#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316450.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_4316450
loop_
_publ_author_name
'Apurba Biswas'
'Michael G. B. Drew'
'Carlos J. Gómez-García'
'Ashutosh Ghosh'
_publ_section_title
;
 Use of a Reduced Schiff-Base Ligand to Prepare Novel Chloro-Bridged
 Chains of Rare Cu(II) Trinuclear Complexes with Mixed Azido/Oxo and
 Chloro/Oxo Bridges
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8155
_journal_page_last               8163
_journal_paper_doi               10.1021/ic101183n
_journal_volume                  49
_journal_year                    2010
_chemical_formula_sum            'C22.46 H35.84 Cl4 Cu3 N4 O2.46'
_chemical_formula_weight         733.69
_chemical_name_systematic
; 
 ? 
;
_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'
_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                 104.487(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4006(6)
_cell_length_b                   17.4750(6)
_cell_length_c                   15.0750(7)
_cell_measurement_reflns_used    19988
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.33
_cell_volume                     2907.8(2)
_computing_cell_refinement       'Crysalis, Oxford Diffraction'
_computing_data_collection       'Crysalis, Oxford Diffraction'
_computing_data_reduction        'Crysalis, Oxford Diffraction'
_computing_molecular_graphics    PLATON(Spek,2004)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device       'Oxford Diffaction X-Calibur System'
_diffrn_measurement_method       '321 frames, counting time 10 s.'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0545
_diffrn_reflns_av_sigmaI/netI    0.0990
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            19998
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.33
_diffrn_standards_decay_%        n/a
_diffrn_standards_interval_count n/a
_diffrn_standards_interval_time  n/a
_diffrn_standards_number         n/a
_exptl_absorpt_coefficient_mu    2.571
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.855
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            deep_green
_exptl_crystal_density_diffrn    1.676
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1493
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.855
_refine_diff_density_min         -1.062
_refine_diff_density_rms         0.175
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.246
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     336
_refine_ls_number_reflns         8419
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.246
_refine_ls_R_factor_all          0.1352
_refine_ls_R_factor_gt           0.0939
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
_refine_ls_weighting_details 
  w=1/[σ²(Fo²)+(0.0000P)²+38.7379P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1821
_refine_ls_wR_factor_ref         0.1913
_reflns_number_gt                5690
_reflns_number_total             8419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101183n_si_001_2.cif
_cod_data_source_block           2
_cod_database_code               4316450
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C12 C 0.7553(9) 0.1979(5) 0.9805(6) 0.0269(19) Uani 1 1 d . . .
C13 C 0.8697(9) 0.2306(6) 0.9934(6) 0.032(2) Uani 1 1 d . . .
H13 H 0.9061 0.2533 1.0493 0.039 Uiso 1 1 calc R . .
C14 C 0.9299(9) 0.2297(6) 0.9245(7) 0.037(2) Uani 1 1 d . . .
H14 H 1.0063 0.2518 0.9343 0.044 Uiso 1 1 calc R . .
C15 C 0.8765(10) 0.1960(5) 0.8404(6) 0.036(2) Uani 1 1 d . . .
H15 H 0.9164 0.1955 0.7936 0.043 Uiso 1 1 calc R . .
C16 C 0.7647(11) 0.1639(5) 0.8281(7) 0.039(3) Uani 1 1 d . . .
H16 H 0.7297 0.1414 0.7718 0.047 Uiso 1 1 calc R . .
C17 C 0.6993(9) 0.1631(5) 0.8961(6) 0.029(2) Uani 1 1 d . . .
C18 C 0.5772(10) 0.1287(5) 0.8793(6) 0.032(2) Uani 1 1 d . . .
H18A H 0.5803 0.0840 0.9180 0.039 Uiso 1 1 calc R . .
H18B H 0.5510 0.1123 0.8160 0.039 Uiso 1 1 calc R . .
N19 N 0.4890(7) 0.1843(4) 0.8989(5) 0.0222(15) Uani 1 1 d . . .
H19 H 0.4938 0.2267 0.8650 0.027 Uiso 1 1 calc R . .
C20 C 0.3640(9) 0.1566(6) 0.8686(6) 0.035(2) Uani 1 1 d . . .
H20A H 0.3601 0.1029 0.8840 0.042 Uiso 1 1 calc R . .
H20B H 0.3349 0.1621 0.8027 0.042 Uiso 1 1 calc R . .
C21 C 0.2860(9) 0.2041(6) 0.9170(6) 0.037(2) Uani 1 1 d . . .
H21A H 0.2805 0.2564 0.8945 0.044 Uiso 1 1 calc R . .
H21B H 0.2048 0.1830 0.9041 0.044 Uiso 1 1 calc R . .
