#------------------------------------------------------------------------------
#$Date: 2016-03-23 03:24:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179244 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/64/4316449.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_4316449
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 H34 Cl2 Cu3 N10 O2'
_chemical_formula_weight         732.11
_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                 110.392(6)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.5818(6)
_cell_length_b                   16.2364(9)
_cell_length_c                   16.2417(9)
_cell_measurement_reflns_used    19017
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.00
_cell_measurement_theta_min      2.26
_cell_volume                     2862.8(3)
_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 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0586
_diffrn_reflns_av_sigmaI/netI    0.1151
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            19017
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         2.26
_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    2.436
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'ABSPACK, Oxford Diffraction Ltd'
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.699
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1492
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.834
_refine_diff_density_min         -0.830
_refine_diff_density_rms         0.112
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.832
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     356
_refine_ls_number_reflns         8292
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.832
_refine_ls_R_factor_all          0.0888
_refine_ls_R_factor_gt           0.0418
_refine_ls_shift/su_max          0.001
_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)+(0.0300P)²+0.0000P] where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0760
_refine_ls_wR_factor_ref         0.0818
_reflns_number_gt                4705
_reflns_number_total             8292
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic101183n_si_001_1.cif
_cod_data_source_block           1
_cod_database_code               4316449
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
Cu1 Cu 0.47107(3) 0.61984(2) 0.84686(2) 0.01706(10) Uani 1 1 d . . .
Cu2 Cu 0.14654(3) 0.84814(2) 0.78440(2) 0.01717(10) Uani 1 1 d . . .
Cu3 Cu 0.23868(3) 0.69619(3) 0.70612(2) 0.02027(10) Uani 1 1 d . . .
Cl1 Cl 0.14827(8) 0.63488(5) 0.57729(5) 0.0284(2) Uani 1 1 d . . .
Cl2 Cl 0.03553(7) 0.96423(5) 0.66971(5) 0.02285(18) Uani 1 1 d . . .
C12 C 0.2435(3) 0.61824(19) 0.88354(19) 0.0162(7) Uani 1 1 d . . .
C13 C 0.1295(3) 0.57902(19) 0.8560(2) 0.0188(7) Uani 1 1 d . . .
H13 H 0.0941 0.5618 0.7980 0.023 Uiso 1 1 calc R . .
C14 C 0.0692(3) 0.5656(2) 0.9140(2) 0.0219(8) Uani 1 1 d . . .
H14 H -0.0068 0.5391 0.8949 0.026 Uiso 1 1 calc R . .
C15 C 0.1196(3) 0.5908(2) 1.0003(2) 0.0260(8) Uani 1 1 d . . .
H15 H 0.0764 0.5839 1.0386 0.031 Uiso 1 1 calc R . .
C16 C 0.2346(3) 0.6262(2) 1.0289(2) 0.0224(8) Uani 1 1 d . . .
H16 H 0.2706 0.6412 1.0875 0.027 Uiso 1 1 calc R . .
C17 C 0.2979(3) 0.63995(19) 0.97155(19) 0.0166(7) Uani 1 1 d . . .
C18 C 0.4245(3) 0.6768(2) 1.0026(2) 0.0218(8) Uani 1 1 d . . .
H18A H 0.4219 0.7309 0.9766 0.026 Uiso 1 1 calc R . .
H18B H 0.4535 0.6832 1.0659 0.026 Uiso 1 1 calc R . .
C20 C 0.6412(3) 0.6462(2) 1.0204(2) 0.0254(8) Uani 1 1 d . . .
H20A H 0.6725 0.6250 1.0799 0.031 Uiso 1 1 calc R . .
H20B H 0.6499 0.7056 1.0227 0.031 Uiso 1 1 calc R . .
C21 C 0.7116(3) 0.6097(2) 0.9672(2) 0.0223(8) Uani 1 1 d . . .
H21A H 0.7966 0.6279 0.9904 0.027 Uiso 1 1 calc R . .
H21B H 0.7104 0.5501 0.9707 0.027 Uiso 1 1 calc R . .
C23 C 0.7080(3) 0.5881(3) 0.8197(2) 0.0367(10) Uani 1 1 d . . .
H23A H 0.7945 0.5998 0.8371 0.055 Uiso 1 1 calc R . .
H23B H 0.6680 0.6027 0.7591 0.055 Uiso 1 1 calc R . .
H23C H 0.6964 0.5304 0.8273 0.055 Uiso 1 1 calc R . .
C24 C 0.6770(3) 0.7250(2) 0.8653(3) 0.0366(10) Uani 1 1 d . . .
H24A H 0.6399 0.7566 0.8995 0.055 Uiso 1 1 calc R . .
H24B H 0.6416 0.7408 0.8047 0.055 Uiso 1 1 calc R . .
H24C H 0.7641 0.7352 0.8859 0.055 Uiso 1 1 calc R . .
C32 C 0.3894(3) 0.86063(19) 0.7650(2) 0.0165(7) Uani 1 1 d . . .
C33 C 0.4538(3) 0.8550(2) 0.7069(2) 0.0204(7) Uani 1 1 d . . .
H33 H 0.4234 0.8218 0.6573 0.024 Uiso 1 1 calc R . .
