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_4115593
_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            'C107 H128 Cu10 Gd2 N20 O43'
_chemical_formula_weight         3332.17
_chemical_name_systematic
;
 ?
;
_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                 102.185(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.098(3)
_cell_length_b                   28.257(6)
_cell_length_c                   16.887(3)
_cell_measurement_reflns_used    7087
_cell_measurement_temperature    158(2)
_cell_measurement_theta_max      24.02
_cell_measurement_theta_min      2.16
_cell_volume                     7042(2)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      158(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_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  0.0572
_diffrn_reflns_av_sigmaI/netI    0.0720
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            60507
_diffrn_reflns_theta_full        24.77
_diffrn_reflns_theta_max         24.77
_diffrn_reflns_theta_min         1.43
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.863
_exptl_absorpt_correction_T_min  0.641
_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    1.570
_exptl_crystal_description       block
_exptl_crystal_F_000             3342
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.038
_refine_diff_density_min         -1.035
_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   -0.003(13)
_refine_ls_extinction_coef       0.00067(7)
_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   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1730
_refine_ls_number_reflns         23826
_refine_ls_number_restraints     742
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0820
_refine_ls_R_factor_gt           0.0610
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1566
_refine_ls_wR_factor_ref         0.1660
_reflns_number_gt                17837
_reflns_number_total             23826
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja015610t_s1_3.cif
_cod_data_source_block           ac1093b_compound2a
_cod_database_code               4115593