N22 N 0.3402(7) 0.2034(4) 1.0160(5) 0.0274(16) Uani 1 1 d . . .
C23 C 0.2821(9) 0.2603(6) 1.0613(7) 0.038(2) Uani 1 1 d . . .
H23A H 0.3003 0.3106 1.0429 0.056 Uiso 1 1 calc R . .
H23B H 0.3117 0.2552 1.1265 0.056 Uiso 1 1 calc R . .
H23C H 0.1960 0.2525 1.0444 0.056 Uiso 1 1 calc R . .
C24 C 0.3232(11) 0.1272(6) 1.0556(7) 0.045(3) Uani 1 1 d . . .
H24A H 0.3511 0.1294 1.1211 0.068 Uiso 1 1 calc R . .
H24B H 0.3688 0.0893 1.0323 0.068 Uiso 1 1 calc R . .
H24C H 0.2389 0.1138 1.0388 0.068 Uiso 1 1 calc R . .
C32 C 0.7091(7) 0.0483(5) 1.3193(5) 0.0215(17) Uani 1 1 d . . .
C33 C 0.6136(8) 0.0765(6) 1.3486(6) 0.029(2) Uani 1 1 d . . .
H33 H 0.5950 0.1284 1.3423 0.035 Uiso 1 1 calc R . .
C34 C 0.5443(10) 0.0280(7) 1.3879(7) 0.047(3) Uani 1 1 d . . .
H34 H 0.4783 0.0477 1.4063 0.057 Uiso 1 1 calc R . .
C35 C 0.5717(9) -0.0501(6) 1.4003(7) 0.039(3) Uani 1 1 d . . .
H35 H 0.5249 -0.0825 1.4265 0.047 Uiso 1 1 calc R . .
C36 C 0.6697(9) -0.0772(5) 1.3727(6) 0.029(2) Uani 1 1 d . . .
H36 H 0.6896 -0.1288 1.3808 0.035 Uiso 1 1 calc R . .
C37 C 0.7402(8) -0.0300(5) 1.3328(5) 0.0227(17) Uani 1 1 d . . .
C38 C 0.8449(8) -0.0612(4) 1.3035(5) 0.0222(18) Uani 1 1 d . . .
H38A H 0.8297 -0.0569 1.2374 0.027 Uiso 1 1 calc R . .
H38B H 0.8538 -0.1151 1.3191 0.027 Uiso 1 1 calc R . .
N39 N 0.9593(6) -0.0209(3) 1.3469(4) 0.0202(14) Uani 1 1 d . A .
H39 H 0.9682 -0.0227 1.4085 0.024 Uiso 1 1 calc R . .
C40 C 1.0659(9) -0.0581(5) 1.3282(6) 0.031(2) Uani 1 1 d . . .
H40A H 1.0516 -0.0698 1.2634 0.037 Uiso 1 1 calc R . .
H40B H 1.0838 -0.1054 1.3626 0.037 Uiso 1 1 calc R . .
C41 C 1.1702(8) -0.0024(5) 1.3572(7) 0.033(2) Uani 1 1 d . . .
H41A H 1.1877 0.0062 1.4227 0.039 Uiso 1 1 calc R . .
H41B H 1.2422 -0.0233 1.3429 0.039 Uiso 1 1 calc R . .
N42 N 1.1368(8) 0.0700(4) 1.3081(6) 0.0356(19) Uani 1 1 d . A .
C43 C 1.2204(10) 0.1316(6) 1.3531(11) 0.070(5) Uani 1 1 d . . .
H43A H 1.2373 0.1257 1.4184 0.104 Uiso 1 1 calc R . .
H43B H 1.1834 0.1805 1.3360 0.104 Uiso 1 1 calc R . .
H43C H 1.2946 0.1283 1.3341 0.104 Uiso 1 1 calc R . .
C44 C 1.1462(15) 0.0629(7) 1.2132(10) 0.083(6) Uani 1 1 d . . .
H44A H 1.2285 0.0518 1.2127 0.124 Uiso 1 1 calc R . .
H44B H 1.1215 0.1100 1.1812 0.124 Uiso 1 1 calc R . .
H44C H 1.0946 0.0222 1.1834 0.124 Uiso 1 1 calc R . .
O11 O 0.6990(5) 0.2023(3) 1.0492(4) 0.0243(13) Uani 1 1 d . A .
O31 O 0.7800(5) 0.0968(3) 1.2834(4) 0.0238(13) Uani 1 1 d . A .
Cu3 Cu 0.73698(9) 0.14274(5) 1.16228(6) 0.0188(2) Uani 1 1 d . . .
Cu2 Cu 0.95908(9) 0.08950(5) 1.31189(7) 0.0190(2) Uani 1 1 d . . .
