Synthesis and structure of tridentate bis(phosphinic amide)-phosphine oxide complexes of yttrium nitrate. Applications of (31)P,(89)Y NMR methods in structural elucidation in solution.
Popovici, Cristinel; Fernández, Ignacio; Oña-Burgos, Pascual; Roces, Laura; García-Granda, Santiago; Ortiz, Fernando López; Dalton transactions (Cambridge, England : 2003) 40 (2011) 6691–6703; doi:10.1039/c1dt10194c

data_7016084
_publ_section_title
;
 Synthesis and structure of tridentate bis(phosphinic amide)-phosphine
 oxide complexes of yttrium nitrate. Applications of (31)P,(89)Y NMR
 methods in structural elucidation in solution.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6691
_journal_page_last               6703
_journal_paper_doi               10.1039/c1dt10194c
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C42 H51 N2 O3 P3'
_chemical_formula_sum            'C42 H51 N2 O3 P3'
_chemical_formula_weight         724.76
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.4
_audit_creation_date             2010-10-12T20:51:07-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90.334(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.567(2)
_cell_length_b                   19.623(3)
_cell_length_c                   14.296(2)
_cell_measurement_temperature    150(2)
_cell_volume                     3805.9(10)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-2008 (Beurskens et al., 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.865
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0711
_diffrn_reflns_av_unetI/netI     0.1377
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            19397
_diffrn_reflns_theta_full        25
_diffrn_reflns_theta_max         25.71
_diffrn_reflns_theta_min         1.5
_exptl_absorpt_coefficient_mu    0.198
_exptl_absorpt_correction_T_max  1.1197
_exptl_absorpt_correction_T_min  0.7051
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Parkin S,Moezzi B & Hope H, (1995) J. Appl. Cryst. 28, 53-56
Linear fit to sin(theta)/lambda - 12 parameters
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.265
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1544
_exptl_crystal_size_max          0.204
_exptl_crystal_size_mid          0.174
_exptl_crystal_size_min          0.064
_refine_diff_density_max         0.349
_refine_diff_density_min         -0.341
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.877
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     451
_refine_ls_number_reflns         6271
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.877
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0446
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0005P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0572
_refine_ls_wR_factor_ref         0.0623
_reflns_number_gt                3686
_reflns_number_total             6271
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10194c.txt
_cod_data_source_block           lil2m
_cod_original_cell_volume        3806.1(10)
_cod_original_sg_symbol_Hall     '-P 2ybc '
_cod_original_sg_symbol_H-M      'P 21/c '
_cod_database_code               7016084