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#$Date: 2022-09-15 14:08:19 +0300 (Thu, 15 Sep 2022) $
#$Revision: 277870 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/10/11/7101164.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_7101164
loop_
_publ_author_name
'Tomoaki Tanase'
'Merii Kato'
'Ajay Sah'
_publ_section_title
;
Trinuclear coordinatively labile Cu(II) complex of
4,6-O-ethylidene-beta-D-glucopyranosylamine derived Schiff base ligand
and its reactivity towards primary alcohols and amines
;
_journal_issue                   5
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b413923b
_journal_year                    2005
_chemical_formula_moiety         'C5 H25 Cl2 Cu N5 '
_chemical_formula_sum            'C5 H25 Cl2 Cu N5'
_chemical_formula_weight         289.74
_space_group_IT_number           62
_space_group_name_Hall           '-P 2ac 2n'
_space_group_name_H-M_alt        'P n m a'
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      62
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.0065(10)
_cell_length_b                   11.6044(11)
_cell_length_c                   8.5136(5)
_cell_measurement_reflns_used    2274
_cell_measurement_temperature    153.1
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.3
_cell_volume                     1383.8(2)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_molecular_graphics    ORTEP-II
_computing_publication_material  'CrystalStructure 3.6.0'
_computing_structure_refinement  CRYSTALS
_computing_structure_solution    SIR97
_diffrn_detector_area_resol_mean 7.31
_diffrn_measured_fraction_theta_full 0.7004
_diffrn_measured_fraction_theta_max 0.1546
_diffrn_measurement_device_type  'Rigaku Mercury'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.019
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            7810
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         48.76
_exptl_absorpt_coefficient_mu    1.938
_exptl_absorpt_correction_T_max  0.824
_exptl_absorpt_correction_T_min  0.731
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             612.00
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.95
_refine_diff_density_min         -0.47
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.735
_refine_ls_hydrogen_treatment    refall
_refine_ls_number_parameters     70
_refine_ls_number_reflns         1023
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.0000
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
'w = 1/[0.0010Fo² + 3.0000σ(Fo²) + 0.5000]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                1021
_reflns_number_total             1158
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            b413923b.txt
_cod_original_formula_sum        'C5 H25 Cl2 Cu N5 '
_cod_database_code               7101164
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 1/2-X,1/2+Y,1/2+Z
3 +X,1/2-Y,+Z
4 1/2-X,-Y,1/2+Z
5 -X,-Y,-Z
6 1/2+X,1/2-Y,1/2-Z
7 -X,1/2+Y,-Z
8 1/2+X,+Y,1/2-Z
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
Cu(1) Cu 0.13043(4) 0.2500 0.78432(7) 0.0194(2) Uani 1.00 2 d S
Cl(1) Cl 0.35125(6) 0.01282(8) 0.65351(12) 0.0271(3) Uani 1.00 1 d .
N(1) N 0.1307(2) 0.0754(3) 0.7816(3) 0.0242(9) Uani 1.00 1 d .
N(2) N 0.2219(3) 0.2500 0.9998(5) 0.0242(12) Uani 1.00 2 d S
N(3) N 0.2228(3) 0.2500 0.5947(5) 0.0264(13) Uani 1.00 2 d S
N(4) N -0.0063(3) 0.2500 0.8781(5) 0.0245(12) Uani 1.00 2 d S
C(1) C 0.0793(3) 0.0165(3) 0.6549(5) 0.0373(12) Uani 1.00 1 d .
C(2) C 0.3242(4) 0.2500 0.9697(7) 0.030(2) Uani 1.00 2 d S
C(3) C 0.1848(5) 0.2500 0.4312(6) 0.048(2) Uani 1.00 2 d S
C(4) C -0.0102(4) 0.2500 1.0517(6) 0.033(2) Uani 1.00 2 d S
H(1) H 0.1140 0.0361 0.5658 0.046 Uiso 1.00 1 c R
H(2) H 0.0134 0.0625 0.6341 0.046 Uiso 1.00 1 c R
H(3) H 0.0804 -0.0695 0.6691 0.046 Uiso 1.00 1 c R
H(4) H 0.1059 0.0475 0.8754 0.029 Uiso 1.00 1 c R
H(5) H 0.1868 0.0516 0.7846 0.029 Uiso 1.00 1 c R
H(6) H 0.2031 0.3163 1.0543 0.029 Uiso 1.00 1 c R
H(7) H 0.3599 0.2500 1.0572 0.036 Uiso 1.00 2 c R
H(8) H 0.3417 0.1807 0.9091 0.037 Uiso 1.00 1 c R
H(9) H -0.0382 0.1817 0.8470 0.029 Uiso 1.00 1 c R
H(10) H -0.0750 0.2500 1.0850 0.040 Uiso 1.00 2 c R
H(11) H 0.0197 0.3135 1.0850 0.040 Uiso 1.00 1 c R
H(12) H 0.2604 0.3152 0.6098 0.032 Uiso 1.00 1 c R
H(13) H 0.2305 0.2500 0.3699 0.060 Uiso 1.00 2 c R
H(14) H 0.1454 0.1825 0.4125 0.060 Uiso 1.00 1 c R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.003 0.002
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.000 0.000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
Cu Cu 0.320 1.265
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.006 0.003
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
Cl Cl 0.148 0.159
;
International Tables for Crystallography
(1992, 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_2
_geom_angle_site_symmetry_3
N(1) Cu(1) N(1) 178.7(1) 55503 . .
