#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/36/4323602.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_4323602
loop_
_publ_author_name
'Hitoshi Miyasaka'
'Shingo Okamura'
'Toshio Nakashima'
'Naohide Matsumoto'
_publ_section_title
;
 Copper(II) Complexes of
 N,N'-Bis((2-substituted-imidazol-4-yl)methylene)-3,3'-diaminodi-
 propylamine (2-Substituent = H, Me): Δ and Λ Enantiomorphs of the
 Protonated Complex and Helical Structure of the Deprotonated Complex
 Formed by Hydrogen Bonds
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4329
_journal_page_last               4335
_journal_paper_doi               10.1021/ic970425v
_journal_volume                  36
_journal_year                    1997
_chemical_formula_sum            'C16 H20 Cl2 Cu N7 O2'
_chemical_formula_weight         476.83
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_date             'Sun Mar 16 21:58:48 1997'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 98.57(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   9.884(2)
_cell_length_b                   15.073(3)
_cell_length_c                   15.295(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    20.0
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      29.74
_cell_volume                     2253.2(7)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan: PROCESS (MSC)'
_computing_publication_material  'teXsan: FINISH (MSC)'
_computing_structure_refinement  'teXsan: LS (MSC)'
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       AFC7R
_diffrn_measurement_method       'omega/2-theta scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoKalpha
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  3.08
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_theta_max         27.5331
_diffrn_standards_decay_%        -2.11
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.2309
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.823
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.406
_exptl_crystal_description       prismatic
_exptl_crystal_size_max          0.500
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.220
_refine_diff_density_max         0.46790
_refine_diff_density_min         -0.52080
_refine_ls_extinction_coef       1.77926
_refine_ls_extinction_method     Zachariasen_type_2_Gaussian_isotropic
_refine_ls_goodness_of_fit_obs   6.490
_refine_ls_matrix_type           full
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4262
_refine_ls_number_restraints     0
_refine_ls_R_factor_obs          0.0420
_refine_ls_shift/esd_max         0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_obs         0.0390
_reflns_number_observed          4262
_reflns_number_total             5678
_cod_data_source_file            ic970425v_2.cif
_cod_data_source_block           '[Cu(H2L2)](Cl)2(2c)'
_cod_original_cell_volume        2253.1(7)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        C16H20O2N7Cl2Cu
_cod_database_code               4323602
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
1/2+x,1/2-y,1/2+z
loop_
_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_calc_attached_atom
Cu 0.04062(4) 0.77424(3) 0.60966(3) 0.0404 Uij ? ?
Cl1 -0.41644(10) 0.97578(7) 0.26521(6) 0.0596 Uij ? ?
Cl2 0.0438(1) 0.98942(7) 0.16935(7) 0.0744 Uij ? ?
O1 0.5284(3) 0.3779(2) 0.5038(2) 0.0870 Uij ? ?
O2 0.7131(3) 0.0261(2) 0.6742(2) 0.0970 Uij ? ?
N1 -0.0114(2) 0.6611(2) 0.5193(2) 0.0365 Uij ? ?
N2 -0.0947(3) 0.5635(2) 0.4186(2) 0.0449 Uij ? ?
N3 -0.1271(3) 0.7301(2) 0.6532(2) 0.0431 Uij ? ?
N4 0.1432(3) 0.7455(2) 0.7315(2) 0.0460 Uij ? ?
N5 0.2048(3) 0.8198(2) 0.5610(2) 0.0435 Uij ? ?
N6 -0.1645(3) 0.9308(2) 0.4015(2) 0.0540 Uij ? ?
N7 -0.0568(3) 0.8606(2) 0.5164(2) 0.0402 Uij ? ?
C1 0.1254(4) 0.6351(2) 0.3980(2) 0.0602 Uij ? ?
C2 0.0086(3) 0.6206(2) 0.4466(2) 0.0383 Uij ? ?
C3 -0.1860(3) 0.5674(2) 0.4766(2) 0.0454 Uij ? ?
C4 -0.1353(3) 0.6278(2) 0.5382(2) 0.0390 Uij ? ?
C5 -0.1878(3) 0.6638(2) 0.6140(2) 0.0430 Uij ? ?
C6 -0.1691(4) 0.7664(3) 0.7340(2) 0.0564 Uij ? ?
