Crystal Structure and Highly Luminescent Properties Studies of Bis-β-diketonate Lanthanide Complexes
Jing Shi; Yanjun Hou; Wenyi Chu; Xiaohong Shi; Huiquan Gu; Bilin Wang; Zhizhong Sun; Inorganic Chemistry 52 (2013) 5013–5022; doi:10.1021/ic302726z

data_4334622
_publ_section_title
;
 Crystal Structure and Highly Luminescent Properties Studies of
 Bis-\b-diketonate Lanthanide Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5013
_journal_page_last               5022
_journal_paper_doi               10.1021/ic302726z
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C62 H34 F18 N4 Sm2 O12, 2(C H2 Cl2)'
_chemical_formula_sum            'C64 H38 Cl4 F18 N4 O12 Sm2'
_chemical_formula_weight         1839.48
_chemical_name_systematic
;
bis(2,2'-Bipyridyl)-tris(\m2-1,3-bis(4,4,4-Trifluoro-3-oxido-
1-(oxo)but-2-en-1-yl)phenyl)-di-Samarium(iii) dichloromethane
 solvate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                96.92
_cell_angle_beta                 103.56
_cell_angle_gamma                91.55
_cell_formula_units_Z            2
_cell_length_a                   12.3311(4)
_cell_length_b                   15.1841(5)
_cell_length_c                   19.6059(7)
_cell_measurement_reflns_used    9871
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.2816
_cell_measurement_theta_min      2.2219
_cell_volume                     3536.8(2)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD area-detector'
_diffrn_measurement_method       '\f and \w'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0147
_diffrn_reflns_av_sigmaI/netI    0.0214
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            24337
_diffrn_reflns_theta_full        25.10
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    1.904
_exptl_absorpt_correction_T_max  0.5989
_exptl_absorpt_correction_T_min  0.5810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.727
_exptl_crystal_description       block
_exptl_crystal_F_000             1800
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.460
_refine_diff_density_min         -1.078
_refine_diff_density_rms         0.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     991
_refine_ls_number_reflns         12461
_refine_ls_number_restraints     253
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+7.6020P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0965
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                11039
_reflns_number_total             12461
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302726z_si_002_4.cif
_cod_data_source_block           complex-5
_cod_original_cell_volume        3536.7(2)
_cod_database_code               4334622