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#$Date: 2016-03-23 16:19:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179371 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/68/4326870.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_4326870
loop_
_publ_author_name
'Agnieszka Wojciechowska'
'Marek Daszkiewicz'
'Zbigniew Staszak'
'Agnieszka Trusz-Zdybek'
'Alina Bieńko'
'Andrzej Ozarowski'
_publ_section_title
;
 Synthesis, Crystal Structure, Spectroscopic, Magnetic, Theoretical, and
 Microbiological Studies of a Nickel(II) Complex ofl-Tyrosine and
 Imidazole, [Ni(Im)2(l-tyr)2].4H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11532
_journal_page_last               11542
_journal_paper_doi               10.1021/ic201471f
_journal_volume                  50
_journal_year                    2011
_chemical_absolute_configuration rm
_chemical_formula_moiety         'C24 H28 N6 Ni O6, 4(H2 O)'
_chemical_formula_sum            'C24 H36 N6 Ni O10'
_chemical_formula_weight         627.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           92
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4abw 2nw'
_symmetry_space_group_name_H-M   'P 41 21 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                   9.3901(1)
_cell_length_b                   9.3901(1)
_cell_length_c                   32.1248(6)
_cell_measurement_reflns_used    2589
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      26.62
_cell_measurement_theta_min      2.89
_cell_volume                     2832.57(7)
_computing_cell_refinement       'CrysAlis 1.171.32.6'
_computing_data_collection       'CrysAlis 1.171.32.6'
_computing_data_reduction        'CrysAlis 1.171.32.6'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean '1024x1024 with blocks 2x2, 33.133pixel/mm'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'KUMA KM-4 with area CCD detector'
_diffrn_measurement_method       ω-scan
_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  0.0390
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            39102
_diffrn_reflns_theta_full        26.61
_diffrn_reflns_theta_max         26.61
_diffrn_reflns_theta_min         2.89
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.774
_exptl_absorpt_correction_T_min  0.532
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis 1.171.32.6'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_description       prism
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.38
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.161
_refine_diff_density_rms         0.039
_refine_ls_abs_structure_details
'Flack H D (1983), Acta Cryst. A39, 876-881, 1368 pairs'
_refine_ls_abs_structure_Flack   -0.019(13)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     187
_refine_ls_number_reflns         2972
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0262
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0318P)²+0.4673P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0573
_refine_ls_wR_factor_ref         0.0644
_reflns_number_gt                2589
_reflns_number_total             2972
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201471f_si_002.cif
_cod_data_source_block           ni
_cod_database_code               4326870
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-y+1/2, x+1/2, z+1/4'
'y+1/2, -x+1/2, z+3/4'
'-x+1/2, y+1/2, -z+1/4'
'x+1/2, -y+1/2, -z+3/4'
'y, x, -z'
'-y, -x, -z+1/2'
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
Ni Ni 0.07567(3) 0.07567(3) 0.0000 0.03129(10) Uani 1 2 d S
C1A C -0.2182(2) 0.0403(2) -0.02086(6) 0.0396(5) Uani 1 1 d .
O1A O -0.09734(16) 0.02086(15) -0.03763(4) 0.0412(3) Uani 1 1 d .
O2A O -0.33114(17) -0.01567(18) -0.03198(5) 0.0571(4) Uani 1 1 d .
C2A C -0.2262(2) 0.1410(2) 0.01691(6) 0.0368(5) Uani 1 1 d .
H2A H -0.2536 0.0831 0.0410 0.044 Uiso 1 1 calc R
N2A N -0.08429(18) 0.20231(17) 0.02604(5) 0.0352(4) Uani 1 1 d .
H2A1 H -0.0718 0.2078 0.0538 0.042 Uiso 1 1 calc R
H2A2 H -0.0789 0.2910 0.0155 0.042 Uiso 1 1 calc R
C3A C -0.3423(2) 0.2542(2) 0.01105(6) 0.0424(5) Uani 1 1 d .
H3A1 H -0.4329 0.2066 0.0069 0.051 Uiso 1 1 calc R
H3A2 H -0.3496 0.3099 0.0364 0.051 Uiso 1 1 calc R
C4A C -0.3166(2) 0.3539(2) -0.02499(6) 0.0364(5) Uani 1 1 d .
C5A C -0.2621(2) 0.4896(2) -0.01871(6) 0.0430(5) Uani 1 1 d .
H5A H -0.2394 0.5179 0.0082 0.052 Uiso 1 1 calc R
C6A C -0.2403(2) 0.5843(3) -0.05109(6) 0.0433(5) Uani 1 1 d .
H6A H -0.2036 0.6745 -0.0459 0.052 Uiso 1 1 calc R
C7A C -0.2738(2) 0.5430(2) -0.09135(6) 0.0382(5) Uani 1 1 d .
O7A O -0.25901(19) 0.63158(17) -0.12523(5) 0.0503(4) Uani 1 1 d .
H7A H -0.2204 0.7059 -0.1180 0.075 Uiso 1 1 calc R
C8A C -0.3261(2) 0.4082(2) -0.09844(6) 0.0419(5) Uani 1 1 d .
