Iodosylbenzene and iodylbenzene adducts of cerium(iv) complexes bearing chelating oxygen ligands.
Au-Yeung, Ka-Chun; So, Yat-Ming; Wang, Guo-Cang; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 45 (2016) 5434–5438; doi:10.1039/c6dt00267f

data_7038666
_publ_section_title
;
 Iodosylbenzene and iodylbenzene adducts of cerium(iv) complexes bearing
 chelating oxygen ligands.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5434
_journal_page_last               5438
_journal_paper_doi               10.1039/c6dt00267f
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C46 H80 Ce Cl2 Co2 I2 O20 P6, C H2 Cl2'
_chemical_formula_sum            'C47 H82 Ce Cl4 Co2 I2 O20 P6'
_chemical_formula_weight         1806.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_space_group_name_H-M_alt        'P 1 2/c 1'
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-08-04
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2016-02-02 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.574(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.8983(5)
_cell_length_b                   12.6591(2)
_cell_length_c                   44.0778(11)
_cell_measurement_reflns_used    14865
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      28.7590
_cell_measurement_theta_min      3.3420
_cell_volume                     13445.9(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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_environment      N~2~
_diffrn_ambient_temperature      99.9(5)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
  1 omega  -52.00   54.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0886  -57.0000   90.0000 142

  2 omega  -20.00   65.50   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0886  -99.0000 -120.0000 114

