Tris(nitrato-κ^2^<i>O</i>,<i>O</i>')tris(triphenylphosphine oxide-κ<i>O</i>)terbium(III) acetone sesquisolvate
Matthews, Melissa L.; Webster, Michael; Acta Crystallographica Section E 59 (2003) m322–m323; doi:10.1107/S160053680300967X

data_2201835
_publ_section_title
;
 Tris(nitrato-\k^2^<i>O</i>,<i>O</i>')tris(triphenylphosphine
 oxide-\k<i>O</i>)terbium(III) acetone sesquisolvate
;
_journal_issue                   6
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m322
_journal_page_last               m323
_journal_paper_doi               10.1107/S160053680300967X
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Tb (N O3)3 (C18 H15 O P)3], 1.5C3 H6 O'
_chemical_formula_moiety         'C54 H45 N3 O12 P3 Tb, 1.5C3 H6 O'
_chemical_formula_sum            'C58.5 H54 N3 O13.5 P3 Tb'
_chemical_formula_weight         1266.88
_chemical_name_systematic
;
Tris(nitrato-\k^2^O,O')tris(triphenylphosphine oxide-\kO)terbium(III)
acetone solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 + hand edit'
_cell_angle_alpha                90.00
_cell_angle_beta                 94.895(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.0612(10)
_cell_length_b                   19.180(2)
_cell_length_c                   27.641(4)
_cell_measurement_reflns_used    41633
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.91
_cell_volume                     5842.8(12)
_computing_cell_refinement       'COLLECT and DENZO'
_computing_data_collection
'COLLECT (Hooft, 1998) and DENZO (Otwinowski & Minor, 1997)'
_computing_data_reduction        'COLLECT and DENZO'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.964
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Nonius rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1112
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40261
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.95
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.358
_exptl_absorpt_correction_T_max  0.873
_exptl_absorpt_correction_T_min  0.847
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SORTAV; Blessing, 1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2576
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.238
_refine_diff_density_min         -0.834
_refine_ls_extinction_coef       0.00179(16)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     711
_refine_ls_number_reflns         10247
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0194P)^2^+9.57P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1167
_refine_ls_wR_factor_ref         0.1354
_reflns_number_gt                6620
_reflns_number_total             10247
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            bt6278.cif
_cod_data_source_block           I
_cod_original_cell_volume        5842.7(12)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C58.50 H54 N3 O13.50 P3 Tb'
_cod_database_code               2201835
_cod_database_fobs_code          2201835