H8A H -0.3475 0.3796 -0.1254 0.050 Uiso 1 1 calc R
C9A C -0.3470(2) 0.3153(2) -0.06572(6) 0.0410(5) Uani 1 1 d .
H9A H -0.3822 0.2246 -0.0711 0.049 Uiso 1 1 calc R
N1B N 0.3986(2) 0.1455(2) 0.08918(5) 0.0477(5) Uani 1 1 d .
H1B H 0.4620 0.1165 0.1065 0.057 Uiso 1 1 calc R
C2B C 0.3146(2) 0.0627(3) 0.06542(6) 0.0413(5) Uani 1 1 d .
H2B H 0.3165 -0.0364 0.0655 0.050 Uiso 1 1 calc R
N3B N 0.22957(18) 0.14013(18) 0.04212(5) 0.0350(4) Uani 1 1 d .
C4B C 0.2630(2) 0.2787(2) 0.05197(6) 0.0449(5) Uani 1 1 d .
H4B H 0.2205 0.3586 0.0402 0.054 Uiso 1 1 calc R
C5B C 0.3654(3) 0.2819(3) 0.08094(7) 0.0487(6) Uani 1 1 d .
H5B H 0.4057 0.3625 0.0930 0.058 Uiso 1 1 calc R
O1W O 0.5978(2) 0.0496(2) 0.14713(5) 0.0703(5) Uani 1 1 d .
H1W1 H 0.5840 0.0991 0.1712 0.105 Uiso 1 1 d .
H2W1 H 0.5549 -0.0319 0.1540 0.105 Uiso 1 1 d .
O2W O 0.63611(17) 0.40031(18) 0.14019(5) 0.0543(4) Uani 1 1 d .
H1W2 H 0.5879 0.3971 0.1620 0.081 Uiso 1 1 d .
H2W2 H 0.6530 0.4854 0.1349 0.081 Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ni Ni 0.3393 1.1124 '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
N3B Ni N3B 91.09(9) . 7
N3B Ni O1A 173.20(6) . .
N3B Ni O1A 91.21(6) 7 .
N3B Ni O1A 91.21(6) . 7
N3B Ni O1A 173.20(6) 7 7
O1A Ni O1A 87.24(8) . 7
N3B Ni N2A 94.22(6) . .
N3B Ni N2A 94.28(6) 7 .
O1A Ni N2A 79.22(6) . .
O1A Ni N2A 91.93(6) 7 .
N3B Ni N2A 94.28(6) . 7
N3B Ni N2A 94.22(6) 7 7
O1A Ni N2A 91.93(6) . 7
O1A Ni N2A 79.22(6) 7 7
N2A Ni N2A 167.85(10) . 7
O2A C1A O1A 125.7(2) . .
O2A C1A C2A 116.50(19) . .
O1A C1A C2A 117.81(17) . .
C1A O1A Ni 114.46(12) . .
N2A C2A C3A 113.20(17) . .
N2A C2A C1A 110.53(16) . .
C3A C2A C1A 111.33(17) . .
N2A C2A H2A 107.1 . .
C3A C2A H2A 107.1 . .
C1A C2A H2A 107.1 . .
C2A N2A Ni 110.24(12) . .
C2A N2A H2A1 109.6 . .
Ni N2A H2A1 109.6 . .
C2A N2A H2A2 109.6 . .
Ni N2A H2A2 109.6 . .
H2A1 N2A H2A2 108.1 . .
C4A C3A C2A 114.22(16) . .
C4A C3A H3A1 108.7 . .
C2A C3A H3A1 108.7 . .
C4A C3A H3A2 108.7 . .
C2A C3A H3A2 108.7 . .
H3A1 C3A H3A2 107.6 . .
C9A C4A C5A 116.94(19) . .
C9A C4A C3A 121.89(19) . .
C5A C4A C3A 121.17(18) . .
C6A C5A C4A 122.36(19) . .
C6A C5A H5A 118.8 . .
C4A C5A H5A 118.8 . .
C5A C6A C7A 119.2(2) . .
C5A C6A H6A 120.4 . .
C7A C6A H6A 120.4 . .
O7A C7A C8A 117.41(18) . .
O7A C7A C6A 123.1(2) . .
C8A C7A C6A 119.48(19) . .
C7A O7A H7A 109.5 . .
C7A C8A C9A 120.39(19) . .
C7A C8A H8A 119.8 . .
C9A C8A H8A 119.8 . .
C8A C9A C4A 121.6(2) . .
C8A C9A H9A 119.2 . .
C4A C9A H9A 119.2 . .
C5B N1B C2B 107.69(19) . .
C5B N1B H1B 126.2 . .
C2B N1B H1B 126.2 . .
N3B C2B N1B 111.0(2) . .
N3B C2B H2B 124.5 . .
N1B C2B H2B 124.5 . .
C2B N3B C4B 104.72(18) . .
C2B N3B Ni 129.39(15) . .
C4B N3B Ni 125.89(14) . .