  3 omega  -15.00   96.00   0.7500   10.0000
omega____ theta____ kappa____ phi______ frames
    -       18.0886   57.0000   30.0000 148
;
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Mo at zero, Atlas'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0000229000
_diffrn_orient_matrix_UB_12      -0.0211869000
_diffrn_orient_matrix_UB_13      0.0148926000
_diffrn_orient_matrix_UB_21      -0.0283247000
_diffrn_orient_matrix_UB_22      0.0141388000
_diffrn_orient_matrix_UB_23      -0.0023854000
_diffrn_orient_matrix_UB_31      -0.0080117000
_diffrn_orient_matrix_UB_32      -0.0499126000
_diffrn_orient_matrix_UB_33      -0.0069961000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0850
_diffrn_reflns_av_unetI/netI     0.1163
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -54
_diffrn_reflns_number            78433
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.340
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_diffrn_source_current           0.80
_diffrn_source_power             0.040
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    2.439
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.52996
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.785
_exptl_crystal_description       block
_exptl_crystal_F_000             7200
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.637
_refine_diff_density_min         -1.169
_refine_diff_density_rms         0.181
_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     1478
_refine_ls_number_reflns         26334
_refine_ls_number_restraints     119
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0582
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1058
_refine_ls_wR_factor_ref         0.1259
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16680
_reflns_number_total             26334
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00267f2.cif
_cod_data_source_block           ka40molt
_cod_depositor_comments
'Adding full bibliography for 7038664--7038666.cif.'
_cod_database_code               7038666
_chemical_oxdiff_formula         'Cp2 Co2 Et12 O18 P6 Ce1 Cl2 I2'
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All C(H,H,H,H,H,H) groups
2. Restrained distances
 C14A-C13A
 1.52 with sigma of 0.02
 C14A-C13A
 1.52 with sigma of 0.02
 C33-C33B = C33B-C34B
 1.52 with sigma of 0.02
 C36B-C35B = C36-C35
 1.52 with sigma of 0.02
 C16-C15 = C15B-C16B
 1.52 with sigma of 0.02
 C16-C15 = C15B-C16B
 1.52 with sigma of 0.02
 C16-C15 = C15B-C16B
 1.52 with sigma of 0.02
 C16-C15 = C15B-C16B
 1.52 with sigma of 0.02
 C39-C40 = C40B-C39B
 1.52 with sigma of 0.02
 C39-C40 = C40B-C39B
 1.52 with sigma of 0.02
 C22C-C21A = C21A-C22A
 1.52 with sigma of 0.02
 C22C-C21A = C21A-C22A
 1.52 with sigma of 0.02
 C14A-C13A
 1.52 with sigma of 0.02
 C38-C37 = C37B-C38B
 1.52 with sigma of 0.02
 C42A-C41A
 1.52 with sigma of 0.02
 C42A-C41A = C42C-C41A
 1.52 with sigma of 0.02
 C22-C21
 1.52 with sigma of 0.02
 C22-C21 = C22B-C21
 1.52 with sigma of 0.02
 Cl4S-C2S = Cl5S-C2SA = C2S-Cl3S = C2SA-Cl3S
 1.72 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C31A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C1) \\sim Ueq, Uanis(C2) \\sim Ueq, Uanis(C3) \\sim Ueq, Uanis(C4) \\sim
Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C10) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.002
Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of
0.005 and sigma for terminal atoms of 0.002
Uanis(C35A) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.003
Uanis(C19) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.005
Uanis(C5A) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: O15B(0.45) O15(0.55) C15(0.6) H15A(0.6) H15B(0.6) C15B(0.4)
 H15C(0.4) H15D(0.4) C16B(0.5) H16A(0.5) H16B(0.5) H16C(0.5) C16(0.5) H16D(0.5)
 H16E(0.5) H16F(0.5) C22(0.7) H22A(0.7) H22B(0.7) H22C(0.7) C22B(0.3) H22D(0.3)
 H22E(0.3) H22F(0.3) C33(0.7) H33A(0.7) H33B(0.7) C33B(0.3) H33C(0.3) H33D(0.3)
 C34(0.6) H34A(0.6) H34B(0.6) H34C(0.6) C34B(0.4) H34D(0.4) H34E(0.4) H34F(0.4)
 C35B(0.4) H35A(0.4) H35B(0.4) C35(0.6) H35C(0.6) H35D(0.6) C36B(0.4) H36A(0.4)
 H36B(0.4) H36C(0.4) C36(0.6) H36D(0.6) H36E(0.6) H36F(0.6) C37B(0.4) H37A(0.4)
 H37B(0.4) C37(0.6) H37C(0.6) H37D(0.6) C38(0.6) H38A(0.6) H38B(0.6) H38C(0.6)
 C38B(0.4) H38D(0.4) H38E(0.4) H38F(0.4) C39(0.6) H39A(0.6) H39B(0.6) C39B(0.4)
 H39C(0.4) H39D(0.4) C40(0.6) H40A(0.6) H40B(0.6) H40C(0.6) C40B(0.4) H40D(0.4)
 H40E(0.4) H40F(0.4) O1C(0.3) O1A(0.7) O6A(0.7) O6C(0.3) C11A(0.7) H11C(0.7)
 H11D(0.7) C11C(0.3) H11E(0.3) H11F(0.3) C12A(0.7) H12D(0.7) H12E(0.7)
 H12F(0.7) C12C(0.3) H12G(0.3) H12H(0.3) H12I(0.3) C15A(0.73) H15E(0.73)
 H15F(0.73) C15C(0.27) H15G(0.27) H15H(0.27) H16G(0.73) H16H(0.73) H16I(0.73)
 H16J(0.27) H16K(0.27) H16L(0.27) C17C(0.4) H17C(0.4) H17D(0.4) C17A(0.6)
 H17E(0.6) H17F(0.6) C18C(0.25) H18D(0.25) H18E(0.25) H18F(0.25) C18A(0.75)
 H18G(0.75) H18H(0.75) H18I(0.75) H21C(0.7) H21D(0.7) H21E(0.3) H21F(0.3)
 C22A(0.7) H22G(0.7) H22H(0.7) H22I(0.7) C22C(0.3) H22J(0.3) H22K(0.3)
 H22L(0.3) H41C(0.58) H41D(0.58) H41E(0.42) H41F(0.42) C42A(0.58) H42D(0.58)
 H42E(0.58) H42F(0.58) C42C(0.42) H42G(0.42) H42H(0.42) H42I(0.42) C2S(0.8)
 H2SA(0.8) H2SB(0.8) Cl4S(0.5) Cl5S(0.5) C2SA(0.2) H2SC(0.2) H2SD(0.2)
5.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C15(H15A,H15B), C15B(H15C,H15D), C17(H17A,
 H17B), C19(H19A,H19B), C21(H21A,H21B), C31(H31A,H31B), C33(H33A,H33B),
 C33B(H33C,H33D), C35B(H35A,H35B), C35(H35C,H35D), C37B(H37A,H37B), C37(H37C,
 H37D), C39(H39A,H39B), C39B(H39C,H39D), C41(H41A,H41B), C11A(H11C,H11D),
 C11C(H11E,H11F), C13A(H13C,H13D), C15A(H15E,H15F), C15C(H15G,H15H), C17C(H17C,
 H17D), C17A(H17E,H17F), C19A(H19C,H19D), C21A(H21C,H21D), C21A(H21E,H21F),
 C31A(H31C,H31D), C33A(H33E,H33F), C35A(H35E,H35F), C37A(H37E,H37F), C39A(H39E,
 H39F), C41A(H41C,H41D), C41A(H41E,H41F), C1S(H1SA,H1SB), C2S(H2SA,H2SB),
 C2SA(H2SC,H2SD)
5.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), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66), C1A(H1A), C2A(H2A), C3A(H3A), C4A(H4A),
 C5A(H5A), C6A(H6A), C7A(H7A), C8A(H8A), C9A(H9A), C10A(H10A), C52A(H52A),
 C53A(H53A), C54A(H54A), C55A(H55A), C56A(H56A), C62A(H62A), C63A(H63A),
 C64A(H64A), C65A(H65A), C66A(H66A)
5.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C16B(H16A,H16B,H16C), C16(H16D,H16E,
 H16F), C18(H18A,H18B,H18C), C20(H20A,H20B,H20C), C22(H22A,H22B,H22C),
 C22B(H22D,H22E,H22F), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C34B(H34D,H34E,
 H34F), C36B(H36A,H36B,H36C), C36(H36D,H36E,H36F), C38(H38A,H38B,H38C),
 C38B(H38D,H38E,H38F), C40(H40A,H40B,H40C), C40B(H40D,H40E,H40F), C42(H42A,H42B,
 H42C), C12A(H12D,H12E,H12F), C12C(H12G,H12H,H12I), C14A(H14D,H14E,H14F),
 C16A(H16G,H16H,H16I), C16A(H16J,H16K,H16L), C18C(H18D,H18E,H18F), C18A(H18G,
 H18H,H18I), C20A(H20D,H20E,H20F), C22A(H22G,H22H,H22I), C22C(H22J,H22K,H22L),
 C32A(H32D,H32E,H32F), C34A(H34G,H34H,H34I), C36A(H36G,H36H,H36I), C38A(H38G,
 H38H,H38I), C40A(H40G,H40H,H40I), C42A(H42D,H42E,H42F), C42C(H42G,H42H,H42I)
;
_shelx_res_checksum              10543
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'