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_7038665
_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 O22 P6, 0.2(H2O)'
_chemical_formula_sum            'C46 H80.4 Ce Cl2 Co2 I2 O22.2 P6'
_chemical_formula_weight         1757.20
_chemical_name_systematic
;
 ? 
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           7
_space_group_name_Hall           'P -2yac'
_space_group_name_H-M_alt        'P 1 n 1'
_symmetry_space_group_name_Hall  'P -2yac'
_symmetry_space_group_name_H-M   'P 1 n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-02-05
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2016-02-07 deposited with the CCDC.
2016-02-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.136(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   12.0266(4)
_cell_length_b                   12.5297(4)
_cell_length_c                   21.8315(6)
_cell_measurement_reflns_used    7079
_cell_measurement_temperature    99.9(6)
_cell_measurement_theta_max      29.5310
_cell_measurement_theta_min      3.6560
_cell_volume                     3289.77(18)
_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, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.9(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 10.3587
_diffrn_detector_type            Atlas
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_details
;
  1 omega  -39.00   63.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      -12.9246   37.0000  -30.0000 102

  2 omega  -36.00   49.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -       13.3934  -85.0000   74.0000 85
;
_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      0.0260696000
_diffrn_orient_matrix_UB_12      0.0369179000
_diffrn_orient_matrix_UB_13      0.0200291000
_diffrn_orient_matrix_UB_21      -0.0121553000
_diffrn_orient_matrix_UB_22      0.0419472000
_diffrn_orient_matrix_UB_23      -0.0207689000
_diffrn_orient_matrix_UB_31      -0.0514974000
_diffrn_orient_matrix_UB_32      0.0088345000
_diffrn_orient_matrix_UB_33      0.0149720000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0677
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            25469
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.999
_diffrn_reflns_theta_min         3.657
_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    2.413
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.48640
_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    1.774
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.810
_refine_diff_density_min         -0.575
_refine_diff_density_rms         0.106
_refine_ls_abs_structure_details
;
 Flack x determined using 4470 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.019(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     720
_refine_ls_number_reflns         12972
_refine_ls_number_restraints     172
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0469
_refine_ls_R_factor_gt           0.0372
_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^)+(0.0171P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0583
_refine_ls_wR_factor_ref         0.0612
_reflns_Friedel_coverage         0.820
_reflns_Friedel_fraction_full    0.847
_reflns_Friedel_fraction_max     0.815
_reflns_number_gt                11559
_reflns_number_total             12972
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt00267f2.cif
_cod_data_source_block           ka32molt
_cod_depositor_comments
'Adding full bibliography for 7038664--7038666.cif.'
_cod_original_formula_sum        'C46 H80.40 Ce Cl2 Co2 I2 O22.20 P6'
_cod_database_code               7038665
_reflns_odcompleteness_completeness 93.37
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C14-C13
 1.52 with sigma of 0.02
 C36-C35
 1.52 with sigma of 0.02
 P4-O11 = P4-O11A = P5-O16A = P5-O16 = P5-O15 = P5-O15A = P6-O14 = P6-O14A =
 P6-O13 = P4-O12
 1.6 with sigma of 0.03
 P5-O16A = P5-O16 = P5-O15 = P5-O15A = P6-O14 = P6-O14A = P6-O13 = P4-O12 = P4-
 O11 = P4-O11A
 1.6 with sigma of 0.03
 O3-C15 \\sim O3-C15A \\sim O2-C13 \\sim O6-C21
 with sigma of 0.02
 C16A-C15A \\sim C16-C15 \\sim C18-C17 \\sim C22A-C21 \\sim C21-C22
 with sigma of 0.02
 C34-C33 \\sim C34A-C33A \\sim C36-C35 \\sim C36A-C35A \\sim C38-C37 \\sim
C38-C37A \\sim C40A-C39A ~
 C40-C39 \\sim C42-C41 \\sim C42A-C41A \\sim C32-C31 \\sim C32A-C31A
 with sigma of 0.02
 O13-C35 \\sim O13-C35A \\sim O14-C37 \\sim O14A-C37A \\sim O15-C39 \\sim
O15A-C39A \\sim O16-C41 ~
 O16A-C41A \\sim O11-C31 \\sim O11A-C31A \\sim O12-C33A \\sim O12-C33
 with sigma of 0.02
3. Others
 Fixed Sof: O11(0.6) O11A(0.4) O14(0.5) O14A(0.5) O15(0.6) O15A(0.4) O16(0.5)
 O16A(0.5) C15(0.65) C15A(0.35) C16(0.65) C16A(0.35) C22(0.65) C22A(0.35)
 C31(0.6) C31A(0.4) C32(0.6) C32A(0.4) C33(0.4) C33A(0.6) C34(0.4) C34A(0.6)
 C35(0.5) C35A(0.5) C36(0.5) C36A(0.5) C37(0.6) C37A(0.4) C39(0.6) C39A(0.4)
 C40(0.6) C40A(0.4) C41A(0.35) C41(0.65) C42A(0.35) C42(0.65) O1W(0.2)
4.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C17(H17A,H17B), C19(H19A,H19B)
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), C52(H52), C53(H53), C54(H54), C55(H55), C56(H56), C62(H62), C63(H63),
  C64(H64), C65(H65), C66(H66)
4.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C14(H14A,H14B,H14C), C18(H18A,H18B,H18C), C20(H20A,H20B,
 H20C)
;
_shelx_res_checksum              34995
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'