Cu1 Cu 0.52237(9) 0.21877(5) 1.02924(6) 0.0185(2) Uani 1 1 d . A .
Cl1 Cl 0.57262(19) 0.22659(13) 1.18721(13) 0.0260(4) Uani 1 1 d . A .
Cl2 Cl 0.9413(2) 0.20056(12) 1.22581(14) 0.0265(5) Uani 1 1 d . A .
Cl4 Cl 0.50236(19) 0.36229(11) 0.97635(13) 0.0231(4) Uani 1 1 d . . .
Cl3a Cl 0.7776(5) 0.0329(2) 1.0919(3) 0.0339(8) Uani 0.543(4) 1 d P A 1
Cl3b Cl 0.6443(5) 0.0411(2) 1.0941(3) 0.0339(8) Uani 0.457(4) 1 d P A 2
O81 O 0.919(3) -0.0134(17) 1.107(2) 0.101(8) Uiso 0.457(4) 1 d PD A 2
H81 H 0.850(16) -0.01(2) 1.07(2) 0.121 Uiso 0.457(4) 1 d PD A 2
C82 C 0.955(4) 0.014(2) 1.022(3) 0.098(13) Uiso 0.457(4) 1 d P A 2
H82A H 1.0098 0.0560 1.0372 0.117 Uiso 0.457(4) 1 calc PR A 2
H82B H 0.8840 0.0292 0.9764 0.117 Uiso 0.457(4) 1 calc PR A 2
H82C H 0.9940 -0.0275 0.9981 0.117 Uiso 0.457(4) 1 calc PR A 2
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'
O O 0.0106 0.0060 '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'
Cu Cu 0.3201 1.2651 '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'
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
O11 C12 C13 118.5(8) . . ?
O11 C12 C17 121.4(9) . . ?
C13 C12 C17 120.0(8) . . ?
C14 C13 C12 121.0(9) . . ?
C13 C14 C15 120.2(10) . . ?
C16 C15 C14 118.7(9) . . ?
C15 C16 C17 123.5(10) . . ?
C12 C17 C16 116.6(10) . . ?
C12 C17 C18 121.6(8) . . ?
C16 C17 C18 121.8(9) . . ?
C17 C18 N19 110.9(7) . . ?
C20 N19 C18 112.2(7) . . ?
C20 N19 Cu1 109.7(5) . . ?
C18 N19 Cu1 115.0(5) . . ?
N19 C20 C21 108.0(7) . . ?
N22 C21 C20 109.5(8) . . ?
C23 N22 C21 110.3(8) . . ?
C23 N22 C24 107.6(8) . . ?
C21 N22 C24 110.6(7) . . ?
C23 N22 Cu1 115.7(6) . . ?
C21 N22 Cu1 104.9(5) . . ?
C24 N22 Cu1 107.9(6) . . ?
C33 C32 O31 120.1(8) . . ?
C33 C32 C37 119.6(8) . . ?
O31 C32 C37 120.2(8) . . ?
C32 C33 C34 120.1(9) . . ?
C33 C34 C35 121.3(10) . . ?
C36 C35 C34 117.8(9) . . ?
C35 C36 C37 122.0(9) . . ?
C36 C37 C32 119.0(8) . . ?
C36 C37 C38 120.6(8) . . ?
C32 C37 C38 120.4(7) . . ?
C37 C38 N39 112.4(6) . . ?
C40 N39 C38 112.6(6) . . ?
C40 N39 Cu2 108.9(5) . . ?
C38 N39 Cu2 113.5(5) . . ?
N39 C40 C41 106.8(7) . . ?
N42 C41 C40 108.8(8) . . ?
C44 N42 C41 110.2(8) . . ?
C44 N42 C43 108.3(10) . . ?
C41 N42 C43 109.8(9) . . ?
C44 N42 Cu2 110.6(8) . . ?
C41 N42 Cu2 105.1(6) . . ?
C43 N42 Cu2 112.9(6) . . ?
C12 O11 Cu3 126.6(5) . . ?
C12 O11 Cu1 123.5(5) . . ?
Cu3 O11 Cu1 101.9(3) . . ?
C32 O31 Cu3 126.2(5) . . ?
C32 O31 Cu2 123.5(5) . . ?
Cu3 O31 Cu2 103.6(3) . . ?
O31 Cu3 O11 172.2(3) . . ?
O31 Cu3 Cl3b 94.8(2) . . ?
O11 Cu3 Cl3b 92.7(2) . . ?
O31 Cu3 Cl3a 93.2(2) . . ?
O11 Cu3 Cl3a 93.9(2) . . ?
Cl3b Cu3 Cl3a 40.0(2) . . ?
O31 Cu3 Cl1 97.18(19) . . ?
