#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:43:47 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179125 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/87/4308723.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4308723
loop_
_publ_author_name
'Natasza Sprutta'
'Sankar Prasad Rath'
'Marilyn M. Olmstead'
'Alan L. Balch'
_publ_section_title
;
Metal Complexes of meso-Amino-octaethylporphyrin and the Oxidation of
NiII(meso-amino-octaethylporphyrin)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1452
_journal_page_last               1459
_journal_paper_doi               10.1021/ic0486623
_journal_volume                  44
_journal_year                    2005
_chemical_formula_moiety         'C36 H45 N5 Ni'
_chemical_formula_sum            'C36 H45 N5 Ni'
_chemical_formula_weight         606.48
_chemical_name_common            Ni(OEP-NH2)
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                   14.7645(12)
_cell_length_b                   14.7645(12)
_cell_length_c                   13.9225(14)
_cell_measurement_reflns_used    34
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      24.72
_cell_measurement_theta_min      4.4
_cell_volume                     3035.0(5)
_computing_cell_refinement       'Siemens P3-PC'
_computing_data_collection       'Siemens P3-PC'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'SHELXTL 5.1 (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Siemens P4'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Cu rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0348
_diffrn_reflns_av_sigmaI/netI    0.0281
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -3
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            2123
_diffrn_reflns_theta_full        56.06
_diffrn_reflns_theta_max         56.06
_diffrn_reflns_theta_min         4.36
_diffrn_standards_decay_%        1.3
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    1.172
_exptl_absorpt_correction_T_max  0.783
_exptl_absorpt_correction_T_min  0.735
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;XABS2, Parkin, S., Moezzi, B. and Hope, H. J. Appl. Crystallogr. 28 (1995)
53-56.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1296
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.139
_refine_diff_density_min         -0.315
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     104
_refine_ls_number_reflns         994
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0279P)²+3.0835P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0783
_reflns_number_gt                905
_reflns_number_total             994
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ic0486623si20050112_113330_2.cif
_cod_data_source_block           mn1432
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Tetragonal' changed to 'tetragonal'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4308723
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-y+3/4, x+1/4, z+1/4'
'y+3/4, -x+3/4, z+3/4'
'x+1/2, y+1/2, z+1/2'
'-x+1, -y+1/2, z+1'
'-y+5/4, x+3/4, z+3/4'
'y+5/4, -x+5/4, z+5/4'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'y-3/4, -x-1/4, -z-1/4'
'-y-3/4, x-3/4, -z-3/4'
'-x+1/2, -y+1/2, -z+1/2'
'x, y+1/2, -z'
'y-1/4, -x+1/4, -z+1/4'
'-y-1/4, x-1/4, -z-1/4'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni1 Ni 0.5000 0.2500 0.8750 0.0289(2) Uani 1 4 d S . .
N1 N 0.50486(11) 0.37971(11) 0.87422(11) 0.0300(4) Uani 1 1 d . . .
N2 N 0.2885(5) 0.4653(5) 0.7804(6) 0.0386(18) Uani 0.25 1 d P A 1
H2A H 0.2342 0.4445 0.7662 0.046 Uiso 0.25 1 calc PR A 1
H2B H 0.3039 0.5206 0.7636 0.046 Uiso 0.25 1 calc PR A 1
C1 C 0.57652(14) 0.43448(14) 0.89953(14) 0.0309(5) Uani 1 1 d . . .
C2 C 0.55333(15) 0.52857(14) 0.88907(14) 0.0336(5) Uani 1 1 d . . .
C3 C 0.46737(15) 0.53135(14) 0.85381(15) 0.0336(5) Uani 1 1 d . . .
C4 C 0.43648(14) 0.43888(14) 0.84708(14) 0.0311(5) Uani 1 1 d . A .
C5 C 0.34864(14) 0.41167(14) 0.82858(15) 0.0346(5) Uani 1 1 d . . .
H5A H 0.3081 0.4549 0.7989 0.041 Uiso 0.75 1 d P B 2
C6 C 0.61490(17) 0.60823(16) 0.90824(18) 0.0453(6) Uani 1 1 d . . .
H6A H 0.5772 0.6619 0.9231 0.054 Uiso 1 1 calc R . .
H6B H 0.6522 0.5949 0.9656 0.054 Uiso 1 1 calc R . .
