Heterobimetallic cerium(iv) oxo clusters supported by a tripodal oxygen ligand.
Wong, Kang-Long; So, Yat-Ming; Wang, Guo-Cang; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 45 (2016) 8770–8776; doi:10.1039/c6dt00678g

data_7039122
_publ_section_title
;
 Heterobimetallic cerium(iv) oxo clusters supported by a tripodal oxygen
 ligand.
;
_journal_issue                   21
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              8770
_journal_page_last               8776
_journal_paper_doi               10.1039/c6dt00678g
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety
'C68 H140 Ce4 Co4 O53 P12 V4, 0.33(C6 H14), 0.67(C6 H12), 0.5(O H2)'
_chemical_formula_sum            'C74 H153.67 Ce4 Co4 O53.5 P12 V4'
_chemical_formula_weight         3271.23
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-07-22
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-01-30 deposited with the CCDC.
2016-04-26 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 107.710(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   32.0185(8)
_cell_length_b                   17.4325(4)
_cell_length_c                   24.4487(7)
_cell_measurement_reflns_used    13179
_cell_measurement_temperature    99.9(4)
_cell_measurement_theta_max      73.9200
_cell_measurement_theta_min      4.4070
_cell_volume                     12999.6(6)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      99.9(4)
_diffrn_detector_area_resol_mean 10.3587
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega   33.00   89.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000  -90.0000 56

  2 omega  -69.00   32.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   57.0000    0.0000 101

  3 omega  -49.00   35.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203   37.0000  120.0000 84

  4 omega -108.00  -22.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  -57.0000 -150.0000 86

  5 omega  -94.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -40.8203  125.0000   90.0000 92

  6 omega   39.00  115.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  120.0000 76

  7 omega   34.00   90.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -30.0000   30.0000 56

  8 omega   41.00   96.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -45.0000  -30.0000 55

  9 omega   36.00  135.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -61.0000  120.0000 99

 10 omega   67.00  114.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703 -111.0000  -90.0000 47

 11 omega   30.00  108.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703  -94.0000  -60.0000 78

 12 omega   58.00  166.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   15.0000 -120.0000 108

 13 omega   80.00  173.00   1.0000   25.0000
omega____ theta____ kappa____ phi______ frames
    -      110.5703   30.0000  -60.0000 93
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0089467000
_diffrn_orient_matrix_UB_12      0.0844291000
_diffrn_orient_matrix_UB_13      -0.0111829000
_diffrn_orient_matrix_UB_21      -0.0179715000
_diffrn_orient_matrix_UB_22      0.0251287000
_diffrn_orient_matrix_UB_23      0.0489975000
_diffrn_orient_matrix_UB_31      0.0463449000
_diffrn_orient_matrix_UB_32      -0.0068970000
_diffrn_orient_matrix_UB_33      0.0429815000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0464
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35670
_diffrn_reflns_theta_full        66.500
_diffrn_reflns_theta_max         66.998
_diffrn_reflns_theta_min         4.893
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    18.831
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78083
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET)
(compiled Aug  2 2013,16:46:58)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.671
_exptl_crystal_description       plate
_exptl_crystal_F_000             6551
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.03
_refine_diff_density_max         1.353
_refine_diff_density_min         -0.973
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         11528
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0584
_refine_ls_R_factor_gt           0.0426
_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/[\s^2^(Fo^2^)+(0.0760P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1135
_refine_ls_wR_factor_ref         0.1222
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9229
_reflns_number_total             11528
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00678g2.cif
_cod_data_source_block           colin7a
_cod_depositor_comments
'Adding full bibliography for 7039121--7039122.cif.'
_cod_original_formula_sum        'C74 H153.67 Ce4 Co4 O53.50 P12 V4'
_cod_database_code               7039122
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C3S-C2S = C1S-C2S
 1.5 with sigma of 0.02
 C13S-C14S \\sim C14S-C15S \\sim C15S-C11S \\sim C12S-C11S \\sim C13S-C12S
 with sigma of 0.02
3. Others
 Fixed Sof: C19(0.55) H19A(0.55) H19B(0.55) C19A(0.45) H19C(0.45) H19D(0.45)
 C20(0.5) H20A(0.5) H20B(0.5) H20C(0.5) C20A(0.5) H20D(0.5) H20E(0.5) H20F(0.5)
 C1S(0.33333) H1SA(0.33333) H1SB(0.33333) H1SC(0.33333) C2S(0.33333)
 H2SA(0.33333) H2SB(0.33333) C3S(0.33333) H3SA(0.33333) H3SB(0.33333)
 C11S(0.33333) C12S(0.33333) C13S(0.33333) C14S(0.33333) C15S(0.33333)
 C16S(0.33333) O1W(0.25)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C17(H17A,H17B), C19(H19A,
 H19B), C19A(H19C,H19D), C21(H21A,H21B), C31(H31A,H31B), C33(H33A,H33B),
 C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,H41B), C2S(H2SA,H2SB),
  C3S(H3SA,H3SB)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C3(H3), C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C9(H9),
 C10(H10)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C18(H18A,H18B,
 H18C), C20(H20A,H20B,H20C), C20A(H20D,H20E,H20F), C22(H22A,H22B,H22C),
 C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C36(H36A,H36B,H36C), C38(H38A,H38B,
 H38C), C40(H40A,H40B,H40C), C42(H42A,H42B,H42C), C1S(H1SA,H1SB,H1SC)
;
_shelx_res_checksum              37670
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2014-11-06
_olex2_submission_special_instructions 'No special instructions were received'