Total spontaneous resolution of nine-coordinate complexes
Lennartson, Anders; Håkansson, Mikael; CrystEngComm 11 (2009) 1979–; doi:10.1039/b903554k

data_7201036
_publ_section_title
;
 Total spontaneous resolution of nine-coordinate complexes
;
_journal_issue                   9
_journal_name_full               CrystEngComm
_journal_page_first              1979
_journal_paper_doi               10.1039/b903554k
_journal_volume                  11
_journal_year                    2009
_chemical_formula_moiety         'C12 H24 B2 Er F8 Na5 O21'
_chemical_formula_sum            'C12 H24 B2 Er F8 Na5 O21'
_chemical_formula_weight         960.14
_chemical_name_common
;
Pentasodium tris(2,2?-oxydiacetato)-erbium(iii)
bis(tetrafluoroborate) hexahydrate
;
_chemical_name_systematic
;Pentasodium tris(2,2?-oxydiacetato)-erbium(III)
bis(tetrafluoroborate) hexahydrate
;
_space_group_IT_number           155
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      155
_symmetry_space_group_name_Hall  'R 3 2"'
_symmetry_space_group_name_H-M   'R 3 2 :H'
_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                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            3
_cell_length_a                   9.6578(15)
_cell_length_b                   9.6578(15)
_cell_length_c                   27.923(5)
_cell_measurement_reflns_used    4432
_cell_measurement_temperature    289(2)
_cell_measurement_theta_max      25.96
_cell_measurement_theta_min      4.93
_cell_volume                     2255.5(6)
_computing_cell_refinement       'CrystalClear(Rigaku, 2000)'
_computing_data_collection       'CrystalClear(Rigaku, 2000)'
_computing_data_reduction        'CrystalClear(Rigaku, 2000)'
_computing_molecular_graphics
'ORTEP-3 (Farrugia, 1997) and PLUTON (Spek, 1990)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SIR92 (Altomare et al., 1993)'
_computing_structure_solution    'CrystalClear(Rigaku, 2000)'
_diffrn_ambient_temperature      289(2)
_diffrn_detector_area_resol_mean 105
_diffrn_measured_fraction_theta_full 0.853
_diffrn_measured_fraction_theta_max 0.868
_diffrn_measurement_device_type  'Rigaku R-AXIS IIC image-plate system'
_diffrn_measurement_method       \f
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0206
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            4432
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.96
_diffrn_reflns_theta_min         4.93
_diffrn_source                   'rotating anode'
_diffrn_source_type              'Rigaku RU-H3R'
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.998
_exptl_absorpt_correction_T_max  0.5494
_exptl_absorpt_correction_T_min  0.4205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(CrystalClear; Rigaku, 2000)'
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    2.121
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1407
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.696
_refine_diff_density_min         -0.689
_refine_diff_density_rms         0.196
_refine_ls_abs_structure_details 'Flack (1983), 359 Friedel pairs'
_refine_ls_abs_structure_Flack   -0.051(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.428
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     76
_refine_ls_number_reflns         873
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.428
_refine_ls_R_factor_all          0.0163
_refine_ls_R_factor_gt           0.0149
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0458P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0403
_refine_ls_wR_factor_ref         0.0691
_reflns_number_gt                872
_reflns_number_total             873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b903554k.txt
_cod_data_source_block           1b
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               7201036