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_4330171
_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
'C44 H45 N3 O12 P3 Y, 0.25(C4 H10 O), 0.5(C2 H3 N)'
_chemical_formula_sum            'C46 H49 N3.5 O12.25 P3 Y'
_chemical_formula_weight         1028.71
_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                71.6120(13)
_cell_angle_beta                 78.2180(16)
_cell_angle_gamma                78.3240(15)
_cell_formula_units_Z            4
_cell_length_a                   12.9013(3)
_cell_length_b                   18.2387(5)
_cell_length_c                   22.5329(6)
_cell_measurement_reflns_used    77088
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      2.6
_cell_volume                     4870.7(2)
_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 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.1089
_diffrn_reflns_av_sigmaI/netI    0.1246
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            77088
_diffrn_reflns_theta_full        27.57
_diffrn_reflns_theta_max         27.57
_diffrn_reflns_theta_min         2.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.360
_exptl_absorpt_correction_T_max  0.875
_exptl_absorpt_correction_T_min  0.740
_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    1.403
_exptl_crystal_description       needle
_exptl_crystal_F_000             2126
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.225
_refine_diff_density_min         -0.514
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1143
_refine_ls_number_reflns         22201
_refine_ls_number_restraints     16
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.1500
_refine_ls_R_factor_gt           0.0761
_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^)+(0.0888P)^2^+7.0183P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1693
_refine_ls_wR_factor_ref         0.2021
_reflns_number_gt                12953
_reflns_number_total             22201
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3010147_si_002_7.cif
_cod_data_source_block           k11186_2c
_cod_original_formula_sum        'C46 H49 N3.50 O12.25 P3 Y'
_cod_database_code               4330171