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_4326513
_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         'C88 H64 Cu2 N4 O18, 2(C4 H8 O)'
_chemical_formula_sum            'C96 H80 Cu2 N4 O20'
_chemical_formula_weight         1736.72
_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                 90.6580(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0013(8)
_cell_length_b                   23.3563(12)
_cell_length_c                   23.8248(12)
_cell_measurement_reflns_used    8701
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      20.673
_cell_measurement_theta_min      2.210
_cell_volume                     8347.1(7)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0430
_diffrn_reflns_av_sigmaI/netI    0.0597
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43700
_diffrn_reflns_theta_full        22.59
_diffrn_reflns_theta_max         22.59
_diffrn_reflns_theta_min         1.36
_exptl_absorpt_coefficient_mu    0.587
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8292
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS Version 2.05 (Bruker, 2001)'
_exptl_crystal_colour            green-blue
_exptl_crystal_density_diffrn    1.382
_exptl_crystal_description       'irregular, cleaved'
_exptl_crystal_F_000             3608
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.24
_refine_diff_density_max         0.869
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.089
_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_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1969
_refine_ls_number_reflns         22082
_refine_ls_number_restraints     442
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1387P)^2^+0.6425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1838
_refine_ls_wR_factor_ref         0.2014
_reflns_number_gt                17430
_reflns_number_total             22082
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201238n_si_002_4.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               4326513