Control of molecular topology by stereochemical preferences of metal ions: double helical versus side-by-side structures in tetranuclear copper(II) and nickel(II) complexes
Roland Krämer; Igor O. Fritsky; Hans Pritzkow; Larisa A. Kovbasyuk; J. Chem. Soc., Dalton Trans.  (2002) 1307–1314; doi:10.1039/b107593b

data_7011104
_publ_section_title
;
 Control of molecular topology by stereochemical preferences of metal
 ions: double helical versus side-by-side structures in tetranuclear
 copper(II) and nickel(II) complexes
;
_journal_issue                   7
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              1307
_journal_page_last               1314
_journal_paper_doi               10.1039/b107593b
_journal_year                    2002
_chemical_formula_sum            'C120 H153 Cu12 N60 O76.5'
_chemical_formula_weight         4422.50
_chemical_name_systematic
; 
bis[di(aqua)copper(II){N,N'-bis[5-(2-Pyridyl)-4H-pyrazole-3-carbonyl]-1,2
-diaminoethane(2-)}] tetranitrate tetrahydrate
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   29.828(4)
_cell_length_b                   29.828(4)
_cell_length_c                   33.759(7)
_cell_measurement_temperature    293(2)
_cell_volume                     26012(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'P4 Bruker diffractometer'
_diffrn_measurement_method       'profile data from theta/2theta 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0622
_diffrn_reflns_limit_h_max       0
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       39
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            7214
_diffrn_reflns_theta_full        28.34
_diffrn_reflns_theta_max         28.34
_diffrn_reflns_theta_min         2.17
_exptl_absorpt_coefficient_mu    1.552
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             13518
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.028
_refine_diff_density_min         -0.668
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.835
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7214
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.835
_refine_ls_R_factor_all          0.1118
_refine_ls_R_factor_gt           0.0485
_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^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1498
_reflns_number_gt                3345
_reflns_number_total             7214
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107593b.txt
_cod_data_source_block           3b
_cod_original_sg_symbol_H-M      R-3c
_cod_original_formula_sum        'C120 H153 Cu12 N60 O76.50'
_cod_database_code               7011104