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_7016086
_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 N5 O12 P3 Y, C2 H3 N'
_chemical_formula_sum            'C44 H54 N6 O12 P3 Y'
_chemical_formula_weight         1040.75
_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             2010-11-28T19:49:51-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 119.372(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   21.5641(7)
_cell_length_b                   20.9926(8)
_cell_length_c                   24.1037(8)
_cell_measurement_reflns_used    2081
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.59
_cell_measurement_theta_min      2.15
_cell_volume                     9508.8(6)
_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    SUPERFLIP
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0912
_diffrn_reflns_av_unetI/netI     0.1699
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            49562
_diffrn_reflns_theta_full        24.46
_diffrn_reflns_theta_max         24.46
_diffrn_reflns_theta_min         1.08
_exptl_absorpt_coefficient_mu    1.395
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.201
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.501
_refine_diff_density_min         -0.823
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.825
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1189
_refine_ls_number_reflns         15665
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.825
_refine_ls_R_factor_all          0.0968
_refine_ls_R_factor_gt           0.0426
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0666
_refine_ls_wR_factor_ref         0.0754
_reflns_number_gt                7722
_reflns_number_total             15665
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10194c.txt
_cod_data_source_block           ag24
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7016086