Tetravalent Titanium, Zirconium, and Cerium Oxo and Peroxo Complexes Containing an Imidodiphosphinate Ligand
Guo-Cang Wang; Herman H. Y. Sung; Ian D. Williams; Wa-Hung Leung; Inorganic Chemistry 51 (2012) 3640–3647; doi:10.1021/ic202564h

data_4328655
_publ_contact_author_name
;
;
_publ_section_title
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 Tetravalent Titanium, Zirconium, and Cerium Oxo and Peroxo Complexes
 Containing an Imidodiphosphinate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3640
_journal_page_last               3647
_journal_paper_doi               10.1021/ic202564h
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C48 H112 Ce2 N4 O12 P8'
_chemical_formula_sum            'C48 H112 Ce2 N4 O12 P8'
_chemical_formula_weight         1465.42
_space_group_IT_number           13
_space_group_name_Hall           '-P 2yc'
_symmetry_cell_setting           monoclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-01-30
_audit_creation_method
;
  Olex2 1.1-beta
  (compiled Nov  1 2011 20:42:30, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 112.255(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.197(8)
_cell_length_b                   13.107(7)
_cell_length_c                   18.862(10)
_cell_measurement_reflns_used    9946
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      27.658
_cell_measurement_theta_min      2.232
_cell_volume                     3477(3)
_computing_cell_refinement       'SAINT v7.34A (Bruker, 200?)'
_computing_data_collection       'SMART v5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT v7.34A (Bruker, 200?)'
_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
;
olex2.solve (L.J. Bourhis, O.V. Dolomanov, R.J. Gildea, J.A.K. Howard,
H. Puschmann, in preparation, 2011)
;
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0589
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            25716
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         1.94
_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    1.528
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.594807
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2004/1 (Bruker,2004) was used for absorption correction.
R(int) was 0.1198 before and 0.0737 after correction.
The Ratio of minimum to maximum transmission is 0.5948.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.400
_exptl_crystal_description       block
_exptl_crystal_F_000             1520
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.25
_refine_diff_density_max         1.388
_refine_diff_density_min         -0.893
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     348
_refine_ls_number_reflns         7513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0535
_refine_ls_R_factor_gt           0.0441
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0670P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1192
_reflns_number_gt                6112
_reflns_number_total             7513
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202564h_si_001_5.cif
_cod_data_source_block           wang78
_cod_database_code               4328655