Probing the Reactivity of the Ce═O Multiple Bond in a Cerium(IV) Oxo Complex.
So, Yat-Ming; Li, Yang; Au-Yeung, Ka-Chun; Wang, Guo-Cang; Wong, Kang-Long; Sung, Herman H. Y.; Arnold, Polly L.; Williams, Ian D.; Lin, Zhenyang; Leung, Wa-Hung; Inorganic chemistry 55 (2016) 10003–10012; doi:10.1021/acs.inorgchem.6b00480

data_4347687
_publ_section_title
;
 Probing the Reactivity of the Ce&#x2550;O Multiple Bond in a Cerium(IV)
 Oxo Complex.
;
_journal_issue                   20
_journal_name_full               'Inorganic chemistry'
_journal_page_first              10003
_journal_page_last               10012
_journal_paper_doi               10.1021/acs.inorgchem.6b00480
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C34 H74 Ce Co2 O20 P6, C17 H35 Co O9 P3'
_chemical_formula_sum            'C51 H109 Ce Co3 O29 P9'
_chemical_formula_weight         1782.02
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2013-04-23
_audit_creation_method
;
  Olex2 1.2-beta
  (compiled May  9 2012 12:37:22, GUI svn.r4230)
;
_cell_angle_alpha                88.223(3)
_cell_angle_beta                 83.785(4)
_cell_angle_gamma                65.020(4)
_cell_formula_units_Z            2
_cell_length_a                   15.2055(6)
_cell_length_b                   15.2969(6)
_cell_length_c                   18.2720(8)
_cell_measurement_reflns_used    9556
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      71.4700
_cell_measurement_theta_min      4.0210
_cell_volume                     3829.3(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      143(2)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.9843
_diffrn_measured_fraction_theta_max 0.5356
_diffrn_measurement_details
;
  1 omega   40.00   66.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000 -120.0000 26

  2 omega  -70.00  -24.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  150.0000 46

  3 omega  -23.00   28.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000  -77.0000  150.0000 51

  4 omega   34.00   75.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -        0.0000 -178.0000   60.0000 41

  5 omega -127.00  -30.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -      -55.0000  -38.0000  -30.0000 97

  6 omega   77.00  124.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000  125.0000  -30.0000 47

  7 omega    0.00   91.00   1.0000    5.0000
omega____ theta____ kappa____ phi______ frames
    -       55.0000 -125.0000  120.0000 91

  8 omega  -72.00    9.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   25.0000  -30.0000 81

  9 omega -139.00  -81.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000  178.0000  120.0000 58

 10 omega  -68.00  -11.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      -64.0000   38.0000 -150.0000 57

 11 omega   39.00   71.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000  120.0000 32

 12 omega   39.00  112.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -90.0000 73

 13 omega   40.00   75.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000   30.0000 35

 14 omega   46.00   79.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -50.0000  -90.0000 33

 15 omega   37.00   64.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -150.0000 27

 16 omega   42.00   68.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   60.0000 26

 17 omega   39.00   78.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000 -111.0000 -120.0000 39

 18 omega   41.00   67.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000 -180.0000 26

 19 omega   37.00   72.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -25.0000  -30.0000 35

 20 omega   88.00  177.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000   50.0000    0.0000 89

 21 omega   48.00  123.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  150.0000 75

 22 omega   49.00  141.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000    0.0000 92

 23 omega   42.00   70.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -38.0000   90.0000 28

 24 omega  122.00  148.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -92.0000  -90.0000 26

 25 omega   58.00  173.00   1.0000   20.0000
omega____ theta____ kappa____ phi______ frames
    -      110.0000  -12.0000  -30.0000 115
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0807148000
_diffrn_orient_matrix_UB_12      0.1030823000
_diffrn_orient_matrix_UB_13      -0.0035600000
_diffrn_orient_matrix_UB_21      -0.0287380000
_diffrn_orient_matrix_UB_22      -0.0273761000
_diffrn_orient_matrix_UB_23      -0.0712618000
_diffrn_orient_matrix_UB_31      -0.0727427000
_diffrn_orient_matrix_UB_32      -0.0311763000
_diffrn_orient_matrix_UB_33      0.0458689000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0642
_diffrn_reflns_av_unetI/netI     0.0975
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            23016
_diffrn_reflns_theta_full        66.50
_diffrn_reflns_theta_max         67.00
_diffrn_reflns_theta_min         3.22
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           35
_diffrn_source_power             1.75
_diffrn_source_target            Cu
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    11.923
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75066
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET)
(compiled Dec  3 2012,18:21:49)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.546
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1842
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.851
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         13407
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0599
_refine_ls_R_factor_gt           0.0452
_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 
 [0.00000+1.00000exp(0.10(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0120P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0939
_refine_ls_wR_factor_ref         0.0995
_reflns_number_gt                10803
_reflns_number_total             13407
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic6b00480_si_001.cif
_cod_data_source_block           so59cult
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_symmetry_cell_setting' value 'Triclinic' was changed to
'triclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4347687
_reflns_odcompleteness_completeness 98.43
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     68.13