Chiral 15-Metallacrown-5 Complexes Differentially Bind Carboxylate Anions
Annabel D. Cutland; Jason A. Halfen; Jeff W. Kampf; Vincent L. Pecoraro; Journal of the American Chemical Society 123 (2001) 6211–6212; doi:10.1021/ja015610t

data_4115591
_publ_section_title
;
 Chiral 15-Metallacrown-5 Complexes Differentially Bind Carboxylate Anions
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              6211
_journal_page_last               6212
_journal_paper_doi               10.1021/ja015610t
_journal_volume                  123
_journal_year                    2001
_chemical_formula_sum            'C45 H66.5 Cu5 La N12.5 O26'
_chemical_formula_weight         1655.22
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           154
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 32 2"'
_symmetry_space_group_name_H-M   'P 32 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.0000(7)
_cell_angle_beta                 90.0000(4)
_cell_angle_gamma                120.0000(5)
_cell_formula_units_Z            6
_cell_length_a                   15.2671(2)
_cell_length_b                   15.26710(10)
_cell_length_c                   48.4117(6)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      29.50
_cell_measurement_theta_min      2.20
_cell_volume                     9772.24(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       64
_diffrn_reflns_limit_l_min       -63
_diffrn_reflns_number            121641
_diffrn_reflns_theta_full        29.50
_diffrn_reflns_theta_max         29.50
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    2.333
_exptl_absorpt_correction_T_max  0.726
_exptl_absorpt_correction_T_min  0.522
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Blessing, Acta Cryst. (1995) A51 33-38.'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.688
_exptl_crystal_description       multi-faceted
_exptl_crystal_F_000             5004
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.42
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.934
_refine_diff_density_rms         0.132
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.046(15)
_refine_ls_extinction_coef       0.00032(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.215
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     868
_refine_ls_number_reflns         17062
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.222
_refine_ls_R_factor_all          0.0559
_refine_ls_R_factor_gt           0.0541
_refine_ls_shift/su_max          0.009
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0296P)^2^+50.2542P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1239
_reflns_number_gt                16691
_reflns_number_total             17062
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja015610t_s1_1.cif
_cod_data_source_block           lacu_compound1
_cod_original_formula_sum        'C45 H66.50 Cu5 La N12.50 O26'
_cod_database_code               4115591