N(2) Cu(1) N(1) 90.48(8) . . .
N(3) Cu(1) N(1) 89.44(8) . . .
N(4) Cu(1) N(1) 90.34(8) . . .
Cu(1) N(1) C(1) 118.3(2) . . .
N(2) Cu(1) N(1) 90.48(8) . . 55503
N(3) Cu(1) N(1) 89.44(8) . . 55503
N(4) Cu(1) N(1) 90.34(8) . . 55503
Cu(1) N(1) C(1) 118.3(2) . 55503 55503
N(3) Cu(1) N(2) 106.4(2) . . .
N(4) Cu(1) N(2) 102.3(2) . . .
Cu(1) N(2) C(2) 114.8(3) . . .
N(4) Cu(1) N(3) 151.3(2) . . .
Cu(1) N(3) C(3) 120.4(4) . . .
Cu(1) N(4) C(4) 114.8(3) . . .
Cu(1) N(1) H(4) 109.7473 . . .
Cu(1) N(1) H(5) 109.4367 . . .
Cu(1) N(1) H(4) 109.7473 . 55503 55503
Cu(1) N(1) H(5) 109.4367 . 55503 55503
Cu(1) N(2) H(6) 104.1265 . . .
Cu(1) N(2) H(6) 104.1265 . . 55503
Cu(1) N(3) H(12) 104.2383 . . .
Cu(1) N(3) H(12) 104.2383 . . 55503
Cu(1) N(4) H(9) 109.1452 . . .
Cu(1) N(4) H(9) 109.1452 . . 55503
N(1) C(1) H(1) 103.2508 . . .
N(1) C(1) H(2) 108.0168 . . .
H(4) N(1) C(1) 106.6729 . . .
H(5) N(1) C(1) 109.3257 . . .
N(1) C(1) H(3) 111.4602 . . .
H(5) N(1) H(4) 102.1528 . . .
H(6) N(2) C(2) 111.4317 . . .
H(6) N(2) C(2) 111.4317 55503 . .
N(2) C(2) H(8) 109.6749 . . .
N(2) C(2) H(8) 109.6749 . . 55503
N(2) C(2) H(7) 113.6313 . . .
H(6) N(2) H(6) 110.5119 55503 . .
H(12) N(3) C(3) 109.3263 . . .
H(12) N(3) C(3) 109.3263 55503 . .
N(3) C(3) H(14) 110.8861 . . .
N(3) C(3) H(14) 110.8862 . . 55503
N(3) C(3) H(13) 108.3105 . . .
H(12) N(3) H(12) 108.8041 55503 . .
H(9) N(4) C(4) 105.1339 . . .
H(9) N(4) C(4) 105.1339 55503 . .
N(4) C(4) H(11) 107.4305 . . .
N(4) C(4) H(11) 107.4305 . . 55503
N(4) C(4) H(10) 109.4522 . . .
H(9) N(4) H(9) 113.5647 55503 . .
H(2) C(1) H(1) 101.0578 . . .
H(3) C(1) H(1) 109.4716 . . .
H(3) C(1) H(2) 121.6322 . . .
H(8) C(2) H(7) 107.2414 . . .
H(8) C(2) H(7) 107.2414 55503 . .
H(8) C(2) H(8) 109.2630 55503 . .
H(14) C(3) H(13) 109.6512 . . .
H(14) C(3) H(13) 109.6512 55503 . .
H(14) C(3) H(14) 107.4480 55503 . .
H(11) C(4) H(10) 110.6456 . . .
H(11) C(4) H(10) 110.6456 55503 . .
H(11) C(4) H(11) 111.1167 55503 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu(1) N(1) 2.027(3) .
Cu(1) N(1) 2.027(3) 55503
Cu(1) N(2) 2.238(4) .
Cu(1) N(2) 2.238(4) 55503
Cu(1) N(3) 2.069(4) .
Cu(1) N(4) 2.074(4) .
N(1) C(1) 1.466(5) .
N(2) Cu(1) 2.238(4) .
N(2) Cu(1) 2.238(4) 55503
N(2) C(2) 1.456(7) .
N(2) C(2) 1.456(7) 55503
N(3) C(3) 1.490(7) .
N(4) C(4) 1.479(7) .
C(2) N(2) 1.456(7) .
C(2) N(2) 1.456(7) 55503
N(1) H(4) 0.9287 .
N(1) H(5) 0.8333 .
N(2) H(6) 0.9363 .
N(2) H(6) 0.9363 55503
N(3) H(12) 0.9301 .
N(3) H(12) 0.9301 55503
N(4) H(9) 0.9478 .
N(4) H(9) 0.9478 55503
C(1) H(1) 0.9291 .
C(1) H(2) 1.0803 .
C(1) H(3) 1.0048 .
C(2) H(7) 0.8971 .
C(2) H(8) 0.9862 .
C(2) H(8) 0.9862 55503
C(3) H(13) 0.8254 .
C(3) H(14) 0.9716 .
C(3) H(14) 0.9716 55503
C(4) H(10) 0.9506 .
C(4) H(11) 0.8938 .
C(4) H(11) 0.8938 55503
H(6) N(2) 0.9363 .
H(6) N(2) 0.9363 55503