C7 -0.0606(4) 0.7493(3) 0.8110(2) 0.0594 Uij ? ?
C8 0.0784(4) 0.7878(3) 0.8029(2) 0.0603 Uij ? ?
C9 0.2925(4) 0.7647(3) 0.7449(2) 0.0652 Uij ? ?
C10 0.3597(4) 0.7331(3) 0.6709(3) 0.0687 Uij ? ?
C11 0.3495(4) 0.7970(3) 0.5936(2) 0.0569 Uij ? ?
C12 0.1774(4) 0.8680(2) 0.4923(2) 0.0469 Uij ? ?
C13 0.0354(4) 0.8896(2) 0.4636(2) 0.0447 Uij ? ?
C14 -0.0310(4) 0.9325(2) 0.3917(2) 0.0548 Uij ? ?
C15 -0.1780(4) 0.8866(2) 0.4767(2) 0.0454 Uij ? ?
C16 -0.3119(4) 0.8723(3) 0.5077(2) 0.0612 Uij ? ?
H1 0.2148 0.6441 0.4320 0.0637 Uij ? ?
H2 0.1326 0.6932 0.3765 0.0637 Uij ? ?
H3 0.1281 0.5950 0.3546 0.0637 Uij ? ?
H4 -0.0993 0.5229 0.3687 0.0637 Uij ? ?
H5 -0.2749 0.5307 0.4744 0.0637 Uij ? ?
H6 -0.2778 0.6327 0.6317 0.0637 Uij ? ?
H7 -0.2631 0.7412 0.7432 0.0637 Uij ? ?
H8 -0.1940 0.8339 0.7244 0.0637 Uij ? ?
H9 -0.0912 0.7757 0.8622 0.0637 Uij ? ?
H10 -0.0416 0.6804 0.8307 0.0637 Uij ? ?
H11 0.1387 0.7854 0.8561 0.0637 Uij ? ?
H12 0.0709 0.8547 0.7872 0.0637 Uij ? ?
H13 0.1313 0.6753 0.7337 0.0637 Uij ? ?
H14 0.3250 0.7351 0.8045 0.0637 Uij ? ?
H15 0.3004 0.8400 0.7523 0.0637 Uij ? ?
H16 0.4617 0.7200 0.6895 0.0637 Uij ? ?
H17 0.3113 0.6674 0.6445 0.0637 Uij ? ?
H18 0.3953 0.8545 0.6215 0.0637 Uij ? ?
H19 0.3890 0.7725 0.5430 0.0637 Uij ? ?
H20 0.2506 0.9019 0.4520 0.0637 Uij ? ?
H21 0.0030 0.9571 0.3336 0.0637 Uij ? ?
H22 -0.2397 0.9486 0.3584 0.0637 Uij ? ?
H23 -0.3818 0.8945 0.4738 0.0637 Uij ? ?
H24 -0.3122 0.8989 0.5677 0.0637 Uij ? ?
H25 -0.3363 0.8037 0.5052 0.0637 Uij ? ?
loop_
_atom_type_symbol
_atom_type_oxidation_number
_atom_type_number_in_cell
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0 64 0.003 0.002 'International Tables'
H 0 80 0.000 0.000 'International Tables'
N 0 28 0.006 0.003 'International Tables'
Cl 0 8 0.148 0.159 'International Tables'
Cu 0 4 0.320 1.265 'International Tables'
O 0 8 0.011 0.006 'International Tables'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
? ? ?
? ? ?
? ? ?
