Design, Synthesis, and Characterization of Binuclear Ni(II) Complexes with Inherent Helical Chirality
Vadim A. Soloshonok; Hisanori Ueki; Journal of the American Chemical Society 129 (2007) 2426–2427; doi:10.1021/ja0671215

data_4109142
_publ_contact_author
; 
   Prof. Soloshonok, Vadim A.  
   Department of Chemistry and Biochemistry
   University of Oklahoma 
   620 Parrington Oval, Room 208
   Norman, OK  73019-3051  USA 
;
_publ_contact_author_email       vadim@ou.edu
_publ_contact_author_fax         1(405)3256111
_publ_contact_author_phone       1(405)3258279
_publ_section_title
;
 Design, Synthesis, and Characterization of Binuclear Ni(II) Complexes
 with Inherent Helical Chirality
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2426
_journal_page_last               2427
_journal_paper_doi               10.1021/ja0671215
_journal_volume                  129
_journal_year                    2007
_chemical_formula_moiety         'C46 H58 N6 Ni2 O2, 0.25(H2 O)'
_chemical_formula_sum            'C46 H58.5 N6 Ni2 O2.25'
_chemical_formula_weight         848.91
_chemical_melting_point          563
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.393(5)
_cell_angle_beta                 74.856(5)
_cell_angle_gamma                80.224(5)
_cell_formula_units_Z            2
_cell_length_a                   9.7788(16)
_cell_length_b                   14.374(2)
_cell_length_c                   15.608(2)
_cell_measurement_reflns_used    6178
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.28
_cell_measurement_theta_min      2.40
_cell_volume                     2085.6(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2000)'
_computing_publication_material  'SHELXTL (Sheldrick, 2000)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2000)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2000)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX'
_diffrn_measurement_method       '\w 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  0.0161
_diffrn_reflns_av_sigmaI/netI    0.0301
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            14774
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.94
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.949
_exptl_absorpt_correction_T_max  0.8477
_exptl_absorpt_correction_T_min  0.7027
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_description       prism
_exptl_crystal_F_000             901
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.424
_refine_diff_density_min         -0.281
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     514
_refine_ls_number_reflns         8145
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0281
_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^)+(0.0400P)^2^+0.9600P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0743
_refine_ls_wR_factor_ref         0.0765
_reflns_number_gt                7316
_reflns_number_total             8145
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ja0671215si20070122_063031_3.cif
_cod_data_source_block           (P/M)-7a
_cod_original_formula_sum        'C46 H58.50 N6 Ni2 O2.25'
_cod_database_code               4109142