C7 C 0.67677(17) 0.63085(18) 0.8256(2) 0.0564(7) Uani 1 1 d . . .
H7A H 0.7118 0.6853 0.8411 0.085 Uiso 1 1 calc R . .
H7B H 0.6406 0.6419 0.7678 0.085 Uiso 1 1 calc R . .
H7C H 0.7182 0.5801 0.8141 0.085 Uiso 1 1 calc R . .
C8 C 0.41372(16) 0.61407(15) 0.82811(17) 0.0414(6) Uani 1 1 d . . .
H8A H 0.4349 0.6657 0.8675 0.050 Uiso 1 1 calc R . .
H8B H 0.3491 0.6034 0.8433 0.050 Uiso 1 1 calc R . .
C9 C 0.42270(17) 0.63826(18) 0.72230(18) 0.0517(7) Uani 1 1 d . . .
H9A H 0.3846 0.6909 0.7079 0.078 Uiso 1 1 calc R . .
H9B H 0.4033 0.5867 0.6830 0.078 Uiso 1 1 calc R . .
H9C H 0.4860 0.6527 0.7078 0.078 Uiso 1 1 calc R . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni -3.0029 0.5091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N1 Ni1 N1 179.35(10) 6_554 . ?
N1 Ni1 N1 90.002(1) 6_554 16_657 ?
N1 Ni1 N1 90.002(1) . 16_657 ?
N1 Ni1 N1 90.002(1) 6_554 11_667 ?
N1 Ni1 N1 90.002(1) . 11_667 ?
N1 Ni1 N1 179.35(10) 16_657 11_667 ?
C1 N1 C4 105.00(17) . . ?
C1 N1 Ni1 127.87(14) . . ?
C4 N1 Ni1 127.13(14) . . ?
C5 N2 H2A 120.0 . . ?
C5 N2 H2B 120.0 . . ?
H2A N2 H2B 120.0 . . ?
H2A N2 H5A 130.0 . . ?
H2B N2 H5A 109.0 . . ?
N1 C1 C5 123.17(19) . 11_667 ?
N1 C1 C2 110.99(18) . . ?
C5 C1 C2 125.47(19) 11_667 . ?
C3 C2 C1 106.72(18) . . ?
C3 C2 C6 127.0(2) . . ?
C1 C2 C6 126.2(2) . . ?
C2 C3 C4 106.83(18) . . ?
C2 C3 C8 127.1(2) . . ?
C4 C3 C8 126.1(2) . . ?
C5 C4 N1 123.40(19) . . ?
C5 C4 C3 125.73(19) . . ?
N1 C4 C3 110.38(18) . . ?
N2 C5 C1 113.9(3) . 16_657 ?
N2 C5 C4 122.2(3) . . ?
C1 C5 C4 123.71(19) 16_657 . ?
C1 C5 H5A 118.3 16_657 . ?
C4 C5 H5A 117.9 . . ?
C7 C6 C2 113.7(2) . . ?
C7 C6 H6A 108.8 . . ?
C2 C6 H6A 108.8 . . ?
C7 C6 H6B 108.8 . . ?
C2 C6 H6B 108.8 . . ?
H6A C6 H6B 107.7 . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C3 C8 C9 112.10(19) . . ?
C3 C8 H8A 109.2 . . ?
C9 C8 H8A 109.2 . . ?
C3 C8 H8B 109.2 . . ?
C9 C8 H8B 109.2 . . ?
H8A C8 H8B 107.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
H9A C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ni1 N1 1.9164(16) 6_554 ?
Ni1 N1 1.9164(16) . ?
Ni1 N1 1.9164(16) 16_657 ?
Ni1 N1 1.9164(16) 11_667 ?
N1 C1 1.378(3) . ?
N1 C4 1.388(3) . ?
N2 C5 1.366(7) . ?
N2 H2A 0.8800 . ?
N2 H2B 0.8800 . ?
C1 C5 1.383(3) 11_667 ?
C1 C2 1.438(3) . ?
C2 C3 1.361(3) . ?
C2 C6 1.510(3) . ?
C3 C4 1.442(3) . ?
C3 C8 1.499(3) . ?
C4 C5 1.382(3) . ?
C5 C1 1.383(3) 16_657 ?
C5 H5A 0.9672 . ?
C6 C7 1.507(3) . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C8 C9 1.522(3) . ?
C8 H8A 0.9900 . ?
C8 H8B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
