#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/72/2017209.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2017209
loop_
_publ_author_name
'Shi, Wen-Juan'
_publ_section_title
;
 The chiral helical structure of a copper(II) complex with a tridentate
 Schiff base ligand
;
_journal_coeditor_code           BM3081
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m284
_journal_page_last               m286
_journal_paper_doi               10.1107/S010827010902575X
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Cu (C9 H9 N2 O2) (H2 O)] Cl O4'
_chemical_formula_moiety         'C9 H11 Cu N2 O3 +, Cl O4 -'
_chemical_formula_sum            'C9 H11 Cl Cu N2 O7'
_chemical_formula_weight         358.19
_chemical_name_systematic
;catena-poly[[[aquacopper(II)]-μ-3-(2-pyridylmethyleneamino)propanoato-
κ⁴N,N',O:O']
 perchlorate]
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   7.9552(13)
_cell_length_b                   11.6740(19)
_cell_length_c                   14.050(2)
_cell_measurement_reflns_used    1230
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.31
_cell_measurement_theta_min      2.26
_cell_volume                     1304.8(4)
_computing_cell_refinement       'SAINT (Bruker, 2002)'
_computing_data_collection       'SMART (Bruker, 2002)'
_computing_data_reduction        'SAINT (Bruker, 2002)'
_computing_molecular_graphics
'SHELXTL (Sheldrick, 2008) and DIAMOND (Brandenburg & Berndt, 2005)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type
;
Bruker SMART APEX CCD area-detector
;
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0338
_diffrn_reflns_av_sigmaI/netI    0.0609
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -5
_diffrn_reflns_number            5173
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.27
_exptl_absorpt_coefficient_mu    1.911
_exptl_absorpt_correction_T_max  0.8318
_exptl_absorpt_correction_T_min  0.7757
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.823
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             724
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.48
_refine_diff_density_min         -0.34
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.02(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0640
_refine_ls_R_factor_gt           0.0540
_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)+(0.0694P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1222
_refine_ls_wR_factor_ref         0.1289
_reflns_number_gt                2092
_reflns_number_total             2457
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            bm3081.cif
_cod_data_source_block           I
_cod_database_code               2017209
_cod_database_fobs_code          2017209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
Cu Cu1 0.80083(9) 0.64574(5) 0.94224(5) 0.0439(2) Uani . . 1.000
O O1 1.0294(5) 0.6929(3) 0.9762(3) 0.0483(14) Uani . . 1.000
O O1W 0.7201(6) 0.6400(4) 1.1065(3) 0.0657(16) Uani . . 1.000
O O2 1.2467(5) 0.6917(3) 1.0726(3) 0.0493(14) Uani . . 1.000
N N1 0.5962(7) 0.5794(4) 0.8811(3) 0.0483(17) Uani . . 1.000
N N2 0.8664(6) 0.4825(4) 0.9459(4) 0.0507(16) Uani . . 1.000
C C1 0.6040(9) 0.4641(6) 0.8758(4) 0.0517(19) Uani . . 1.000
C C2 0.4783(10) 0.4004(6) 0.8334(4) 0.063(3) Uani . . 1.000
C C3 0.3409(11) 0.4559(8) 0.7964(5) 0.073(3) Uani . . 1.000
