#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/09/2010958.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_2010958
loop_
_publ_author_name
'Kani, Yoshiyuki'
'Ohba, Shigeru'
'Ito, Sayo'
'Nishida, Yuzo'
_publ_section_title
;
 Redetermination of
 bis{[(2-hydroxyphenylmethyl)bis(2-pyridylmethyl)aminato]copper(II)}
 diperchlorate
;
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              e201
_journal_page_last               e201
_journal_paper_doi               10.1107/S0108270100005680
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Cu2 (C19 H18 N3 O)2] (Cl O4)2'
_chemical_formula_sum            'C38 H36 Cl2 Cu2 N6 O10'
_chemical_formula_weight         934.74
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 104.790(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.3800(10)
_cell_length_b                   9.877(2)
_cell_length_c                   17.400(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     1891.0(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1993)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1999)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measured_fraction_theta_full .9995
_diffrn_measured_fraction_theta_max .9995
_diffrn_measurement_device_type  'Rigaku AFC-5S'
_diffrn_measurement_method       θ-2θ
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .059
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            4819
_diffrn_reflns_theta_full        27.5
_diffrn_reflns_theta_max         27.5
_diffrn_standards_decay_%        5.5
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.334
_exptl_absorpt_correction_T_max  .897
_exptl_absorpt_correction_T_min  .662
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .1
_refine_diff_density_max         .59
_refine_diff_density_min         -.63
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   .98
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4338
_refine_ls_R_factor_gt           .063
_refine_ls_shift/su_max          .009
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²) + (0.1(Fo² + 2Fc²)/3)²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .185
_reflns_number_gt                2393
_reflns_number_total             4338
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            qa0277.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               2010958
_cod_database_fobs_code          2010958
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_adp_type
_atom_site_occupancy
_atom_site_type_symbol
Cu1 .54358(6) .02660(8) .42187(4) .0373(2) Uani 1.00 Cu
Cl1 .49550(10) .2387(2) .16920(10) .0603(5) Uani 1.00 Cl
O1 .6029(3) -.0563(4) .5432(2) .0430(10) Uani 1.00 O
O2 .5814(5) .1502(6) .1495(4) .085(2) Uani 1.00 O
O3 .4568(5) .1790(10) .2322(4) .142(3) Uani 1.00 O
O4 .3945(6) .2534(9) .1043(4) .126(3) Uani 1.00 O
O5 .5546(7) .3610(9) .1932(7) .160(4) Uani 1.00 O
N1 .6163(4) .2133(6) .4286(3) .0450(10) Uani 1.00 N
N2 .7031(4) -.0249(6) .3969(3) .0430(10) Uani 1.00 N
N3 .4837(4) -.1444(5) .3634(3) .0380(10) Uani 1.00 N
C1 .5920(5) .3222(6) .4677(4) .045(2) Uani 1.00 C
C2 .6567(7) .4417(7) .4739(4) .059(2) Uani 1.00 C
C3 .7500(7) .4480(9) .4364(5) .071(3) Uani 1.00 C
