Syntheses and Characterization of Copper(II) Carboxylate Dimers Formed from Enantiopure Ligands Containing a Strong π...π Stacking Synthon: Enantioselective Single-Crystal to Single-Crystal Gas/Solid-Mediated Transformations
Daniel L. Reger; Jacob J. Horger; Agota Debreczeni; Mark D. Smith; Inorganic Chemistry 50 (2011) 10225–10240; doi:10.1021/ic201238n

data_4326516
_publ_contact_author_address
;
Department of Chemistry and Biochemistry
University of South Carolina
Columbia, South Carolina 29208
USA
;
_publ_contact_author_email       reger@mail.chem.sc.edu
_publ_contact_author_fax         '1 803 777 9521'
_publ_contact_author_name        'Professor Daniel L. Reger'
_publ_contact_author_phone       '1 803 777 2587'
_publ_section_title
;
 Syntheses and Characterization of Copper(II) Carboxylate Dimers Formed
 from Enantiopure Ligands Containing a Strong \p...\p Stacking Synthon:
 Enantioselective Single-Crystal to Single-Crystal Gas/Solid-Mediated
 Transformations
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10225
_journal_page_last               10240
_journal_paper_doi               10.1021/ic201238n
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C136.32 H100.48 Cu4 N17 O42.16'
_chemical_formula_sum            'C136.32 H100.48 Cu4 N17 O42.16'
_chemical_formula_weight         2905.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.250(2)
_cell_length_b                   21.548(3)
_cell_length_c                   52.359(7)
_cell_measurement_reflns_used    7850
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      19.190
_cell_measurement_theta_min      2.258
_cell_volume                     17206(4)
_computing_cell_refinement       'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_data_collection       'SMART Version 5.625 (Bruker, 2001)'
_computing_data_reduction        'SAINT-Plus Version 6.45 (Bruker, 2001)'
_computing_molecular_graphics    various
_computing_publication_material  'SHELXTL Version 6.14 (Bruker, 2000)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker SMART APEX CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1064
_diffrn_reflns_av_sigmaI/netI    0.0654
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       60
_diffrn_reflns_limit_l_min       -60
_diffrn_reflns_number            232763
_diffrn_reflns_theta_full        24.25
_diffrn_reflns_theta_max         24.25
_diffrn_reflns_theta_min         1.02
_exptl_absorpt_coefficient_mu    0.559
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.7968
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.122
_exptl_crystal_description       'rectangular bar'
_exptl_crystal_F_000             5963
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.859
_refine_diff_density_min         -0.486
_refine_diff_density_rms         0.104
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.089(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     787
_refine_ls_number_reflns         27766
_refine_ls_number_restraints     995
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0979
_refine_ls_R_factor_gt           0.0800
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1451P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2106
_refine_ls_wR_factor_ref         0.2215
_reflns_number_gt                21452
_reflns_number_total             27766
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201238n_si_002_7.cif
_cod_data_source_block           7
_cod_database_code               4326516