Synthesis and optical resolution of a Cu(I) double-stranded helicate with ketimine-bridged tris(bipyridine) ligands
Yoshio Furusho; Hidetoshi Goto; Ken Itomi; Hiroshi Katagiri; Toyoharu Miyagawa; Eiji Yashima; Chem.Commun. 47 (2011) 9795–; doi:10.1039/c1cc13333k

data_7106800
_publ_section_title
;
 Synthesis and optical resolution of a Cu(I) double-stranded helicate with
 ketimine-bridged tris(bipyridine) ligands
;
_journal_name_full               Chem.Commun.
_journal_page_first              9795
_journal_paper_doi               10.1039/c1cc13333k
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         '(C88 H92 N16 Cu4) 4(P F6) (H2 O)'
_chemical_formula_sum            'C88 H92 Cu4 F24 N16 O P4'
_chemical_formula_weight         2225.86
_chemical_name_systematic
;
?
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/c 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                 107.539(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   32.027(9)
_cell_length_b                   11.894(3)
_cell_length_c                   24.907(7)
_cell_measurement_reflns_used    5087
_cell_measurement_temperature    90
_cell_measurement_theta_max      24.88
_cell_measurement_theta_min      2.18
_cell_volume                     9047(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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      90
_diffrn_detector_area_resol_mean 8.333
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0972
_diffrn_reflns_av_sigmaI/netI    0.1247
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            35152
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  0.9890
_exptl_absorpt_correction_T_min  0.5567
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS Sheldrick 1996
;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.635
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             4528
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.302
_refine_diff_density_min         -2.109
_refine_diff_density_rms         0.181
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.168
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1235
_refine_ls_number_reflns         12956
_refine_ls_number_restraints     1872
_refine_ls_restrained_S_all      1.099
_refine_ls_R_factor_all          0.1791
_refine_ls_R_factor_gt           0.1338
_refine_ls_shift/su_max          0.017
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0221P)^2^+389.8422P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2857
_refine_ls_wR_factor_ref         0.3032
_reflns_number_gt                8687
_reflns_number_total             12956
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc13333k.txt
_cod_data_source_block           pc
_cod_original_sg_symbol_H-M      P2/c
_cod_database_code               7106800