Crystal structure of tris(phenylselenolato-κ<i>Se</i>)tris(tetrahydrofuran-κ<i>O</i>)thulium(III)
Takaluoma, Esther M.; Oilunkaniemi, Raija; Lehmann, Christian W.; Laitinen, Risto S.; Acta Crystallographica Section E 70 (2014) m389–; doi:10.1107/S1600536814023733

data_2240151
_publ_section_title
;
 Crystal structure of
 tris(phenylselenolato-\k<i>Se</i>)tris(tetrahydrofuran-\k<i>O</i>)thulium(III)
;
_journal_coeditor_code           SU5009
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m389
_journal_paper_doi               10.1107/S1600536814023733
_journal_volume                  70
_journal_year                    2014
_chemical_formula_iupac          '[Tm (C6 H5 Se)3 (C4 H8 O)3]'
_chemical_formula_moiety         'C30 H39 O3 Se3 Tm'
_chemical_formula_sum            'C30 H39 O3 Se3 Tm'
_chemical_formula_weight         853.42
_chemical_name_systematic
;
Tris(phenylselenolato-\k<i>Se</i>)tris(tetrahydrofuran-\k<i>O</i>)thulium(III)
;
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_symmetry_space_group_name_Hall  'P 3 -2c'
_symmetry_space_group_name_H-M   'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   15.277(2)
_cell_length_b                   15.277(2)
_cell_length_c                   7.8708(16)
_cell_measurement_reflns_used    2053
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      28.066
_cell_measurement_theta_min      3.079
_cell_volume                     1590.8(4)
_computing_cell_refinement
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
COLLECT (Bruker, 2008)
;
_computing_data_reduction
;
DENZO-SMN (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2006)
;
_computing_publication_material
;
WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2008)
;
_computing_structure_solution
;
SIR92 (Altomare <i>et al.</i>,  1993)
;
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker--Nonius KappaCCD'
_diffrn_measurement_method       '\f scans, and \w scans with \k offsets'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            5660
_diffrn_reflns_theta_full        25.250
_diffrn_reflns_theta_max         28.066
_diffrn_reflns_theta_min         3.079
_exptl_absorpt_coefficient_mu    6.248
_exptl_absorpt_correction_T_max  0.574
_exptl_absorpt_correction_T_min  0.189
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(XPREP in SHELXTL; Sheldrick, 2008)
;
_exptl_crystal_colour            'pale yellow-green'
_exptl_crystal_density_diffrn    1.782
_exptl_crystal_description       block
_exptl_crystal_F_000             828
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.762
_refine_diff_density_min         -1.426
_refine_ls_abs_structure_details
;
Flack <i>x</i> determined using 812 quotients
[(<i>I</i>^+^)-(<i>I</i>^-^)]/[(<i>I</i>^+^)+(<i>I</i>^-^)]
(Parsons & Flack, 2004)
;
_refine_ls_abs_structure_Flack   -0.03(3)
_refine_ls_extinction_coef       0.0089(14)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL2013 (Sheldrick, 20008)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     127
_refine_ls_number_reflns         2151
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0381
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+8.3800P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0847
_refine_ls_wR_factor_ref         0.0865
_reflns_number_gt                2053
_reflns_number_total             2151
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            su5009sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        1590.9(6)
_cod_database_code               2240151
_cod_database_fobs_code          2240151
_shelx_estimated_absorpt_t_min   0.189
_shelx_estimated_absorpt_t_max   0.574
_shelx_hkl_checksum              62933
_shelx_res_checksum              93177
_shelxl_version_number           2013-4