Synthesis, Characterization, and Activity of Yttrium(III) Nitrate Complexes Bearing Tripodal Phosphine Oxide and Mixed Phosphine-Phosphine Oxide Ligands
Peter E. Sues; Alan J. Lough; Robert H. Morris; Inorganic Chemistry 51 (2012) 9322–9332; doi:10.1021/ic3010147

data_4330168
_publ_section_title
;
 Synthesis, Characterization, and Activity of Yttrium(III) Nitrate
 Complexes Bearing Tripodal Phosphine Oxide and Mixed Phosphine-Phosphine
 Oxide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9322
_journal_page_last               9332
_journal_paper_doi               10.1021/ic3010147
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C50 H57 O3 P3, 2(H2 O)'
_chemical_formula_sum            'C50 H61 O5 P3'
_chemical_formula_weight         834.90
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                82.379(5)
_cell_angle_beta                 79.060(5)
_cell_angle_gamma                75.520(4)
_cell_formula_units_Z            2
_cell_length_a                   8.5322(8)
_cell_length_b                   14.5956(13)
_cell_length_c                   19.4546(17)
_cell_measurement_reflns_used    17529
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      25.2
_cell_measurement_theta_min      2.6
_cell_volume                     2293.9(4)
_computing_cell_refinement       'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius B.V., 1997-2002)'
_computing_data_reduction        Denzo-SMN
_computing_molecular_graphics    'PLATON (Spek, 2009)'
_computing_publication_material  'SHELXTL V6.1'
_computing_structure_refinement  'SHELXTL V6.1 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150(1)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.924
_diffrn_measured_fraction_theta_max 0.924
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\f scans and \w scans with \k offsets'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_sigmaI/netI    0.1144
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            17529
_diffrn_reflns_theta_full        25.23
_diffrn_reflns_theta_max         25.23
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    0.175
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.841
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.209
_exptl_crystal_description       block
_exptl_crystal_F_000             892
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.280
_refine_diff_density_min         -0.417
_refine_diff_density_rms         0.061
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     535
_refine_ls_number_reflns         7649
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.016
_refine_ls_R_factor_all          0.1394
_refine_ls_R_factor_gt           0.0688
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0789P)^2^+0.6615P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1517
_refine_ls_wR_factor_ref         0.1879
_reflns_number_gt                4329
_reflns_number_total             7649
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3010147_si_002_4.cif
_cod_data_source_block           k1184_1d
_cod_database_code               4330168