . ?
C1 C2 1.3900 . ?
C1 H1B 0.9300 . ?
C2 C3 1.3900 . ?
C2 H2 0.9300 . ?
C3 C4 1.3900 . ?
C3 H3 0.9300 . ?
C4 C5 1.3900 . ?
C4 H4 0.9300 . ?
C5 H5 0.9300 . ?
N1B C1B 1.3900 . ?
N1B C5B 1.3900 . ?
N1B H1C 0.8600 . ?
C1B C2B 1.3900 . ?
C1B H1D 0.9300 . ?
C2B C3B 1.3900 . ?
C2B H2B 0.9300 . ?
C3B C4B 1.3900 . ?
C3B H3B 0.9300 . ?
C4B C5B 1.3900 . ?
C4B H4B 0.9300 . ?
C5B H5B 0.9300 . ?
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 H1A Cl1 0.86 2.75 3.504(9) 146.9 5_666 yes
N1B^b H1C^b Cl2 0.86 2.95 3.744(11) 154.9 1_556 yes
