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_7013160
_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_sum            'C58 H66 B2 Gd2 N12 O8'
_chemical_formula_weight         1395.35
_chemical_name_common
;
Tetrakis(mu-2-
phenylbutyrate)bis(hydoridotris(pyrazolyl)borate) digadolinium(iii)
;
_chemical_name_systematic
;
Tetrakis(\m-2-phenylbutyrate)bis(hydoridotris(pyrazolyl)borate)
digadolinium(III)
;
_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
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.72(2)
_cell_angle_beta                 68.804(17)
_cell_angle_gamma                65.780(19)
_cell_formula_units_Z            1
_cell_length_a                   11.610(3)
_cell_length_b                   12.185(3)
_cell_length_c                   12.622(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.9
_cell_volume                     1518.1(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_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      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0226
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9095
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.50
_diffrn_standards_decay_%        2.83
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.228
_exptl_absorpt_correction_T_max  0.666
_exptl_absorpt_correction_T_min  0.485
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   Coppens_numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             700
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.932
_refine_diff_density_min         -2.068
_refine_diff_density_rms         0.126
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment
;
constr
except for those bound to the disordered C atoms which were not included
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         8692
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0568
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          0.042
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0745P)^2^+2.2276P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1260
_refine_ls_wR_factor_ref         0.1322
_reflns_number_gt                7521
_reflns_number_total             8692
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            b304928k.txt
_cod_data_source_block           Gd2RSpba
_cod_original_cell_volume        1518.1(6)
_cod_database_code               7013160