C5B C4B N3B 110.2(2) . .
C5B C4B H4B 124.9 . .
N3B C4B H4B 124.9 . .
C4B C5B N1B 106.4(2) . .
C4B C5B H5B 126.8 . .
N1B C5B H5B 126.8 . .
H1W1 O1W H2W1 99.4 . .
H1W2 O2W H2W2 108.1 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ni N3B 2.0703(16) .
Ni N3B 2.0703(16) 7
Ni O1A 2.0894(14) .
Ni O1A 2.0894(14) 7
Ni N2A 2.0905(16) .
Ni N2A 2.0905(16) 7
C1A O2A 1.236(3) .
C1A O1A 1.269(3) .
C1A C2A 1.540(3) .
C2A N2A 1.481(3) .
C2A C3A 1.535(3) .
C2A H2A 0.9800 .
N2A H2A1 0.9000 .
N2A H2A2 0.9000 .
C3A C4A 1.508(3) .
C3A H3A1 0.9700 .
C3A H3A2 0.9700 .
C4A C9A 1.388(3) .
C4A C5A 1.388(3) .
C5A C6A 1.383(3) .
C5A H5A 0.9300 .
C6A C7A 1.386(3) .
C6A H6A 0.9300 .
C7A O7A 1.377(2) .
C7A C8A 1.377(3) .
O7A H7A 0.8200 .
C8A C9A 1.380(3) .
C8A H8A 0.9300 .
C9A H9A 0.9300 .
N1B C5B 1.344(3) .
N1B C2B 1.345(3) .
N1B H1B 0.8600 .
C2B N3B 1.314(3) .
C2B H2B 0.9300 .
N3B C4B 1.375(3) .
C4B C5B 1.339(3) .
C4B H4B 0.9300 .
C5B H5B 0.9300 .
O1W H1W1 0.9128 .
O1W H2W1 0.8915 .
O2W H1W2 0.8341 .
O2W H2W2 0.8321 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N2A H2A1 O7A 0.90 2.37 3.223(2) 158.4 3
O7A H7A O2W 0.82 1.89 2.691(2) 167.1 4_464
N1B H1B O1W 0.86 1.93 2.789(3) 177.5 .
O1W H1W1 O2A 0.91 1.76 2.653(2) 165.0 3
O1W H2W1 O7A 0.89 2.43 2.999(3) 121.7 7
O2W H1W2 O1A 0.83 1.91 2.748(2) 176.3 3
O2W H2W2 O7A 0.83 2.43 3.235(2) 163.6 7_565
O2W H2W2 O1W 0.83 2.63 3.105(2) 118.1 5_655
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
O2A C1A O1A Ni -160.58(17) .
C2A C1A O1A Ni 18.8(2) .
N3B Ni O1A C1A -118.19(14) 7
O1A Ni O1A C1A 68.43(13) 7
N2A Ni O1A C1A -24.07(14) .
N2A Ni O1A C1A 147.54(14) 7
O2A C1A C2A N2A -178.76(17) .
O1A C1A C2A N2A 1.8(2) .
O2A C1A C2A C3A -52.0(2) .
O1A C1A C2A C3A 128.5(2) .
C3A C2A N2A Ni -146.52(13) .
C1A C2A N2A Ni -20.85(18) .
N3B Ni N2A C2A -154.68(12) .
N3B Ni N2A C2A 113.91(12) 7
O1A Ni N2A C2A 23.49(12) .
O1A Ni N2A C2A -63.33(12) 7
N2A Ni N2A C2A -20.38(11) 7
N2A C2A C3A C4A 61.9(2) .
C1A C2A C3A C4A -63.4(2) .
C2A C3A C4A C9A 79.9(2) .
C2A C3A C4A C5A -100.6(2) .
C9A C4A C5A C6A 0.9(3) .
C3A C4A C5A C6A -178.6(2) .
C4A C5A C6A C7A 0.0(3) .
C5A C6A C7A O7A 178.3(2) .
C5A C6A C7A C8A -0.9(3) .
O7A C7A C8A C9A -178.4(2) .
C6A C7A C8A C9A 0.9(3) .
C7A C8A C9A C4A 0.1(3) .
C5A C4A C9A C8A -1.0(3) .
C3A C4A C9A C8A 178.5(2) .
C5B N1B C2B N3B 0.4(2) .
N1B C2B N3B C4B 0.1(2) .
N1B C2B N3B Ni -179.16(13) .
N3B Ni N3B C2B -137.4(2) 7
O1A Ni N3B C2B 36.18(18) 7
N2A Ni N3B C2B 128.21(18) .
N2A Ni N3B C2B -43.10(18) 7
N3B Ni N3B C4B 43.46(15) 7
O1A Ni N3B C4B -142.94(17) 7
N2A Ni N3B C4B -50.91(17) .
N2A Ni N3B C4B 137.78(17) 7
C2B N3B C4B C5B -0.5(2) .
Ni N3B C4B C5B 178.76(14) .
N3B C4B C5B N1B 0.8(3) .
C2B N1B C5B C4B -0.7(2) .
