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_4109144
_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         'C44 H52 N6 Ni2 O3'
_chemical_formula_sum            'C44 H52 N6 Ni2 O3'
_chemical_formula_weight         830.34
_chemical_melting_point_gt       613
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.6194(11)
_cell_length_b                   21.1141(15)
_cell_length_c                   24.6763(18)
_cell_measurement_reflns_used    6234
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      2.3
_cell_volume                     8138.0(10)
_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      120(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            65404
_diffrn_reflns_theta_full        26.50
_diffrn_reflns_theta_max         27.16
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        none
_diffrn_standards_interval_count 0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.973
_exptl_absorpt_correction_T_max  0.9440
_exptl_absorpt_correction_T_min  0.8145
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Bruker(2001)SADABS,BrukerAXSInc.,Madison,WI
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.355
_exptl_crystal_description       plate
_exptl_crystal_F_000             3504
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.520
_refine_diff_density_min         -0.238
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         8998
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0421
_refine_ls_R_factor_gt           0.0315
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0430P)^2^+3.4953P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0756
_refine_ls_wR_factor_ref         0.0815
_reflns_number_gt                7486
_reflns_number_total             8998
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja0671215si20070122_063031_5.cif
_cod_data_source_block           (P/M)-7c
_cod_database_code               4109144