Heterometallic Cerium(IV) Perrhenate, Permanganate, and Molybdate Complexes Supported by the Imidodiphosphinate Ligand [N(i-Pr2PO)2]-
Guo-Cang Wang; Herman H. Y. Sung; Feng-Rong Dai; Wai-Hang Chiu; Wai-Yeung Wong; Ian D. Williams; Wa-Hung Leung; Inorganic Chemistry 52 (2013) 2556–2563; doi:10.1021/ic302567e

data_4334019
_publ_section_title
;
 Heterometallic Cerium(IV) Perrhenate, Permanganate, and Molybdate
 Complexes Supported by the Imidodiphosphinate Ligand [N(i-Pr2PO)2]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2556
_journal_page_last               2563
_journal_paper_doi               10.1021/ic302567e
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C44 H86 Ce Mo2 N2 O10 P4, 0.67(H2 O)'
_chemical_formula_sum            'C44 H87.33 Ce Mo2 N2 O10.67 P4'
_chemical_formula_weight         1271.04
_chemical_name_systematic
;
 ? 
;
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-10-24
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Sep 28 2011 20:31:00, GUI svn.r3868)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 95.839(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.7983(4)
_cell_length_b                   14.1982(4)
_cell_length_c                   21.6789(4)
_cell_measurement_reflns_used    19443
_cell_measurement_temperature    173.15
_cell_measurement_theta_max      28.2500
_cell_measurement_theta_min      3.0160
_cell_volume                     5756.1(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
;
_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
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      172.9(3)
_diffrn_detector_area_resol_mean 15.9578
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_details
;
  1 omega -102.00   23.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205  -38.0000  120.0000 125

  2 omega -114.00  -35.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205 -178.0000 -120.0000 79

  3 omega  -98.00    7.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205  -57.0000   30.0000 105

  4 omega -114.00  -58.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205  178.0000   60.0000 56

  5 omega  -47.00   43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205   38.0000   90.0000 90

  6 omega  -49.00   54.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205   38.0000 -180.0000 103

  7 omega  -93.00   15.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205  -77.0000  -60.0000 108

  8 omega  -46.00   49.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -25.1205   57.0000  -90.0000 95

  9 omega  -41.00   -1.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       25.5892  131.0000  131.0000 40
;
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_UB_11      0.0538855000
_diffrn_orient_matrix_UB_12      -0.0447447000
_diffrn_orient_matrix_UB_13      -0.0037789000
_diffrn_orient_matrix_UB_21      -0.0320623000
_diffrn_orient_matrix_UB_22      -0.0425992000
_diffrn_orient_matrix_UB_23      -0.0013581000
_diffrn_orient_matrix_UB_31      -0.0010856000
_diffrn_orient_matrix_UB_32      0.0109092000
_diffrn_orient_matrix_UB_33      -0.0326431000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0371
_diffrn_reflns_av_unetI/netI     0.0212
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            33384
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         3.02
_diffrn_source                   'sealed tube'
_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Mo
_diffrn_source_voltage           50
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94753
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug  3 2011,13:03:54)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_description       block
_exptl_crystal_F_000             2611
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.665
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     302
_refine_ls_number_reflns         5638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0250
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0570P)^2^+4.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0794
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                5467
_reflns_number_total             5638
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302567e_si_001_4.cif
_cod_data_source_block           wang89
_cod_database_code               4334019
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32