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_4328654
_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            'C50 H117 N4 O12.5 P8 Zr2'
_chemical_formula_weight         1404.68
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.149(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.6095(14)
_cell_length_b                   24.495(3)
_cell_length_c                   21.535(2)
_cell_measurement_reflns_used    6692
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.56
_cell_measurement_theta_min      2.41
_cell_volume                     7177.6(13)
_computing_cell_refinement       'SAINT 6.0 (Bruker, 200x)'
_computing_data_collection       'SMART (Bruker, 200x)'
_computing_data_reduction        'SAINT 6.0 (Bruker, 200x)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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_sigmaI/netI    0.0638
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50506
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.42
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.521
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_description       block
_exptl_crystal_F_000             2980
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.695
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.015
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     716
_refine_ls_number_reflns         14018
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0498
_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^)+(0.0647P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                9588
_reflns_number_total             14018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202564h_si_001_4.cif
_cod_data_source_block           wang38
_cod_original_cell_volume        7177.3(13)
_cod_original_formula_sum        'C50 H117 N4 O12.50 P8 Zr2'
_cod_database_code               4328654