#------------------------------------------------------------------------------
#$Date: 2016-03-25 14:34:24 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179925 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/20/7022065.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_7022065
loop_
_publ_author_name
'Mukherjee, Tirtha'
'Costa Pessoa, João'
'Kumar, Amit'
'Sarkar, Asit R.'
_publ_section_title
;
 Synthesis, structure, magnetic properties and biological activity of
 supramolecular copper(II) and nickel(II) complexes with a Schiff base
 ligand derived from vitamin B6.
;
_journal_issue                   7
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              2594
_journal_page_last               2607
_journal_paper_doi               10.1039/c2dt31575k
_journal_volume                  42
_journal_year                    2013
_chemical_formula_moiety         'C23 H31 Cu N5 O4'
_chemical_formula_sum            'C23 H31 Cu N5 O4'
_chemical_formula_weight         505.08
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'CRYSTALS (Betteridge et al., 2003)'
_cell_angle_alpha                90
_cell_angle_beta                 121.675(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.701(6)
_cell_length_b                   7.0563(19)
_cell_length_c                   16.741(5)
_cell_measurement_reflns_used    435
_cell_measurement_temperature    293
_cell_measurement_theta_max      22.78
_cell_measurement_theta_min      4.84
_cell_volume                     2282.2(11)
_computing_cell_refinement       'SAINT 6.45 ( Bruker, 2003)'
_computing_data_collection       'SMART 5.628 (Bruker, 2003)'
_computing_data_reduction        'SAINT 6.45 ( Bruker, 2003)'
_computing_molecular_graphics    'DIAMOND 3.0(Brandenburg,199)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      293
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\j-ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.057
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8729
_diffrn_reflns_theta_full        27.040
_diffrn_reflns_theta_max         23.510
_diffrn_reflns_theta_min         2.508
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.997
_exptl_absorpt_correction_T_max  0.905
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Bruker, 2008)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.464
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rectangular
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.58
_refine_diff_density_min         -0.69
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.0615
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     155
_refine_ls_number_reflns         1670
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0736
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.0001498
_refine_ls_shift/su_mean         0.0000175
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
Method= Modified Sheldrick
w=1/[σ²(F²) + ( 0.10P)² + 0.00P]
,where P=(max(Fo²,0) + 2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1367
_refine_ls_wR_factor_ref         0.1534
_reflns_limit_h_max              23
_reflns_limit_h_min              -23
_reflns_limit_k_max              7
_reflns_limit_k_min              0
_reflns_limit_l_max              18
_reflns_limit_l_min              0
_reflns_number_gt                2075
_reflns_number_total             3169
_reflns_threshold_expression     I>0.0σ(I)
_cod_data_source_file            c2dt31575k.txt
_cod_data_source_block           1
_cod_original_cell_volume        2282.2(12)
_cod_original_sg_symbol_H-M      'C 1 2/c 1 '
_cod_database_code               7022065
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
-x,y,-z+1/2
x,-y,z+1/2
-x+1/2,y+1/2,-z+1/2
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_refinement_flags_posn
_atom_site_refinement_flags_adp
Cu1 Cu 0.5000 0.26412(10) 0.2500 0.0535 Uani 1.0000 S T
O2 O 0.56398(16) 0.2009(5) 0.3804(2) 0.0585 Uani 1.0000 . .
C3 C 0.6258(2) 0.1250(5) 0.4170(3) 0.0422 Uani 1.0000 . .
C4 C 0.6634(2) 0.1196(6) 0.3717(3) 0.0436 Uani 1.0000 . .
C5 C 0.6386(2) 0.2108(7) 0.2826(3) 0.0540 Uani 1.0000 . .
N6 N 0.5776(2) 0.2753(5) 0.2292(3) 0.0608 Uani 1.0000 . .
C7 C 0.5642(3) 0.3854(12) 0.1478(5) 0.1037 Uani 1.0000 . .
C8 C 0.5643(9) 0.589(3) 0.1644(12) 0.1798 Uani 1.0000 D .
C9 C 0.7300(2) 0.0339(6) 0.4202(3) 0.0478 Uani 1.0000 . .
C10 C 0.7542(2) -0.0321(7) 0.5081(4) 0.0571 Uani 1.0000 . .
