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_7016085
_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         'C84 H102 N5 O9 P6 Y, C2 H3 N, 2(N O3)'
_chemical_formula_sum            'C86 H105 N8 O15 P6 Y'
_chemical_formula_weight         1765.51
_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_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             2010-12-28T22:01:06-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                74.596(2)
_cell_angle_beta                 73.845(3)
_cell_angle_gamma                62.892(3)
_cell_formula_units_Z            2
_cell_length_a                   14.831(2)
_cell_length_b                   15.879(2)
_cell_length_c                   23.473(3)
_cell_measurement_reflns_used    988
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      15.53
_cell_measurement_theta_min      2.318
_cell_volume                     4663.6(11)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker Smart'
_computing_data_reduction        'Bruker Saint'
_computing_structure_refinement  'SHELXL-97 '
_computing_structure_solution    'SHELXS-86 '
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_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  0.0547
_diffrn_reflns_av_unetI/netI     0.1739
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            24286
_diffrn_reflns_theta_full        24.45
_diffrn_reflns_theta_max         24.45
_diffrn_reflns_theta_min         0.92
_exptl_absorpt_coefficient_mu    0.792
_exptl_absorpt_correction_T_max  0.9964
_exptl_absorpt_correction_T_min  0.6352
_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    1.257
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1852
_exptl_crystal_size_max          0.422
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.178
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.804
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1016
_refine_ls_number_reflns         15189
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      0.804
_refine_ls_R_factor_all          0.1044
_refine_ls_R_factor_gt           0.0576
_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^)+(0.0469P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1201
_refine_ls_wR_factor_ref         0.1293
_reflns_number_gt                7436
_reflns_number_total             15189
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1dt10194c.txt
_cod_data_source_block           478_2m_nitrato
_cod_original_cell_volume        4663.7(11)
_cod_database_code               7016085