C4 .7756(6) .3392(9) .3949(4) .064(2) Uani 1.00 C
C5 .7093(5) .2212(7) .3932(4) .050(2) Uani 1.00 C
C6 .7315(5) .0962(8) .3523(4) .057(2) Uani 1.00 C
C7 .6918(6) -.1505(8) .3492(4) .062(2) Uani 1.00 C
C8 .5683(5) -.2142(7) .3366(3) .044(2) Uani 1.00 C
C9 .5431(6) -.3391(7) .3010(4) .053(2) Uani 1.00 C
C10 .4301(7) -.3950(7) .2919(4) .060(2) Uani 1.00 C
C11 .3438(6) -.3230(7) .3184(4) .054(2) Uani 1.00 C
C12 .3731(5) -.1988(7) .3528(3) .044(2) Uani 1.00 C
C13 .8019(4) -.0359(7) .4726(3) .043(2) Uani 1.00 C
C14 .7886(5) -.1479(6) .5270(4) .043(2) Uani 1.00 C
C15 .8802(5) -.2459(7) .5490(4) .049(2) Uani 1.00 C
C16 .8783(6) -.3425(7) .6050(5) .058(2) Uani 1.00 C
C17 .7859(5) -.3416(7) .6435(4) .051(2) Uani 1.00 C
C18 .6940(5) -.2455(6) .6239(3) .043(2) Uani 1.00 C
C19 .6923(4) -.1495(6) .5647(3) .0360(10) Uani 1.00 C
H1 .5260 .3169 .4927 .0543 Uiso 1.00 H
H2 .6377 .5175 .5031 .0707 Uiso 1.00 H
H3 .7970 .5294 .4395 .0847 Uiso 1.00 H
H4 .8388 .3444 .3675 .0764 Uiso 1.00 H
H5 .8152 .0931 .3507 .0682 Uiso 1.00 H
H6 .6803 .0956 .2991 .0682 Uiso 1.00 H
H7 .7055 -.1293 .2984 .0744 Uiso 1.00 H
H8 .7520 -.2140 .3764 .0744 Uiso 1.00 H
H9 .6043 -.3867 .2827 .0633 Uiso 1.00 H
H10 .4112 -.4824 .2676 .0720 Uiso 1.00 H
H11 .2639 -.3598 .3125 .0646 Uiso 1.00 H
H12 .3120 -.1490 .3700 .0533 Uiso 1.00 H
H13 .8776 -.0486 .4587 .0515 Uiso 1.00 H
H14 .8043 .0478 .5011 .0515 Uiso 1.00 H
H15 .9463 -.2452 .5239 .0588 Uiso 1.00 H
H16 .9407 -.4104 .6175 .0699 Uiso 1.00 H
H17 .7853 -.4077 .6839 .0617 Uiso 1.00 H
H18 .6308 -.2451 .6514 .0520 Uiso 1.00 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C .003 .002
;International Tables for Crystallography
(1992, Vol. C)
;
H H .000 .000
;International Tables for Crystallography
(1992, Vol. C)
;
Cl Cl .148 .159
;International Tables for Crystallography
(1992, Vol. C)
;
Cu Cu .320 1.265
;International Tables for Crystallography
(1992, Vol. C)
;
N N .006 .003
;International Tables for Crystallography
(1992, Vol. C)
;
O O .011 .006
;International Tables for Crystallography
(1992, Vol. C)
;
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_3
_geom_angle
_geom_angle_publ_flag
O1 Cu1 O1 . 3_656 80.4(2) yes
O1 Cu1 N1 . . 105.3(2) no
O1 Cu1 N2 . . 92.3(2) no
O1 Cu1 N3 . . 98.9(2) no
O1 Cu1 N1 3_656 . 102.5(2) no
O1 Cu1 N2 3_656 . 172.1(2) no
O1 Cu1 N3 3_656 . 94.5(2) no
N1 Cu1 N2 . . 82.3(2) no
N1 Cu1 N3 . . 152.3(2) no
N2 Cu1 N3 . . 83.5(2) no
O2 Cl1 O3 . . 107.6(5) no
O2 Cl1 O4 . . 110.2(5) no
O2 Cl1 O5 . . 107.3(4) no
O3 Cl1 O4 . . 108.4(4) no
O3 Cl1 O5 . . 110.5(6) no
O4 Cl1 O5 . . 112.7(6) no
Cu1 O1 Cu1 . 3_656 99.6(2) yes
Cu1 O1 C19 . . 122.9(3) no
Cu1 O1 C19 3_656 . 131.5(4) no
Cu1 N1 C1 . . 129.1(4) no
Cu1 N1 C5 . . 112.5(4) no
C1 N1 C5 . . 118.2(6) no
Cu1 N2 C6 . . 103.4(4) no
Cu1 N2 C7 . . 112.0(4) no
Cu1 N2 C13 . . 109.8(3) no
C6 N2 C7 . . 112.1(5) no
C6 N2 C13 . . 107.4(5) no
C7 N2 C13 . . 111.7(5) no
Cu1 N3 C8 . . 115.1(4) no
Cu1 N3 C12 . . 126.6(4) no
C8 N3 C12 . . 118.2(5) no
N1 C1 C2 . . 123.4(6) no
N1 C1 H1 . . 118.3 no
C2 C1 H1 . . 118.3 no
C1 C2 C3 . . 117.5(7) no
C1 C2 H2 . . 121.3 no
C3 C2 H2 . . 121.3 no
C2 C3 C4 . . 120.5(7) no
C2 C3 H3 . . 119.8 no
C4 C3 H3 . . 119.8 no
C3 C4 C5 . . 119.0(7) no
