Control of Lanthanide Coordination Environment: Synthesis, Structure, and Oxygen-Sensitive Luminescence Properties of an Eight-Coordinate Tb(III) Complex.
Nakai, Hidetaka; Seo, Juncheol; Kitagawa, Kazuhiro; Goto, Takahiro; Nonaka, Kyoshiro; Matsumoto, Takahiro; Ogo, Seiji; Inorganic chemistry 55 (2016) 6609–6615; doi:10.1021/acs.inorgchem.6b00800

data_4347958
_publ_section_title
;
 Control of Lanthanide Coordination Environment: Synthesis, Structure, and
 Oxygen-Sensitive Luminescence Properties of an Eight-Coordinate Tb(III)
 Complex.
;
_journal_issue                   13
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6609
_journal_page_last               6615
_journal_paper_doi               10.1021/acs.inorgchem.6b00800
_journal_volume                  55
_journal_year                    2016
_chemical_absolute_configuration 'CHOOSE rm ad rmad syn or unk'
_chemical_formula_moiety         'C56 H80 N4 O4 Tb, 2(C5 H5 N)'
_chemical_formula_sum            'C66 H90 N6 O4 Tb'
_chemical_formula_weight         1190.40
_space_group_crystal_system      tetragonal
_space_group_IT_number           79
_space_group_name_Hall           'I 4'
_space_group_name_H-M_alt        'I 4'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.0000
_cell_angle_beta                 90.0000
_cell_angle_gamma                90.0000
_cell_formula_units_Z            2
_cell_length_a                   18.4142(12)
_cell_length_b                   18.4142(12)
_cell_length_c                   10.3199(9)
_cell_measurement_reflns_used    6931
_cell_measurement_temperature    108
_cell_measurement_theta_max      27.44
_cell_measurement_theta_min      3.13
_cell_volume                     3499.3(4)
_computing_cell_refinement       CrystalClear
_computing_data_collection       'CrystalClear (Rigaku Inc., 2007)'
_computing_data_reduction        CrystalClear
_computing_molecular_graphics    'CrystalStructure 4.1.1'
_computing_publication_material  'CrystalStructure 4.1.1 (Rigaku, 2015)'
_computing_structure_refinement  'SHELXL Version 2014/6 (Sheldrick, 2008)'
_computing_structure_solution    'SIR92 (Altomare, et al., 1994)'
_diffrn_ambient_temperature      108
_diffrn_detector_area_resol_mean 7.111
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Rigaku Saturn724'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0347
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14233
_diffrn_reflns_point_group_measured_fraction_full 0.967
_diffrn_reflns_point_group_measured_fraction_max 0.958
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.427
_diffrn_reflns_theta_min         3.129
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.053
_exptl_absorpt_correction_T_max  0.872
_exptl_absorpt_correction_T_min  0.680
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.130
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1250.00
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.51
_refine_diff_density_min         -0.77
_refine_ls_abs_structure_details
;
 Flack x determined using 1287 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.015(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.092
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3833
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0364
_refine_ls_R_factor_gt           0.0353
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0477P)^2^+0.1000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0918
_refine_ls_wR_factor_ref         0.0922
_reflns_Friedel_coverage         0.821
_reflns_Friedel_fraction_full    0.933
_reflns_Friedel_fraction_max     0.915
_reflns_number_gt                3717
_reflns_number_total             3833
_reflns_threshold_expression     F^2^>2.0\s(F^2^)
_cod_data_source_file            ic6b00800_si_002.cif
_cod_data_source_block           1_tBu
_cod_database_code               4347958
_shelxl_version_number           2014/6
_shelx_res_checksum              49912
_shelx_hkl_checksum              92507