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_7011105
_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            'C61 H96 N20 Ni4 O28 S9'
_chemical_formula_weight         2080.96
_chemical_name_systematic
; 
bis[hexa(dimethylsulfoxide)(aqua)(nitrato)dinickel(II){N,N'-bis[5-(2-Pyridyl)-
4H-pyrazole-3-carbonyl]-1,2-diaminoethane(2-)}] 
trinitrate hydrate tri(dimethylsulfoxide) acetone solvate
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 90.8180(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.3586(5)
_cell_length_b                   14.3017(8)
_cell_length_c                   32.6843(17)
_cell_measurement_temperature    173(2)
_cell_volume                     4374.1(4)
_computing_molecular_graphics    OPTEP,1964
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker CCD area detector diffractometer'
_diffrn_measurement_method       'omega scan'
_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  0.0576
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            38000
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         1.25
_exptl_absorpt_coefficient_mu    1.149
_exptl_crystal_colour            'pale blue'
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2164
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.079
_refine_diff_density_min         -0.952
_refine_diff_density_rms         0.142
_refine_ls_extinction_coef       0.00027(12)
_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   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     666
_refine_ls_number_reflns         10666
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.169
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0810
_refine_ls_shift/su_max          0.013
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0273P)^2^+47.8973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2071
_refine_ls_wR_factor_ref         0.2112
_reflns_number_gt                9008
_reflns_number_total             10666
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b107593b.txt
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7011105