C3 C4 H4 . . 120.5 no
C5 C4 H4 . . 120.5 no
N1 C5 C4 . . 121.5(7) no
N1 C5 C6 . . 114.8(6) no
C4 C5 C6 . . 123.7(6) no
N2 C6 C5 . . 109.3(5) no
N2 C6 H5 . . 109.6 no
N2 C6 H6 . . 109.6 no
C5 C6 H5 . . 109.5 no
C5 C6 H6 . . 109.5 no
H5 C6 H6 . . 109.5 no
N2 C7 C8 . . 112.2(5) no
N2 C7 H7 . . 108.8 no
N2 C7 H8 . . 108.8 no
C8 C7 H7 . . 108.8 no
C8 C7 H8 . . 108.7 no
H7 C7 H8 . . 109.5 no
N3 C8 C7 . . 117.1(6) no
N3 C8 C9 . . 121.6(6) no
C7 C8 C9 . . 121.3(5) no
C8 C9 C10 . . 119.6(6) no
C8 C9 H9 . . 120.2 no
C10 C9 H9 . . 120.2 no
C9 C10 C11 . . 118.6(6) no
C9 C10 H10 . . 120.7 no
C11 C10 H10 . . 120.6 no
C10 C11 C12 . . 119.5(6) no
C10 C11 H11 . . 120.3 no
C12 C11 H11 . . 120.3 no
N3 C12 C11 . . 122.4(6) no
N3 C12 H12 . . 118.8 no
C11 C12 H12 . . 118.8 no
N2 C13 C14 . . 115.9(5) no
N2 C13 H13 . . 107.9 no
N2 C13 H14 . . 107.8 no
C14 C13 H13 . . 107.8 no
C14 C13 H14 . . 107.8 no
H13 C13 H14 . . 109.4 no
C13 C14 C15 . . 119.8(5) no
C13 C14 C19 . . 121.3(5) no
C15 C14 C19 . . 118.4(6) no
C14 C15 C16 . . 122.0(5) no
C14 C15 H15 . . 119.0 no
C16 C15 H15 . . 119.0 no
C15 C16 C17 . . 119.5(6) no
C15 C16 H16 . . 120.3 no
C17 C16 H16 . . 120.3 no
C16 C17 C18 . . 120.2(6) no
C16 C17 H17 . . 119.9 no
C18 C17 H17 . . 119.9 no
C17 C18 C19 . . 120.8(5) no
C17 C18 H18 . . 119.6 no
C19 C18 H18 . . 119.6 no
O1 C19 C14 . . 118.7(5) no
O1 C19 C18 . . 122.3(5) no
C14 C19 C18 . . 118.9(5) 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 . . 2.203(4) yes
Cu1 O1 . 3_656 1.938(3) yes
Cu1 N1 . . 2.013(5) yes
Cu1 N2 . . 2.037(4) yes
Cu1 N3 . . 2.000(5) yes
Cl1 O2 . . 1.416(6) no
Cl1 O3 . . 1.411(7) no
Cl1 O4 . . 1.398(6) no
Cl1 O5 . . 1.393(7) no
O1 C19 . . 1.352(6) no
N1 C1 . . 1.338(8) no
N1 C5 . . 1.357(7) no
N2 C6 . . 1.505(9) no
N2 C7 . . 1.479(8) no
N2 C13 . . 1.502(7) no
N3 C8 . . 1.359(7) no
N3 C12 . . 1.338(7) no
C1 C2 . . 1.381(9) no
C1 H1 . . .960 no
C2 C3 . . 1.380(10) no
C2 H2 . . .960 no
C3 C4 . . 1.370(10) no
C3 H3 . . .960 no
C4 C5 . . 1.384(10) no
C4 H4 . . .960 no
C5 C6 . . 1.480(10) no
C6 H5 . . .960 no
C6 H6 . . .960 no
C7 C8 . . 1.503(9) no
C7 H7 . . .959 no
C7 H8 . . .960 no
C8 C9 . . 1.377(9) no
C9 C10 . . 1.371(10) no
C9 H9 . . .960 no
C10 C11 . . 1.383(9) no
C10 H10 . . .961 no
C11 C12 . . 1.368(9) no
C11 H11 . . .960 no
C12 H12 . . .960 no
C13 C14 . . 1.488(8) no
C13 H13 . . .960 no
C13 H14 . . .960 no
C14 C15 . . 1.402(8) no
C14 C19 . . 1.414(7) no
C15 C16 . . 1.368(10) no
C15 H15 . . .961 no
C16 C17 . . 1.383(9) no
C16 H16 . . .960 no
C17 C18 . . 1.389(8) no
C17 H17 . . .961 no
C18 C19 . . 1.396(8) no
C18 H18 . . .960 no
loop_
_geom_contact_atom_site_label_1
_geom_contact_atom_site_label_2
_geom_contact_distance
_geom_contact_site_symmetry_2
Cu1 O3 3.531(7) .
O2 C7 3.242(8) 2_655
O2 C3 3.372(9) 2_645
O2 C6 3.547(9) .
O3 C11 3.308(8) 2_555
O3 C6 3.387(9) .
O3 C18 3.441(9) 3_656
O3 N1 3.453(8) .
O3 C5 3.487(8) .
O4 C12 3.349(9) 2_555
O4 C11 3.410(10) 2_555
O4 C3 3.570(10) 4_454
O4 C13 3.594(10) 4_454
O5 C7 3.158(10) 2_655
O5 C10 3.465(10) 1_565
O5 C9 3.527(9) 1_565
O5 C6 3.600(10) 2_655
C3 C9 3.560(10) 1_565
C3 C16 3.580(10) 1_565
C10 C17 3.560(10) 4_444
C11 C17 3.364(10) 4_444
C11 C18 3.446(9) 4_444
C12 C17 3.545(9) 4_444