C C4 0.3310(9) 0.5737(7) 0.8026(4) 0.065(3) Uani . . 1.000
C C5 0.4637(8) 0.6324(7) 0.8454(4) 0.058(2) Uani . . 1.000
C C6 0.7563(8) 0.4143(5) 0.9142(4) 0.053(2) Uani . . 1.000
C C7 1.0267(8) 0.4425(5) 0.9810(5) 0.059(2) Uani . . 1.000
C C8 1.0949(8) 0.5176(5) 1.0593(5) 0.054(2) Uani . . 1.000
C C9 1.1272(7) 0.6422(5) 1.0337(4) 0.0407(17) Uani . . 1.000
Cl Cl1 0.5922(2) 0.34785(15) 1.17237(12) 0.0586(5) Uani . . 1.000
O O3 0.5761(11) 0.4523(6) 1.2184(5) 0.131(3) Uani . . 1.000
O O4 0.7570(9) 0.3329(8) 1.1422(6) 0.139(4) Uani . . 1.000
O O5 0.4878(11) 0.3482(7) 1.0954(6) 0.136(3) Uani . . 1.000
O O6 0.5478(11) 0.2652(7) 1.2362(7) 0.158(4) Uani . . 1.000
H H1WB 0.63220 0.68030 1.11430 0.0990 Uiso . R 1.000
H H2 0.48650 0.32100 0.83000 0.0760 Uiso calc R 1.000
H H1WA 0.70010 0.57130 1.12290 0.0990 Uiso . R 1.000
H H3 0.25530 0.41450 0.76730 0.0870 Uiso calc R 1.000
H H4 0.23830 0.61290 0.77880 0.0780 Uiso calc R 1.000
H H5 0.45870 0.71190 0.84890 0.0690 Uiso calc R 1.000
H H6 0.77250 0.33540 0.91550 0.0640 Uiso calc R 1.000
H H7A 1.10660 0.44070 0.92890 0.0710 Uiso calc R 1.000
H H7B 1.01410 0.36490 1.00470 0.0710 Uiso calc R 1.000
H H8A 1.19960 0.48450 1.08160 0.0650 Uiso calc R 1.000
H H8B 1.01630 0.51560 1.11210 0.0650 Uiso calc R 1.000
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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 '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_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 O1W . . . 91.26(17) yes
O1 Cu1 N1 . . . 166.05(18) yes
O1 Cu1 N2 . . . 91.13(18) yes
O1 Cu1 O2 . . 3_467 87.57(16) yes
O1W Cu1 N1 . . . 100.66(17) yes
O1W Cu1 N2 . . . 91.1(2) yes
O1W Cu1 O2 . . 3_467 94.06(17) yes
N1 Cu1 N2 . . . 81.5(2) yes
O2 Cu1 N1 3_467 . . 98.68(18) yes
O2 Cu1 N2 3_467 . . 174.7(2) yes
O3 Cl1 O6 . . . 107.2(5) ?
O4 Cl1 O5 . . . 109.1(5) ?
O4 Cl1 O6 . . . 110.8(5) ?
O5 Cl1 O6 . . . 111.6(5) ?
O3 Cl1 O5 . . . 108.1(5) ?
O3 Cl1 O4 . . . 110.1(5) ?
Cu1 O1 C9 . . . 126.4(4) ?
Cu1 O2 C9 3_567 . . 125.0(4) ?
Cu1 O1W H1WB . . . 109.00 no
Cu1 O1W H1WA . . . 110.00 no
H1WB O1W H1WA . . . 109.00 no
C1 N1 C5 . . . 118.9(6) ?
Cu1 N1 C5 . . . 129.2(5) ?
Cu1 N1 C1 . . . 111.9(4) ?
Cu1 N2 C6 . . . 114.5(4) ?
Cu1 N2 C7 . . . 123.6(4) ?
C6 N2 C7 . . . 121.9(5) ?
C2 C1 C6 . . . 123.4(6) no
N1 C1 C6 . . . 114.7(6) ?
N1 C1 C2 . . . 121.8(6) ?
C1 C2 C3 . . . 119.1(7) no
C2 C3 C4 . . . 119.5(7) no
C3 C4 C5 . . . 118.3(7) no
N1 C5 C4 . . . 122.5(7) ?
N2 C6 C1 . . . 117.3(6) ?
C9 C8 C7 . . . 116.4(5) no
O2 C9 C8 . . . 118.1(5) ?
O1 C9 C8 . . . 119.6(5) ?
O1 C9 O2 . . . 122.3(5) ?
N2 C7 C8 . . . 112.3(5) ?
C1 C2 H2 . . . 121.00 no
C3 C2 H2 . . . 120.00 no
C4 C3 H3 . . . 120.00 no
C2 C3 H3 . . . 120.00 no
C3 C4 H4 . . . 121.00 no
C5 C4 H4 . . . 121.00 no
N1 C5 H5 . . . 119.00 no
C4 C5 H5 . . . 119.00 no
C1 C6 H6 . . . 121.00 no
N2 C6 H6 . . . 121.00 no
C7 C8 H8A . . . 108.00 no
C9 C8 H8B . . . 108.00 no
C9 C8 H8A . . . 108.00 no
C7 C8 H8B . . . 108.00 no
H7A C7 H7B . . . 108.00 no
H8A C8 H8B . . . 107.00 no
N2 C7 H7A . . . 109.00 no
N2 C7 H7B . . . 109.00 no
C8 C7 H7A . . . 109.00 no
C8 C7 H7B . . . 109.00 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 O1 . . 1.959(4) yes
Cu1 O2 . 3_467 1.957(4) yes
Cu1 O1W . . 2.397(4) yes
Cu1 N1 . . 1.997(5) yes
Cu1 N2 . . 1.976(5) yes
Cl1 O4 . . 1.390(8) ?
