Tetravalent cerium pseudohalide complexes supported by the Kläui tripodal ligand [Co(η(5)-C5H5){P(O)(OEt)2}3]().
Au-Yeung, Ka-Chun; So, Yat-Ming; Sung, Herman H.-Y.; Williams, Ian D.; Leung, Wa-Hung; Dalton transactions (Cambridge, England : 2003) 45 (2016) 18163–18170; doi:10.1039/c6dt03740b

data_7041027
_publ_section_title
;
 Tetravalent cerium pseudohalide complexes supported by the Kl\"aui
 tripodal ligand [Co(\h(5)-C5H5){P(O)(OEt)2}3]().
;
_journal_issue                   45
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              18163
_journal_page_last               18170
_journal_paper_doi               10.1039/c6dt03740b
_journal_volume                  45
_journal_year                    2016
_chemical_formula_moiety         'C68 Ce4 Co4 N18 O39 P12, 0.5(C6 H14)'
_chemical_formula_sum            'C71 H147 Ce4 Co4 N18 O39 P12'
_chemical_formula_weight         3044.90
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-05-03
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2016-06-03 deposited with the CCDC.
2016-10-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.9797(3)
_cell_length_b                   20.7737(2)
_cell_length_c                   24.0697(3)
_cell_measurement_reflns_used    20847
_cell_measurement_temperature    99.9(5)
_cell_measurement_theta_max      28.9000
_cell_measurement_theta_min      3.6150
_cell_volume                     11990.3(2)
_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
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_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 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -53.00   54.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9324  -57.0000  -30.0000 214

  2 omega  -20.00   60.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9324  -99.0000  120.0000 160

  3 omega  -12.00   99.00   0.5000   20.0000
omega____ theta____ kappa____ phi______ frames
    -       17.9324   77.0000 -120.0000 222
;
_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      0.0183839000
_diffrn_orient_matrix_UB_12      0.0215052000
_diffrn_orient_matrix_UB_13      -0.0137035000
_diffrn_orient_matrix_UB_21      -0.0155422000
_diffrn_orient_matrix_UB_22      0.0265141000
_diffrn_orient_matrix_UB_23      0.0102599000
_diffrn_orient_matrix_UB_31      0.0171859000
_diffrn_orient_matrix_UB_32      0.0009539000
_diffrn_orient_matrix_UB_33      0.0239787000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            67634
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         3.177
_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    2.265
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.63226
_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    1.687
_exptl_crystal_description       block
_exptl_crystal_F_000             6124
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.571
_refine_diff_density_min         -1.298
_refine_diff_density_rms         0.135
_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     663
_refine_ls_number_reflns         11701
_refine_ls_number_restraints     60
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.0649
_refine_ls_R_factor_gt           0.0466
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0731P)^2^+35.9092P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1309
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9152
_reflns_number_total             11701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6dt03740b2.cif
_cod_data_source_block           ka35molt
_cod_depositor_comments
'Adding full bibliography for 7041024--7041027.cif.'
_cod_original_cell_volume        11990.2(2)
_cod_database_code               7041027
_chemical_oxdiff_formula         'Ce4 O3 N18 Co4 Cp4 Et24 P12 O36 '
_reflns_odcompleteness_completeness 99.68
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     27.04
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C18-C17 = C18A-C17A
 1.52 with sigma of 0.02
 C18A-C17A = C18-C17
 1.52 with sigma of 0.02
 C16-C15 = C16A-C15A
 1.52 with sigma of 0.02
 C14A-C13A = C14-C13
 1.52 with sigma of 0.02
 C20A-C19A
 1.52 with sigma of 0.02
 C20A-C19A
 1.52 with sigma of 0.02
 C22-C21 = C22A-C21A
 1.52 with sigma of 0.02
 C12-C11A = C12A-C11A
 1.52 with sigma of 0.02
 C34-C33 \\sim C34A-C33A
 with sigma of 0.02
 O5A-C19A \\sim O5-C19
 with sigma of 0.02
 C20A-C19A \\sim C20-C19
 with sigma of 0.02
 N2A-N1 \\sim N2-N1
 with sigma of 0.02
 N3A-N2A \\sim N3-N2
 with sigma of 0.02
 C22A-C21A \\sim C22-C21 \\sim C22B-C21A
 with sigma of 0.02
 C12A-C11A \\sim C12B-C11A
 with sigma of 0.02
 C32A-C31A \\sim C32-C31
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C1S) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.002
Uanis(C2) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C4) \\sim
Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of
0.003
4. Others
 Fixed Sof: N2(0.9) N2A(0.1) N3A(0.2) N3(0.8) N5A(0.4) N5(0.6) N6A(0.6)
 N6(0.4) N9(0.6) N9A(0.4) O1(0.6) O1A(0.4) O2(0.5) O2A(0.5) O3(0.55) O3A(0.45)
 O4(0.7) O4A(0.3) O5(0.7) O5A(0.3) O6(0.7) O6A(0.3) O13A(0.75) O13(0.25)
 O14A(0.4) O14(0.6) O15A(0.5) O15(0.5) O16A(0.5) O16(0.5) C11(0.5) C11A(0.5)
 C12(0.32) C12A(0.35) C12B(0.33) C13(0.3) C13A(0.7) C14(0.3) C14A(0.7) C15(0.4)
 C15A(0.6) C16(0.4) C16A(0.6) C17(0.7) C17A(0.3) C18A(0.3) C18(0.7) C19A(0.4)
 C19(0.6) C20A(0.4) C20(0.6) C21(0.5) C21A(0.5) C22(0.25) C22A(0.4) C22B(0.35)
 C31(0.66667) C31A(0.33333) C32(0.66667) C32A(0.18333) C32B(0.15) C33(0.75)
 C33A(0.25) C34(0.75) C34A(0.25) C35A(0.4) C35(0.6) C36A(0.4) C36(0.6) C37(0.7)
 C37A(0.3) C38(0.6) C38A(0.25) C38B(0.15) C39(0.45) C39B(0.12) C39A(0.43)
 C40(0.66667) C40A(0.33333) C41A(0.3) C41(0.7) C42(0.7) C42A(0.3) C1S(0.5)
 H1SA(0.5) H1SB(0.5) C2S(0.5) H2SA(0.5) H2SB(0.5) C3S(0.5) H3SA(0.5) H3SB(0.5)
 H3SC(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C1S(H1SA,H1SB), C2S(H2SA,H2SB)
5.b Idealised Me refined as rotating group:
 C3S(H3SA,H3SB,H3SC)
;
_shelx_res_checksum              80099
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'