#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:03:05 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180057 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/03/7050386.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_7050386
loop_
_publ_author_name
'Dariusz Pawlica'
'Marek Marszałek'
'Grzegorz Mynarczuk'
'Lesław Sieroń'
'Julita Eilmes'
_publ_section_title
;
 New unsymmetrical Schiff base Ni(II) complexes as scaffolds for
 dendritic and amino acid superstructures
;
_journal_issue                   12
_journal_name_full               'New J. Chem.'
_journal_page_first              1615
_journal_page_last               1621
_journal_paper_doi               10.1039/b409298h
_journal_volume                  28
_journal_year                    2004
_chemical_formula_moiety         'C28 H25 N3 Ni O5'
_chemical_formula_sum            'C28 H25 N3 Ni O5'
_chemical_formula_weight         542.22
_chemical_name_systematic
;
[8-(3'-Ac-(D,L)-alanyloxy)-2'-hydroxyphenyl)-(5,6)-benzo
-4,7-diazaocta-2,7-dien-1-onato(2-)]nickel(II)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90
_cell_angle_beta                 96.4760(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.2759(3)
_cell_length_b                   8.43810(10)
_cell_length_c                   25.9355(3)
_cell_measurement_reflns_used    7182
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      65.61
_cell_measurement_theta_min      3.82
_cell_volume                     5061.34(11)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_type            CCD
_diffrn_measured_fraction_theta_full 0.902
_diffrn_measured_fraction_theta_max 0.902
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0089
_diffrn_reflns_av_sigmaI/netI    0.0209
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10263
_diffrn_reflns_theta_full        65.06
_diffrn_reflns_theta_max         65.06
_diffrn_reflns_theta_min         3.82
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.475
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.423
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.218
_refine_diff_density_min         -0.217
_refine_diff_density_rms         0.038
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    refU
_refine_ls_matrix_type           full
_refine_ls_number_parameters     365
_refine_ls_number_reflns         3895
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0342
_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)+(0.0607P)²+2.1850P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0992
_refine_ls_wR_factor_ref         0.1016
_reflns_number_gt                3611
_reflns_number_total             3895
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            b409298h.txt
_cod_data_source_block           6
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7050386
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ni Ni 0.071654(12) 0.76269(4) -0.002356(11) 0.04919(14) Uani 1 1 d . . .
O1 O 0.13194(5) 0.83989(18) 0.04309(5) 0.0550(3) Uani 1 1 d . . .
O2 O 0.02944(6) 0.79711(19) 0.05247(5) 0.0584(4) Uani 1 1 d . . .
O3 O 0.19771(5) 0.99506(15) 0.11776(5) 0.0508(3) Uani 1 1 d . . .
O4 O 0.23516(7) 0.75481(16) 0.13926(6) 0.0620(4) Uani 1 1 d . . .
O5 O 0.27893(7) 1.01581(17) 0.22649(6) 0.0655(4) Uani 1 1 d . . .
N1 N 0.11508(7) 0.74259(18) -0.05748(6) 0.0484(4) Uani 1 1 d . . .
N2 N 0.01020(7) 0.6835(2) -0.04778(6) 0.0531(4) Uani 1 1 d . . .
N3 N 0.21182(7) 0.8370(2) 0.24233(6) 0.0551(4) Uani 1 1 d . . .
H30 H 0.2063(10) 0.745(2) 0.2563(8) 0.051(6) Uiso 1 1 d . . .
C1 C 0.08711(8) 0.6519(2) -0.09888(7) 0.0523(4) Uani 1 1 d . . .
C2 C 0.11222(10) 0.5989(3) -0.14194(8) 0.0611(5) Uani 1 1 d . . .
H2 H 0.1501 0.6261 -0.1461 0.079(7) Uiso 1 1 calc R . .
C3 C 0.08049(11) 0.5059(3) -0.17835(9) 0.0733(6) Uani 1 1 d . . .
H3 H 0.0964 0.4736 -0.2079 0.081(8) Uiso 1 1 calc R . .
C4 C 0.02509(11) 0.4607(3) -0.17101(9) 0.0755(6) Uani 1 1 d . . .
H4A H 0.0045 0.3947 -0.1952 0.088(8) Uiso 1 1 calc R . .