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_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N(1) Cu N(3) 79.8(1) ? ? ? yes
N(1) Cu N(4) 116.6(1) ? ? ? yes
N(1) Cu N(5) 99.14(10) ? ? ? yes
N(1) Cu N(7) 90.78(10) ? ? ? yes
N(3) Cu N(4) 87.0(1) ? ? ? yes
N(3) Cu N(5) 177.6(1) ? ? ? yes
N(3) Cu N(7) 96.7(1) ? ? ? yes
N(4) Cu N(5) 95.3(1) ? ? ? yes
N(4) Cu N(7) 152.6(1) ? ? ? yes
N(5) Cu N(7) 81.2(1) ? ? ? yes
Cu N(1) C(2) 147.3(2) ? ? ? yes
Cu N(1) C(4) 106.2(2) ? ? ? yes
C(2) N(1) C(4) 104.9(3) ? ? ? yes
C(2) N(2) C(3) 108.0(3) ? ? ? yes
Cu N(3) C(5) 117.6(2) ? ? ? yes
Cu N(3) C(6) 120.8(2) ? ? ? yes
C(5) N(3) C(6) 121.2(3) ? ? ? yes
Cu N(4) C(8) 111.8(2) ? ? ? yes
Cu N(4) C(9) 115.7(2) ? ? ? yes
C(8) N(4) C(9) 110.0(3) ? ? ? yes
Cu N(5) C(11) 126.1(2) ? ? ? yes
Cu N(5) C(12) 114.7(2) ? ? ? yes
C(11) N(5) C(12) 119.1(3) ? ? ? yes
C(14) N(6) C(15) 109.0(3) ? ? ? yes
Cu N(7) C(13) 109.0(2) ? ? ? yes
Cu N(7) C(15) 143.6(2) ? ? ? yes
C(13) N(7) C(15) 105.7(3) ? ? ? yes
N(1) C(2) N(2) 111.2(3) ? ? ? yes
N(1) C(2) C(1) 125.9(3) ? ? ? yes
N(2) C(2) C(1) 122.9(3) ? ? ? yes
N(2) C(3) C(4) 105.7(3) ? ? ? yes
N(1) C(4) C(3) 110.2(3) ? ? ? yes
N(1) C(4) C(5) 117.6(3) ? ? ? yes
C(3) C(4) C(5) 132.2(3) ? ? ? yes
N(3) C(5) C(4) 118.3(3) ? ? ? yes
N(3) C(6) C(7) 109.9(3) ? ? ? yes
C(6) C(7) C(8) 115.1(3) ? ? ? yes
N(4) C(8) C(7) 113.1(3) ? ? ? yes
N(4) C(9) C(10) 112.4(3) ? ? ? yes
C(9) C(10) C(11) 114.1(3) ? ? ? yes
N(5) C(11) C(10) 111.0(3) ? ? ? yes
N(5) C(12) C(13) 117.2(3) ? ? ? yes
N(7) C(13) C(12) 116.6(3) ? ? ? yes
N(7) C(13) C(14) 110.2(3) ? ? ? yes
C(12) C(13) C(14) 133.2(4) ? ? ? yes
N(6) C(14) C(13) 105.2(3) ? ? ? yes
N(6) C(15) N(7) 109.9(3) ? ? ? yes
N(6) C(15) C(16) 123.2(3) ? ? ? yes
N(7) C(15) C(16) 126.9(3) ? ? ? yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu N(1) 2.207(3) ? ? yes
Cu N(3) 1.991(3) ? ? yes
Cu N(4) 2.032(3) ? ? yes
Cu N(5) 2.005(3) ? ? yes
Cu N(7) 2.060(3) ? ? yes
N(1) C(2) 1.309(4) ? ? yes
N(1) C(4) 1.392(4) ? ? yes
N(2) C(2) 1.354(4) ? ? yes
N(2) C(3) 1.358(4) ? ? yes
N(3) C(5) 1.269(4) ? ? yes
N(3) C(6) 1.467(4) ? ? yes
N(4) C(8) 1.489(4) ? ? yes
N(4) C(9) 1.488(4) ? ? yes
N(5) C(11) 1.483(4) ? ? yes
N(5) C(12) 1.273(4) ? ? yes
N(6) C(14) 1.351(4) ? ? yes
N(6) C(15) 1.352(4) ? ? yes
N(7) C(13) 1.376(4) ? ? yes
N(7) C(15) 1.320(4) ? ? yes
C(1) C(2) 1.479(4) ? ? yes
C(3) C(4) 1.351(4) ? ? yes
C(4) C(5) 1.445(4) ? ? yes
C(6) C(7) 1.493(5) ? ? yes
C(7) C(8) 1.512(5) ? ? yes
C(9) C(10) 1.474(5) ? ? yes
C(10) C(11) 1.516(5) ? ? yes
C(12) C(13) 1.444(4) ? ? yes
C(13) C(14) 1.358(5) ? ? yes
C(15) C(16) 1.487(5) ? ? yes