N11 N 0.7194(2) -0.0301(5) 0.5529(3) 0.0563 Uani 1.0000 . .
C12 C 0.6562(2) 0.0453(6) 0.5078(3) 0.0514 Uani 1.0000 . .
C13 C 0.6169(3) 0.0431(10) 0.5571(4) 0.0910 Uani 1.0000 . .
C14 C 0.7732(2) 0.0029(7) 0.3770(4) 0.0617 Uani 1.0000 . .
O15 O 0.74992(17) -0.1552(5) 0.3150(2) 0.0672 Uani 1.0000 . .
N16 N 0.5000 0.5977(9) 0.2500 0.1131 Uani 1.0000 S T
C17 C 0.5693(5) 0.6546(14) 0.2590(17) 0.1705 Uani 1.0000 D .
C18 C 0.5247(13) 0.661(2) 0.3398(14) 0.1669 Uani 0.5000 . .
H51 H 0.6683 0.2212 0.2607 0.0668 Uiso 1.0000 . .
H71 H 0.6008 0.3516 0.1353 0.1268 Uiso 1.0000 . .
H72 H 0.5210 0.3503 0.0945 0.1267 Uiso 1.0000 . .
H81 H 0.6084 0.6389 0.1672 0.2212 Uiso 1.0000 . .
H82 H 0.5282 0.6478 0.1105 0.2212 Uiso 1.0000 . .
H101 H 0.7987 -0.0844 0.5399 0.0697 Uiso 1.0000 . .
H131 H 0.6457 -0.0009 0.6204 0.1329 Uiso 1.0000 . .
H132 H 0.6013 0.1690 0.5567 0.1329 Uiso 1.0000 . .
H133 H 0.5788 -0.0390 0.5254 0.1328 Uiso 1.0000 . .
H141 H 0.8222 -0.0159 0.4277 0.0748 Uiso 1.0000 . .
H142 H 0.7713 0.1137 0.3397 0.0752 Uiso 1.0000 . .
H151 H 0.7633 -0.2367 0.3574 0.1017 Uiso 1.0000 . .
H171 H 0.6108 0.6074 0.3278 0.4910 Uiso 1.00000 . .
H172 H 0.5769 0.8000 0.2822 0.4910 Uiso 1.0000 . .
H181 H 0.4811 0.6400 0.3537 0.1961 Uiso 0.5000 . .
H182 H 0.5288 0.7952 0.3517 0.1961 Uiso 0.5000 . .
H183 H 0.5583 0.5954 0.3912 0.1961 Uiso 0.5000 . .
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 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C 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
N6 Cu1 O2 89.86(15) 5_655 5_655 yes
N6 Cu1 O2 91.20(15) 5_655 . yes
O2 Cu1 O2 153.4(2) 5_655 . yes
N6 Cu1 N6 175.4(2) 5_655 . yes
O2 Cu1 N6 91.20(16) 5_655 . yes
O2 Cu1 N6 89.86(15) . . yes
N6 Cu1 N16 87.69(12) 5_655 . yes
O2 Cu1 N16 103.32(11) 5_655 . yes
O2 Cu1 N16 103.32(11) . . yes
N6 Cu1 N16 87.69(12) . . yes
Cu1 O2 C3 127.2(3) . . yes
O2 C3 C4 124.0(4) . . yes
O2 C3 C12 117.6(4) . . yes
C4 C3 C12 118.4(4) . . yes
C3 C4 C5 121.9(4) . . yes
C3 C4 C9 117.8(4) . . yes
C5 C4 C9 120.1(4) . . yes
C4 C5 N6 125.1(4) . . yes
C4 C5 H51 118.5 . . no
N6 C5 H51 116.4 . . no
C5 N6 Cu1 127.3(3) . . yes
C5 N6 C7 117.5(4) . . yes
Cu1 N6 C7 114.9(3) . . yes
N6 C7 C8 111.5(9) . . yes
N6 C7 H71 106.5 . . no
C8 C7 H71 111.1 . . no
N6 C7 H72 110.2 . . no
C8 C7 H72 109.4 . . no
H71 C7 H72 108.0 . . no
C7 C8 C17 117.7(8) . . yes
C7 C8 H81 104.2 . . no
C17 C8 H81 107.1 . . no
C7 C8 H82 109.6 . . no
C17 C8 H82 113.5 . . no
