Synthesis and Characterization of Chiral Tetraaza Macrocyclic Nickel(II) and Palladium(II) Complexes
Guodong Du; Arkady Ellern; L. Keith Woo; Inorganic Chemistry 42 (2003) 873–877; doi:10.1021/ic025818v

data_4313038
_publ_contact_author_address
;
  3759 Gilman Hall, Iowa State University,
  Ames, Iowa, 50011, USA
;
_publ_contact_author_email       kwoo@iastate.edu
_publ_contact_author_fax         +1-515-2945854
_publ_contact_author_name        'L. Keith Woo'
_publ_contact_author_phone       +1-515-2945854
_publ_section_title
;
 Synthesis and Characterization of Chiral Tetraaza Macrocyclic Nickel(II)
 and Palladium(II) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              873
_journal_page_last               877
_journal_paper_doi               10.1021/ic025818v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C24 H34 N4 Ni O2'
_chemical_formula_weight         469.26
_chemical_name_systematic
;
(7,16-diacetyl-1,2,3,4,4a,9a,10,11,12,13,13a,18a-dodecahydro-
5,9,14,18-tetraazadibenzo[a,h]cyclotetrdecenato) nickel(II)
;
_space_group_IT_number           1
_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                67.3100(10)
_cell_angle_beta                 75.226(2)
_cell_angle_gamma                68.5490(10)
_cell_formula_units_Z            2
_cell_length_a                   9.9537(8)
_cell_length_b                   10.9729(8)
_cell_length_c                   11.8826(9)
_cell_measurement_temperature    298(2)
_cell_volume                     1104.59(15)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      298(2)
_diffrn_measured_fraction_theta_full 0.895
_diffrn_measured_fraction_theta_max 0.895
_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  0.0286
_diffrn_reflns_av_sigmaI/netI    0.0372
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9155
_diffrn_reflns_theta_full        28.25
_diffrn_reflns_theta_max         28.25
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    0.907
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS, Bruker'
_exptl_crystal_colour            ruby
_exptl_crystal_density_diffrn    1.411
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             500
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.645
_refine_diff_density_min         -0.538
_refine_diff_density_rms         0.062
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.039(11)
_refine_ls_extinction_coef       0.0017(6)
_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   1.070
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         6732
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0382
_refine_ls_shift/su_max          0.023
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.0934
_reflns_number_gt                6009
_reflns_number_total             6732
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025818v_1.cif
_cod_data_source_block           woo13
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4313038