C5 C -0.00016(10) 0.5118(3) -0.12840(9) 0.0679(6) Uani 1 1 d . . .
H5 H -0.0372 0.4778 -0.1235 0.072(7) Uiso 1 1 calc R . .
C6 C 0.02964(8) 0.6144(2) -0.09269(7) 0.0544(5) Uani 1 1 d . . .
C7 C 0.17919(7) 0.9018(2) 0.03002(7) 0.0468(4) Uani 1 1 d . . .
C8 C 0.21636(8) 0.9829(2) 0.06789(7) 0.0487(4) Uani 1 1 d . . .
C9 C 0.26577(8) 1.0556(3) 0.05786(8) 0.0580(5) Uani 1 1 d . . .
H9 H 0.2881 1.1107 0.0840 0.064(6) Uiso 1 1 calc R . .
C10 C 0.28308(9) 1.0475(3) 0.00804(8) 0.0629(5) Uani 1 1 d . . .
H10 H 0.3172 1.0962 0.0009 0.094(8) Uiso 1 1 calc R . .
C11 C 0.24982(8) 0.9680(2) -0.02987(7) 0.0549(5) Uani 1 1 d . . .
H11 H 0.2617 0.9620 -0.0629 0.065(6) Uiso 1 1 calc R . .
C12 C 0.19756(7) 0.8945(2) -0.02036(7) 0.0474(4) Uani 1 1 d . . .
C13 C 0.16555(8) 0.8083(2) -0.06070(7) 0.0495(4) Uani 1 1 d . . .
H13 H 0.1815 0.7974 -0.0918 0.050(5) Uiso 1 1 calc R . .
C14 C -0.02624(8) 0.8132(3) 0.04757(8) 0.0551(5) Uani 1 1 d . . .
C15 C -0.06174(9) 0.7798(3) 0.00287(9) 0.0630(6) Uani 1 1 d . . .
H15 H -0.1008 0.8025 0.0031 0.076(7) Uiso 1 1 calc R . .
C16 C -0.04523(9) 0.7154(3) -0.04276(9) 0.0606(5) Uani 1 1 d . . .
C17 C -0.09355(10) 0.6920(4) -0.08566(10) 0.0870(8) Uani 1 1 d . . .
H17A H -0.0800 0.7164 -0.1184 0.079(8) Uiso 1 1 calc R . .
H17B H -0.1252 0.7608 -0.0802 0.109(11) Uiso 1 1 calc R . .
H17C H -0.1063 0.5838 -0.0858 0.094(9) Uiso 1 1 calc R . .
C21 C -0.04960(9) 0.8764(3) 0.09438(8) 0.0582(5) Uani 1 1 d . . .
C22 C -0.10560(10) 0.8442(3) 0.10495(10) 0.0764(7) Uani 1 1 d . . .
H22 H -0.1294 0.7810 0.0822 0.143(15) Uiso 1 1 calc R . .
C23 C -0.12626(13) 0.9041(4) 0.14830(12) 0.0946(9) Uani 1 1 d . . .
H23 H -0.1637 0.8804 0.1551 0.120(11) Uiso 1 1 calc R . .
C24 C -0.09218(16) 0.9980(4) 0.18148(12) 0.0963(10) Uani 1 1 d . . .
H24 H -0.1066 1.0398 0.2106 0.124(11) Uiso 1 1 calc R . .
C25 C -0.03575(14) 1.0324(4) 0.17222(11) 0.0880(8) Uani 1 1 d . . .
H25 H -0.0123 1.0956 0.1952 0.062(6) Uiso 1 1 calc R . .
C26 C -0.01506(11) 0.9711(3) 0.12840(9) 0.0686(6) Uani 1 1 d . . .
H26 H 0.0225 0.9940 0.1218 0.064(6) Uiso 1 1 calc R . .
C30 C 0.20679(8) 0.8671(2) 0.14868(7) 0.0476(4) Uani 1 1 d . . .
C31 C 0.17465(8) 0.8830(2) 0.19599(7) 0.0522(4) Uani 1 1 d . . .
H31 H 0.1629 0.9937 0.1994 0.056(5) Uiso 1 1 calc R . .
