Tris(thiocyanato-κ<i>N</i>)tris(triphenylphosphine oxide-κ<i>O</i>)terbium(III)
Pham, Lam N.; Thames, Anthony T.; White, Frankie D.; Xiang, Kang Rui; Sykora, Richard E.; Acta Crystallographica Section E 68 (2012) m1531–; doi:10.1107/S1600536812047289

data_2236919
_publ_section_title
;
 Tris(thiocyanato-\k<i>N</i>)tris(triphenylphosphine
 oxide-\k<i>O</i>)terbium(III)
;
_journal_coeditor_code           HY2605
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1531
_journal_paper_doi               10.1107/S1600536812047289
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Tb (N C S)3 (C18 H15 O P)3]'
_chemical_formula_moiety         'C57 H45 N3 O3 P3 S3 Tb'
_chemical_formula_sum            'C57 H45 N3 O3 P3 S3 Tb'
_chemical_formula_weight         1168.01
_chemical_name_systematic
;
Tris(thiocyanato-\k<i>N</i>)tris(triphenylphosphine
oxide-\k<i>O</i>)terbium(III)
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
  Olex2 1.1
  (compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            12
_cell_length_a                   38.6774(5)
_cell_length_b                   38.6774(5)
_cell_length_c                   12.3956(2)
_cell_measurement_reflns_used    21753
_cell_measurement_temperature    180.00(10)
_cell_measurement_theta_max      25.29
_cell_measurement_theta_min      3.11
_cell_volume                     16058.8(4)
_computing_cell_refinement       'CrysAlis PRO (Agilent, 2012)'
_computing_data_collection       'CrysAlis PRO (Agilent, 2012)'
_computing_data_reduction        'CrysAlis PRO (Agilent, 2012)'
_computing_molecular_graphics    'OLEX2 (Dolomanov <i>et al.</i>, 2009)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      180.00(10)
_diffrn_detector_area_resol_mean 16.0514
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Agilent Xcalibur Eos CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0339
_diffrn_reflns_limit_h_max       46
_diffrn_reflns_limit_h_min       -46
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            79947
_diffrn_reflns_theta_full        25.35
_diffrn_reflns_theta_max         25.35
_diffrn_reflns_theta_min         3.12
_exptl_absorpt_coefficient_mu    1.574
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.913
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrysAlis PRO; Agilent, 2012)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.449
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7080
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.505
_refine_ls_abs_structure_details 'Flack (1983), 6522 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.028(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.059
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     841
_refine_ls_number_reflns         13045
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.0338
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0195P)^2^+17.3876P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0517
_refine_ls_wR_factor_ref         0.0556
_reflns_number_gt                11605
_reflns_number_total             13045
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            hy2605.cif
_cod_data_source_block           global
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               2236919