O11 Cu3 Cl1 78.84(18) . . ?
Cl3b Cu3 Cl1 104.87(17) . . ?
Cl3a Cu3 Cl1 144.24(14) . . ?
O31 Cu3 Cl2 79.33(18) . . ?
O11 Cu3 Cl2 95.80(19) . . ?
Cl3b Cu3 Cl2 143.37(17) . . ?
Cl3a Cu3 Cl2 103.80(14) . . ?
Cl1 Cu3 Cl2 111.72(8) . . ?
O31 Cu3 Cu1 140.39(19) . . ?
O11 Cu3 Cu1 39.44(18) . . ?
Cl3b Cu3 Cu1 80.29(14) . . ?
Cl3a Cu3 Cu1 106.37(12) . . ?
Cl1 Cu3 Cu1 47.99(5) . . ?
Cl2 Cu3 Cu1 126.35(6) . . ?
O31 Cu2 N39 93.0(3) . . ?
O31 Cu2 N42 165.2(3) . . ?
N39 Cu2 N42 85.0(3) . . ?
O31 Cu2 Cl2 83.31(17) . . ?
N39 Cu2 Cl2 161.9(2) . . ?
N42 Cu2 Cl2 94.1(2) . . ?
O31 Cu2 Cl4 97.38(17) . 4_666 ?
N39 Cu2 Cl4 94.32(19) . 4_666 ?
N42 Cu2 Cl4 97.4(3) . 4_666 ?
Cl2 Cu2 Cl4 103.70(8) . 4_666 ?
O11 Cu1 N19 92.4(3) . . ?
O11 Cu1 N22 163.8(3) . . ?
N19 Cu1 N22 85.8(3) . . ?
O11 Cu1 Cl1 82.61(17) . . ?
N19 Cu1 Cl1 165.6(2) . . ?
N22 Cu1 Cl1 95.3(2) . . ?
O11 Cu1 Cl4 101.14(17) . . ?
N19 Cu1 Cl4 90.49(19) . . ?
N22 Cu1 Cl4 95.0(2) . . ?
Cl1 Cu1 Cl4 103.71(8) . . ?
O11 Cu1 Cu3 38.71(15) . . ?
N19 Cu1 Cu3 116.0(2) . . ?
N22 Cu1 Cu3 129.2(2) . . ?
Cl1 Cu1 Cu3 52.92(6) . . ?
Cl4 Cu1 Cu3 127.59(6) . . ?
Cu1 Cl1 Cu3 79.09(7) . . ?
Cu2 Cl2 Cu3 79.54(7) . . ?
Cu2 Cl4 Cu1 126.35(8) 4_565 . ?
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
C12 O11 1.351(10) . ?
C12 C13 1.392(14) . ?
C12 C17 1.410(12) . ?
C13 C14 1.382(12) . ?
C14 C15 1.392(14) . ?
C15 C16 1.362(15) . ?
C16 C17 1.411(13) . ?
C17 C18 1.478(14) . ?
C18 N19 1.480(11) . ?
N19 C20 1.465(11) . ?
N19 Cu1 1.999(7) . ?
C20 C21 1.529(13) . ?
C21 N22 1.466(11) . ?
N22 C23 1.455(12) . ?
N22 C24 1.492(12) . ?
N22 Cu1 2.054(8) . ?
C32 C33 1.366(12) . ?
C32 O31 1.372(10) . ?
C32 C37 1.416(12) . ?
C33 C34 1.389(14) . ?
C34 C35 1.402(15) . ?
C35 C36 1.371(14) . ?
C36 C37 1.389(12) . ?
C37 C38 1.477(12) . ?
C38 N39 1.482(10) . ?
N39 C40 1.467(11) . ?
N39 Cu2 2.000(6) . ?
C40 C41 1.515(13) . ?
C41 N42 1.468(12) . ?
N42 C44 1.466(15) . ?
N42 C43 1.484(13) . ?
N42 Cu2 2.070(8) . ?
O11 Cu3 1.951(5) . ?
O11 Cu1 1.981(6) . ?
O31 Cu3 1.942(5) . ?
O31 Cu2 1.982(6) . ?
Cu3 Cl3b 2.187(5) . ?
Cu3 Cl3a 2.296(4) . ?
Cu3 Cl1 2.480(2) . ?
Cu3 Cl2 2.500(2) . ?
Cu3 Cu1 3.0525(14) . ?
Cu2 Cl2 2.315(2) . ?
Cu2 Cl4 2.547(2) 4_666 ?
Cu1 Cl1 2.310(2) . ?
Cu1 Cl4 2.624(2) . ?
Cl4 Cu2 2.547(2) 4_565 ?
O81 C82 1.52(5) . ?