C32 C 0.12110(10) 0.7791(3) 0.18875(10) 0.0698(6) Uani 1 1 d . . .
H32A H 0.1324 0.6699 0.1876 0.084(8) Uiso 1 1 calc R . .
H32B H 0.0983 0.8066 0.1568 0.083(8) Uiso 1 1 calc R . .
H32C H 0.0987 0.7952 0.2172 0.116(11) Uiso 1 1 calc R . .
C33 C 0.26298(9) 0.9090(2) 0.25378(8) 0.0573(5) Uani 1 1 d . . .
C34 C 0.29850(14) 0.8552(3) 0.30234(10) 0.0859(8) Uani 1 1 d . . .
H34A H 0.3371 0.8325 0.2949 0.116(12) Uiso 1 1 calc R . .
H34B H 0.2816 0.7613 0.3152 0.093(9) Uiso 1 1 calc R . .
H34C H 0.2995 0.9373 0.3281 0.137(13) 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'
O O 0.0492 0.0322 '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
O2 Ni O1 83.38(6) . . ?
O2 Ni N1 176.15(7) . . ?
O1 Ni N1 94.79(6) . . ?
O2 Ni N2 96.08(7) . . ?
O1 Ni N2 179.37(6) . . ?
N1 Ni N2 85.76(7) . . ?
C7 O1 Ni 125.52(11) . . ?
C14 O2 Ni 123.80(13) . . ?
C30 O3 C8 116.26(14) . . ?
C13 N1 C1 121.28(17) . . ?
C13 N1 Ni 125.64(14) . . ?
C1 N1 Ni 113.03(13) . . ?
C16 N2 C6 124.16(17) . . ?
C16 N2 Ni 122.95(15) . . ?
C6 N2 Ni 111.79(12) . . ?
C33 N3 C31 119.59(18) . . ?
C33 N3 H30 118.7(15) . . ?
C31 N3 H30 118.7(14) . . ?
C2 C1 C6 120.82(19) . . ?
C2 C1 N1 125.70(18) . . ?
C6 C1 N1 113.47(17) . . ?
C3 C2 C1 119.5(2) . . ?
C3 C2 H2 120.3 . . ?
C1 C2 H2 120.3 . . ?
C2 C3 C4 120.1(2) . . ?
C2 C3 H3 120.0 . . ?
C4 C3 H3 120.0 . . ?
C5 C4 C3 120.9(2) . . ?
C5 C4 H4A 119.5 . . ?
C3 C4 H4A 119.5 . . ?
C4 C5 C6 120.1(2) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 118.3(2) . . ?
C5 C6 N2 128.23(19) . . ?
C1 C6 N2 113.42(17) . . ?
O1 C7 C8 119.01(16) . . ?
O1 C7 C12 125.10(16) . . ?
C8 C7 C12 115.89(17) . . ?
C9 C8 C7 123.61(17) . . ?
C9 C8 O3 119.85(17) . . ?
C7 C8 O3 116.41(16) . . ?
C8 C9 C10 119.65(19) . . ?
C8 C9 H9 120.2 . . ?
C10 C9 H9 120.2 . . ?
C11 C10 C9 119.56(18) . . ?
C11 C10 H10 120.2 . . ?
C9 C10 H10 120.2 . . ?
C10 C11 C12 121.51(18) . . ?
C10 C11 H11 119.2 . . ?
C12 C11 H11 119.2 . . ?
C11 C12 C13 119.28(16) . . ?
C11 C12 C7 119.73(17) . . ?
C13 C12 C7 120.93(16) . . ?
N1 C13 C12 124.85(17) . . ?
N1 C13 H13 117.6 . . ?
C12 C13 H13 117.6 . . ?
O2 C14 C15 124.1(2) . . ?
O2 C14 C21 114.34(18) . . ?
C15 C14 C21 121.50(18) . . ?
C14 C15 C16 126.7(2) . . ?
C14 C15 H15 116.6 . . ?
C16 C15 H15 116.6 . . ?
N2 C16 C15 121.4(2) . . ?
N2 C16 C17 123.4(2) . . ?
C15 C16 C17 115.1(2) . . ?
C16 C17 H17A 109.5 . . ?
C16 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
C16 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C26 C21 C22 118.7(2) . . ?
