Acetamide Coordination in a Nickel(I) Macrocyclic Complex: Synthesis, Properties, and X-ray Crystal Structure of a Five-Coordinate Nickel(I) Iminol Complex of 1,3,6,8,12,15-Hexaazatricyclo[13.3.1.18,12]icosane
Myunghyun Paik Suh; Kye Young Oh; Jae Woo Lee; Yeon Young Bae; Journal of the American Chemical Society 118 (1996) 777–783; doi:10.1021/ja953106g

data_4117104
_publ_contact_author
;
   Prof. Myunghyun Paik Suh
   Department of Chemistry Education and
   Center for Molecular Catalysis,
   Seoul National University,
   Seoul 151-742, Korea
;
_publ_section_title
;
 Acetamide Coordination in a Nickel(I) Macrocyclic Complex: Synthesis,
 Properties, and X-ray Crystal Structure of a Five-Coordinate Nickel(I)
 Iminol Complex of 1,3,6,8,12,15-Hexaazatricyclo[13.3.1.18,12]icosane
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              777
_journal_page_last               783
_journal_paper_doi               10.1021/ja953106g
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C16 H35 Cl N7 Ni O5'
_chemical_formula_weight         499.67
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.053(5)
_cell_length_b                   14.120(3)
_cell_length_c                   31.005(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4401(2)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2153
_diffrn_reflns_theta_max         24.94
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    1.046
_exptl_absorpt_correction_T_max  1.716
_exptl_absorpt_correction_T_min  0.753
_exptl_absorpt_correction_type   refdelf
_exptl_crystal_density_diffrn    1.508
_exptl_crystal_F_000             2120
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.323
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.104
_refine_ls_goodness_of_fit_obs   1.111
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         2153
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_restrained_S_obs      1.111
_refine_ls_R_factor_all          0.0500
_refine_ls_R_factor_obs          0.0447
_refine_ls_shift/esd_max         0.095
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.7053P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0983
_refine_ls_wR_factor_obs         0.0953
_reflns_number_observed          2025
_reflns_number_total             2153
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja953106g.cif
_cod_data_source_block           Ni
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.7053P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0493P)^2^+1.7053P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        4401.1(24)
_cod_database_code               4117104