H81 C8 H82 103.3 . . no
C4 C9 C10 118.0(4) . . yes
C4 C9 C14 123.5(4) . . yes
C10 C9 C14 118.4(4) . . yes
C9 C10 N11 125.4(4) . . yes
C9 C10 H101 117.1 . . no
N11 C10 H101 117.5 . . no
C10 N11 C12 117.5(4) . . yes
C3 C12 N11 122.8(4) . . yes
C3 C12 C13 119.9(4) . . yes
N11 C12 C13 117.3(4) . . yes
C12 C13 H131 110.8 . . no
C12 C13 H132 108.2 . . no
H131 C13 H132 110.0 . . no
C12 C13 H133 109.5 . . no
H131 C13 H133 108.3 . . no
H132 C13 H133 109.9 . . no
C9 C14 O15 112.2(4) . . yes
C9 C14 H141 109.1 . . no
O15 C14 H141 109.9 . . no
C9 C14 H142 111.4 . . no
O15 C14 H142 106.5 . . no
H141 C14 H142 107.6 . . no
C14 O15 H151 95.1 . . no
C17 N16 Cu1 105.0(5) 5_655 . yes
C17 N16 C18 90.0(13) 5_655 5_655 yes
Cu1 N16 C18 108.9(8) . 5_655 yes
C17 N16 C17 150.0(10) 5_655 . yes
Cu1 N16 C17 105.0(5) . . yes
C18 N16 C17 80.4(12) 5_655 . yes
C17 N16 C18 80.4(12) 5_655 . yes
Cu1 N16 C18 108.9(8) . . yes
C18 N16 C18 142.3(16) 5_655 . yes
C17 N16 C18 90.0(13) . . yes
N16 C17 C8 106.8(11) . . yes
N16 C17 H171 107.2 . . no
C8 C17 H171 122.1 . . no
N16 C17 H172 104.2 . . no
C8 C17 H172 123.1 . . no
H171 C17 H172 91.4 . . no
N16 C18 H181 106.5 . . no
N16 C18 H182 119.0 . . no
H181 C18 H182 94.8 . . no
N16 C18 H183 121.6 . . no
H181 C18 H183 97.4 . . no
H182 C18 H183 110.9 . . no
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
Cu1 N6 1.968(4) 5_655 yes
Cu1 O2 1.935(3) 5_655 yes
Cu1 O2 1.935(3) . yes
Cu1 N6 1.968(4) . yes
Cu1 N16 2.354(6) . yes
O2 C3 1.314(5) . yes
C3 C4 1.410(6) . yes
C3 C12 1.414(6) . yes
C4 C5 1.440(6) . yes
C4 C9 1.422(6) . yes
C5 N6 1.275(6) . yes
C5 H51 0.923 . no
N6 C7 1.456(7) . yes
C7 C8 1.47(2) . yes
C7 H71 0.986 . no
C7 H72 0.948 . no
C8 C17 1.596(19) . yes
C8 H81 1.038 . no
C8 H82 0.938 . no
C9 C10 1.355(7) . yes
C9 C14 1.510(7) . yes
C10 N11 1.345(6) . yes
C10 H101 0.936 . no
N11 C12 1.331(6) . yes
C12 C13 1.500(7) . yes
C13 H131 0.960 . no
C13 H132 0.956 . no
C13 H133 0.940 . no
C14 O15 1.423(6) . yes
C14 H141 0.993 . no
C14 H142 0.987 . no
O15 H151 0.838 . no
N16 C17 1.552(16) 5_655 yes
N16 C18 1.374(18) 5_655 yes
N16 C17 1.552(16) . yes
N16 C18 1.374(18) . yes
C17 H171 1.089 . no
C17 H172 1.078 . no
C18 H181 1.137 . no
C18 H182 0.964 . no
C18 H183 0.919 . no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
O15 . H151 N11 4_646 169.6(3) 0.838 2.120 2.948(13) yes
C18 . H181 C7 5_655 126.2(7) 1.137 2.064 2.885(13) yes
C8 5_655 H181 C18 . 150.8(11) 0.978 1.137 2.046(13) yes