C26 C21 C14 119.36(19) . . ?
C22 C21 C14 122.0(2) . . ?
C23 C22 C21 121.0(3) . . ?
C23 C22 H22 119.5 . . ?
C21 C22 H22 119.5 . . ?
C24 C23 C22 120.1(3) . . ?
C24 C23 H23 119.9 . . ?
C22 C23 H23 119.9 . . ?
C23 C24 C25 120.5(3) . . ?
C23 C24 H24 119.8 . . ?
C25 C24 H24 119.8 . . ?
C26 C25 C24 119.1(3) . . ?
C26 C25 H25 120.4 . . ?
C24 C25 H25 120.4 . . ?
C21 C26 C25 120.7(2) . . ?
C21 C26 H26 119.7 . . ?
C25 C26 H26 119.7 . . ?
O4 C30 O3 124.51(17) . . ?
O4 C30 C31 124.83(17) . . ?
O3 C30 C31 110.64(15) . . ?
N3 C31 C30 110.14(15) . . ?
N3 C31 C32 110.62(17) . . ?
C30 C31 C32 108.80(17) . . ?
N3 C31 H31 109.1 . . ?
C30 C31 H31 109.1 . . ?
C32 C31 H31 109.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
O5 C33 N3 121.57(19) . . ?
O5 C33 C34 122.2(2) . . ?
N3 C33 C34 116.2(2) . . ?
C33 C34 H34A 109.5 . . ?
C33 C34 H34B 109.5 . . ?
H34A C34 H34B 109.5 . . ?
C33 C34 H34C 109.5 . . ?
H34A C34 H34C 109.5 . . ?
H34B C34 H34C 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
Ni O2 1.8404(14) . ?
Ni O1 1.8465(13) . ?
Ni N1 1.8494(16) . ?
Ni N2 1.8708(16) . ?
O1 C7 1.297(2) . ?
O2 C14 1.295(2) . ?
O3 C30 1.348(2) . ?
O3 C8 1.414(2) . ?
O4 C30 1.195(2) . ?
O5 C33 1.229(2) . ?
N1 C13 1.310(2) . ?
N1 C1 1.416(2) . ?
N2 C16 1.339(3) . ?
N2 C6 1.421(3) . ?
N3 C33 1.340(3) . ?
N3 C31 1.452(2) . ?
N3 H30 0.87(2) . ?
C1 C2 1.391(3) . ?
C1 C6 1.401(3) . ?
C2 C3 1.377(3) . ?
C2 H2 0.9300 . ?
C3 C4 1.378(4) . ?
C3 H3 0.9300 . ?
C4 C5 1.378(3) . ?
C4 H4A 0.9300 . ?
C5 C6 1.394(3) . ?
C5 H5 0.9300 . ?
C7 C8 1.411(3) . ?
C7 C12 1.421(2) . ?
C8 C9 1.354(3) . ?
C9 C10 1.398(3) . ?
C9 H9 0.9300 . ?
C10 C11 1.358(3) . ?
C10 H10 0.9300 . ?
C11 C12 1.412(3) . ?
C11 H11 0.9300 . ?
C12 C13 1.415(3) . ?
C13 H13 0.9300 . ?
C14 C15 1.375(3) . ?
C14 C21 1.485(3) . ?
C15 C16 1.395(3) . ?
C15 H15 0.9300 . ?
C16 C17 1.503(3) . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C21 C26 1.380(3) . ?
C21 C22 1.389(3) . ?
C22 C23 1.369(4) . ?
C22 H22 0.9300 . ?
C23 C24 1.358(5) . ?
C23 H23 0.9300 . ?
C24 C25 1.392(4) . ?
C24 H24 0.9300 . ?
C25 C26 1.384(3) . ?
C25 H25 0.9300 . ?
C26 H26 0.9300 . ?
C30 C31 1.513(2) . ?
C31 C32 1.518(3) . ?
C31 H31 0.9800 . ?
C32 H32A 0.9600 . ?
C32 H32B 0.9600 . ?
C32 H32C 0.9600 . ?
C33 C34 1.497(3) . ?
C34 H34A 0.9600 . ?
C34 H34B 0.9600 . ?
C34 H34C 0.9600 . ?
