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_4328652
_publ_section_title
;
 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_sum            'C51 H119 N4 O10 P8 Ti2'
_chemical_formula_weight         1292.06
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
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_atom_sites_solution_hydrogens   geom
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_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 92.523(3)
_cell_angle_gamma                90.00
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_cell_length_a                   13.5594(5)
_cell_length_b                   23.8906(6)
_cell_length_c                   21.9309(6)
_cell_measurement_reflns_used    11205
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      71.41
_cell_measurement_theta_min      2.73
_cell_volume                     7097.5(4)
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;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
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CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET)
(compiled Oct 25 2010,18:11:34)
;
_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    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'kappa diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3, Gemini ultra'
_diffrn_measurement_method       '\w scans'
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_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0477
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       16
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_diffrn_reflns_theta_max         67.50
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_diffrn_source_current           40
_diffrn_source_power             2.0
_diffrn_source_target            Cu
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_exptl_absorpt_coefficient_mu    4.015
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_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       plate
_exptl_crystal_F_000             2788
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.476
_refine_diff_density_min         -0.433
_refine_diff_density_rms         0.065
_refine_ls_extinction_method     none
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_refine_ls_number_reflns         12651
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_refine_ls_wR_factor_ref         0.1087
_reflns_number_gt                9644
_reflns_number_total             12651
_reflns_threshold_expression     >2sigma(I)
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