Cl1 O5 . . 1.369(9) ?
Cl1 O3 . . 1.387(7) ?
Cl1 O6 . . 1.364(9) ?
O1 C9 . . 1.268(7) yes
O2 C9 . . 1.240(7) yes
O1W H1WB . . 0.8500 no
O1W H1WA . . 0.8500 no
N1 C1 . . 1.350(8) ?
N1 C5 . . 1.321(8) ?
N2 C6 . . 1.265(8) yes
N2 C7 . . 1.445(8) yes
C1 C6 . . 1.448(9) no
C1 C2 . . 1.381(10) no
C2 C3 . . 1.373(11) no
C3 C4 . . 1.380(12) no
C4 C5 . . 1.395(10) no
C7 C8 . . 1.508(9) no
C8 C9 . . 1.520(8) no
C2 H2 . . 0.9300 no
C3 H3 . . 0.9300 no
C4 H4 . . 0.9300 no
C5 H5 . . 0.9300 no
C6 H6 . . 0.9300 no
C7 H7A . . 0.9700 no
C7 H7B . . 0.9700 no
C8 H8B . . 0.9700 no
C8 H8A . . 0.9700 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
O1W H1WB O1 3_467 0.85 2.12 2.730(6) 129 yes
O1W H1WA O3 . 0.85 2.17 2.928(9) 149 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
O1W Cu1 O1 C9 . . . . 53.8(5) no
N2 Cu1 O1 C9 . . . . -37.3(5) no
O2 Cu1 O1 C9 3_467 . . . 147.8(5) no
O1W Cu1 N1 C1 . . . . -88.0(4) no
O1W Cu1 N1 C5 . . . . 93.6(5) no
N2 Cu1 N1 C1 . . . . 1.5(4) no
N2 Cu1 N1 C5 . . . . -176.9(5) no
O2 Cu1 N1 C1 3_467 . . . 176.2(4) no
O2 Cu1 N1 C5 3_467 . . . -2.2(5) no
O1 Cu1 N2 C6 . . . . -170.6(5) no
O1 Cu1 N2 C7 . . . . 9.0(5) no
O1W Cu1 N2 C6 . . . . 98.1(5) no
O1W Cu1 N2 C7 . . . . -82.3(5) no
N1 Cu1 N2 C6 . . . . -2.5(5) no
N1 Cu1 N2 C7 . . . . 177.1(5) no
O1 Cu1 O2 C9 . . 3_467 3_467 -127.5(5) no
O1W Cu1 O2 C9 . . 3_467 3_467 -36.4(5) no
N1 Cu1 O2 C9 . . 3_467 3_467 65.1(5) no
Cu1 O1 C9 O2 . . . . -158.6(4) no
Cu1 O1 C9 C8 . . . . 19.2(7) no
Cu1 O2 C9 O1 3_567 . . . 2.7(8) no
Cu1 O2 C9 C8 3_567 . . . -175.1(4) no
Cu1 N1 C1 C2 . . . . -177.9(5) no
Cu1 N1 C1 C6 . . . . -0.4(6) no
C5 N1 C1 C2 . . . . 0.6(9) no
C5 N1 C1 C6 . . . . 178.2(5) no
Cu1 N1 C5 C4 . . . . 178.5(4) no
C1 N1 C5 C4 . . . . 0.2(8) no
Cu1 N2 C6 C1 . . . . 3.1(7) no
C7 N2 C6 C1 . . . . -176.6(6) no
Cu1 N2 C7 C8 . . . . 31.6(7) no
C6 N2 C7 C8 . . . . -148.8(6) no
N1 C1 C2 C3 . . . . -0.6(9) no
C6 C1 C2 C3 . . . . -178.0(6) no
N1 C1 C6 N2 . . . . -1.8(8) no
C2 C1 C6 N2 . . . . 175.7(6) no
C1 C2 C3 C4 . . . . -0.2(10) no
C2 C3 C4 C5 . . . . 1.0(10) no
C3 C4 C5 N1 . . . . -1.0(9) no
C7 C8 C9 O1 . . . . 35.6(8) no
C7 C8 C9 O2 . . . . -146.6(6) no
C9 C8 C7 N2 . . . . -60.4(7) no
