trans-Cyclohexane-1,2-diamine Is a Weak Director of Absolute Helicity in Chiral Nickel-Salen Complexes
Zhenzhen Dong; Glenn P. A. Yap; Joseph M. Fox; Journal of the American Chemical Society 129 (2007) 11850–11853; doi:10.1021/ja073900p

data_4109955
_publ_section_title
;
 trans-Cyclohexane-1,2-diamine Is a Weak Director of Absolute Helicity in
 Chiral Nickel-Salen Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11850
_journal_page_last               11853
_journal_paper_doi               10.1021/ja073900p
_journal_volume                  129
_journal_year                    2007
_chemical_formula_sum            'C80 H97 N6 Ni O12'
_chemical_formula_weight         1393.35
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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            4
_cell_length_a                   14.797(4)
_cell_length_b                   14.844(4)
_cell_length_c                   32.462(8)
_cell_measurement_reflns_used    1019
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      19.89
_cell_measurement_theta_min      2.31
_cell_volume                     7130(3)
_computing_cell_refinement       'SHELXTL, Sheldrick (2001)'
_computing_data_collection       'SMART, Bruker (2002)'
_computing_data_reduction        'SHELXTL, Sheldrick (2001)'
_computing_molecular_graphics    'SHELXTL, Sheldrick (2001)'
_computing_publication_material  'SHELXTL, Sheldrick (2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Bruker AXS APEX diffractometer'
_diffrn_measurement_method       \w
_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  0.0676
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            80586
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         1.25
_diffrn_standards_decay_%        <1
_exptl_absorpt_coefficient_mu    0.340
_exptl_absorpt_correction_T_max  0.9604
_exptl_absorpt_correction_T_min  0.9199
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Sheldrick (2003)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.298
_exptl_crystal_description       block
_exptl_crystal_F_000             2972
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.396
_refine_diff_density_rms         0.068
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.019(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     893
_refine_ls_number_reflns         16626
_refine_ls_number_restraints     574
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0695
_refine_ls_R_factor_gt           0.0587
_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^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1485
_refine_ls_wR_factor_ref         0.1587
_reflns_number_gt                14908
_reflns_number_total             16626
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja073900psi20070522_065418.cif
_cod_data_source_block           joef038
_cod_database_code               4109955