Crystal structure of a binuclear mixed-valence ytterbium complex containing a 2-anthracene-substituted phenoxide ligand
Berg, David J.; Twamley, Brendan; Acta Crystallographica Section E 75 (2019) 1367–1371; doi:10.1107/S205698901901154X

data_2243058
_publ_section_title
;
 Crystal structure of a binuclear mixed-valence ytterbium complex
 containing a 2-anthracene-substituted phenoxide ligand
;
_journal_issue                   9
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1367
_journal_page_last               1371
_journal_paper_doi               10.1107/S205698901901154X
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          '[Yb2 (C20 H13 O)5 (C4 H8 O)2], 3C7 H7'
_chemical_formula_moiety         'C108 H81 O7 Yb2, 3(C7 H8)'
_chemical_formula_sum            'C129 H105 O7 Yb2'
_chemical_formula_weight         2113.20
_chemical_name_systematic
'{[2-(Anthracen-9-yl)phenolato-\k<i>O</i>]bis(tetrahydrofuran)ytterbium(III)}-tris[\m-2-(anthracen-9-yl)phenolato]-\k^2^<i>O</i>:<i>O</i>;\k^2^<i>O</i>:<i>O</i>;\k<i>O</i>:1,2-\h,\k<i>O</i>]-{[2-(anthracen-9-yl)phenolato-\k<i>O</i>]ytterbium(II)} toluene trisolvate'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 95.5080(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.4612(7)
_cell_length_b                   20.8473(10)
_cell_length_c                   32.0864(15)
_cell_measurement_reflns_used    9535
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      29.714
_cell_measurement_theta_min      2.333
_cell_volume                     9628.6(8)
_computing_cell_refinement
;
SAINT (Bruker, 2002)
;
_computing_data_collection
;
SMART (Bruker, 2002)
;
_computing_data_reduction
;
SAINT (Bruker, 2002)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS (Sheldrick, 2008)
;
_diffrn_ambient_temperature      83(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  'Parallel, graphite'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0668
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            109364
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.500
_diffrn_reflns_theta_min         1.415
_diffrn_source_current           5.0
_diffrn_source_power             0.1
_diffrn_source_voltage           20.0
_exptl_absorpt_coefficient_mu    1.993
_exptl_absorpt_correction_T_max  0.8256
_exptl_absorpt_correction_T_min  0.728796
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2002)
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             4300
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.1
_refine_diff_density_max         2.199
_refine_diff_density_min         -0.927
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1480
_refine_ls_number_reflns         22107
_refine_ls_number_restraints     1509
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.0756
_refine_ls_R_factor_gt           0.0481
_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^)+(0.0460P)^2^+19.2482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1029
_refine_ls_wR_factor_ref         0.1151
_reflns_number_gt                15925
_reflns_number_total             22107
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            su5510sup1.cif
_cod_data_source_block           I
_cod_database_code               2243058
_shelx_estimated_absorpt_t_min   0.503
_shelx_estimated_absorpt_t_max   0.826
_shelx_hkl_checksum              45393
_shelx_res_checksum              11146
_cod_database_fobs_code 2243058