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_4330167
_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 O3 P3, 0.5(C4 H10 O)'
_chemical_formula_sum            'C46 H50 O3.5 P3'
_chemical_formula_weight         751.77
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 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                 107.6900(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.0615(5)
_cell_length_b                   19.2094(4)
_cell_length_c                   26.4506(8)
_cell_measurement_reflns_used    35385
_cell_measurement_temperature    150(1)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      2.6
_cell_volume                     8259.0(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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  0.0703
_diffrn_reflns_av_sigmaI/netI    0.0774
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            30084
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.56
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.990
_exptl_absorpt_correction_T_min  0.755
_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             3192
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.837
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.36(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     961
_refine_ls_number_reflns         12673
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0634
_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^)+(0.0987P)^2^+8.3776P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1514
_refine_ls_wR_factor_ref         0.1747
_reflns_number_gt                9621
_reflns_number_total             12673
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3010147_si_002_3.cif
_cod_data_source_block           k11178_1c
_cod_original_sg_symbol_H-M      'C c'
_cod_original_formula_sum        'C46 H50 O3.50 P3'
_cod_database_code               4330167