Synthesis, X-ray structures and NIR chiroptical properties of a series of dinuclear lanthanide(III) complexes [Ln~2~{μ-(S- or RS-pba)}~4~(HBpz~3~)~2~]; novel configurational chirality due to non-bonding Ln⋯O interactions
Subhan, Md. Abdus; Suzuki, Takayoshi; Fuyuhiro, Akira; Kaizaki, Sumio; Dalton Transactions  (2003) 3785–3791; doi:10.1039/b304928k

data_7013159
_publ_section_title
;
 Synthesis, X-ray structures and NIR chiroptical properties of a series of
 dinuclear lanthanide(III) complexes [Ln~2~{\m-(S- or RS-pba)}~4~(HBpz~3~)~2~];
 novel configurational chirality due to non-bonding Ln&#x22EF;O interactions
;
_journal_coden_ASTM              DTARAF
_journal_issue                   19
_journal_name_full               'Dalton Transactions'
_journal_page_first              3785
_journal_page_last               3791
_journal_paper_doi               10.1039/b304928k
_journal_year                    2003
_chemical_formula_moiety         'C58 H64 B2 Dy2 N12 O8'
_chemical_formula_sum            'C58 H64 B2 Dy2 N12 O8'
_chemical_formula_weight         1403.83
_chemical_name_common
;
Tetrakis(mu-2-S-
phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) didysprosium(iii)
;
_chemical_name_systematic
;
Tetrakis(\m-2-S-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate)
didysprosium(III)
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 103.903(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.0708(13)
_cell_length_b                   24.8098(18)
_cell_length_c                   19.2494(18)
_cell_measurement_reflns_used    8828
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      4.7
_cell_volume                     6059.4(9)
_computing_cell_refinement       CRYSTALCLEAR
_computing_data_collection       CRYSTALCLEAR
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material  'SHELXL-97 and teXsan Ver. 1.11'
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 14.62
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'Rigaku/MSC Mercury CCD'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.1282
_diffrn_reflns_av_sigmaI/netI    0.1583
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            31781
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         4.65
_exptl_absorpt_coefficient_mu    2.510
_exptl_absorpt_correction_T_max  0.951
_exptl_absorpt_correction_T_min  0.951
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Jacobson, 1998)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.539
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.085
_refine_diff_density_min         -2.057
_refine_diff_density_rms         0.187
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.008(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1447
_refine_ls_number_reflns         25370
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.1299
_refine_ls_R_factor_gt           0.0925
_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^)+(0.0353P)^2^+50.3082P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1724
_reflns_number_gt                18715
_reflns_number_total             25370
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b304928k.txt
_cod_data_source_block           Dy2Spba
_cod_database_code               7013159