Complexes of Lanthanide Nitrates with Tri Tert Butylphosphine Oxide
Allen Bowden; Simon J. Coles; Mateusz B. Pitak; Andrew W. G. Platt; Inorganic Chemistry 51 (2012) 4379–4389; doi:10.1021/ic300142r

data_4328847
_publ_section_title
;
 Complexes of Lanthanide Nitrates with Tri Tert Butylphosphine Oxide
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4379
_journal_page_last               4389
_journal_paper_doi               10.1021/ic300142r
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C25 H57 Eu N3 O11.50 P2'
_chemical_formula_sum            'C25 H57 Eu N3 O11.5 P2'
_chemical_formula_weight         797.64
_chemical_name_common            Eu
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.8050(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   19.2591(2)
_cell_length_b                   27.2034(3)
_cell_length_c                   13.8018(2)
_cell_measurement_reflns_used    36275
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     7215.00(15)
_computing_cell_refinement
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_data_collection       'COLLECT (Hooft, R.W.W., 1998)'
_computing_data_reduction
'DENZO (Otwinowski & Minor, 1997) & COLLECT (Hooft, R.W.W., 1998)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean '4096x4096pixels / 62x62mm'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type
'Bruker-Nonius APEX II CCD camera on \k-goniostat'
_diffrn_measurement_method       '\f & \w scans'
_diffrn_radiation_monochromator  '10cm confocal mirrors'
_diffrn_radiation_source         'Bruker-Nonius FR591 rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0319
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            39965
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.8954
_exptl_absorpt_correction_T_min  0.8056
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/2 (Sheldrick, G.M., 2007)'
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       Prism
_exptl_crystal_F_000             3304
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.560
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.086
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.078
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     401
_refine_ls_number_reflns         8253
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0331
_refine_ls_R_factor_gt           0.0278
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0001P)^2^+27.4816P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0585
_refine_ls_wR_factor_ref         0.0618
_reflns_number_gt                7404
_reflns_number_total             8253
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic300142r_si_001_3.cif
_cod_data_source_block           Eu
_cod_original_formula_sum        'C25 H57 Eu N3 O11.50 P2'
_cod_database_code               4328847