C34 C 0.5620(3) 0.8979(2) 0.7220(2) 0.0237(8) Uani 1 1 d . . .
H34 H 0.6061 0.8913 0.6843 0.028 Uiso 1 1 calc R . .
C35 C 0.6051(3) 0.9504(2) 0.7928(2) 0.0277(9) Uani 1 1 d . . .
H35 H 0.6765 0.9808 0.8016 0.033 Uiso 1 1 calc R . .
C36 C 0.5425(3) 0.9577(2) 0.8502(2) 0.0230(8) Uani 1 1 d . . .
H36 H 0.5720 0.9933 0.8979 0.028 Uiso 1 1 calc R . .
C37 C 0.4353(3) 0.9128(2) 0.8382(2) 0.0185(7) Uani 1 1 d . . .
C38 C 0.3749(3) 0.9179(2) 0.9050(2) 0.0199(7) Uani 1 1 d . . .
H38A H 0.3869 0.8662 0.9368 0.024 Uiso 1 1 calc R . .
H38B H 0.4144 0.9609 0.9468 0.024 Uiso 1 1 calc R . .
C40 C 0.1869(3) 0.9507(2) 0.9347(2) 0.0246(8) Uani 1 1 d . . .
H40A H 0.2040 1.0068 0.9563 0.029 Uiso 1 1 calc R . .
H40B H 0.2218 0.9134 0.9837 0.029 Uiso 1 1 calc R . .
C41 C 0.0499(3) 0.9375(2) 0.8944(2) 0.0235(8) Uani 1 1 d . . .
H41A H 0.0134 0.9393 0.9398 0.028 Uiso 1 1 calc R . .
H41B H 0.0133 0.9810 0.8525 0.028 Uiso 1 1 calc R . .
C43 C -0.1063(3) 0.8536(2) 0.7945(2) 0.0269(8) Uani 1 1 d . . .
H43A H -0.1257 0.7999 0.7686 0.040 Uiso 1 1 calc R . .
H43B H -0.1231 0.8942 0.7490 0.040 Uiso 1 1 calc R . .
H43C H -0.1557 0.8645 0.8300 0.040 Uiso 1 1 calc R . .
C44 C 0.0506(3) 0.7886(2) 0.9140(2) 0.0264(8) Uani 1 1 d . . .
H44A H 0.0016 0.7954 0.9505 0.040 Uiso 1 1 calc R . .
H44B H 0.1363 0.7890 0.9498 0.040 Uiso 1 1 calc R . .
H44C H 0.0305 0.7370 0.8833 0.040 Uiso 1 1 calc R . .
O11 O 0.29918(18) 0.63447(14) 0.82586(13) 0.0198(5) Uani 1 1 d . . .
O31 O 0.28675(18) 0.81628(13) 0.75176(13) 0.0195(5) Uani 1 1 d . . .
N1 N 0.4098(2) 0.65981(17) 0.72045(16) 0.0215(6) Uani 1 1 d . . .
N2 N 0.4482(2) 0.65326(18) 0.66171(19) 0.0241(6) Uani 1 1 d . . .
N3 N 0.4843(3) 0.6482(2) 0.6048(2) 0.0431(9) Uani 1 1 d . . .
N4 N 0.0873(2) 0.74255(16) 0.72023(16) 0.0198(6) Uani 1 1 d . . .
N5 N -0.0127(3) 0.70889(18) 0.69064(18) 0.0251(7) Uani 1 1 d . . .
N6 N -0.1064(3) 0.6781(2) 0.6618(2) 0.0451(9) Uani 1 1 d . . .
N19 N 0.5105(2) 0.62323(17) 0.97776(15) 0.0187(6) Uani 1 1 d . . .
H19 H 0.5015 0.5712 0.9954 0.022 Uiso 1 1 calc R . .
N22 N 0.6545(2) 0.63623(17) 0.87431(16) 0.0203(6) Uani 1 1 d . . .
N39 N 0.2418(2) 0.93532(16) 0.86706(16) 0.0186(6) Uani 1 1 d . . .
H39 H 0.2332 0.9825 0.8353 0.022 Uiso 1 1 calc R . .
N42 N 0.0249(2) 0.85679(16) 0.84963(16) 0.0175(6) Uani 1 1 d . . .
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 Cu1 N19 91.38(9) . . ?
O11 Cu1 N22 165.16(10) . . ?
N19 Cu1 N22 85.95(10) . . ?
O11 Cu1 N1 78.73(9) . . ?
N19 Cu1 N1 158.34(11) . . ?
N22 Cu1 N1 98.66(10) . . ?
O11 Cu1 Cl2 96.52(7) . 2_546 ?
N19 Cu1 Cl2 97.27(8) . 2_546 ?
N22 Cu1 Cl2 98.29(8) . 2_546 ?
N1 Cu1 Cl2 102.93(8) . 2_546 ?
O31 Cu2 N39 93.07(9) . . ?
O31 Cu2 N4 78.31(9) . . ?
N39 Cu2 N4 165.16(10) . . ?
O31 Cu2 N42 162.21(9) . . ?
N39 Cu2 N42 85.52(10) . . ?
N4 Cu2 N42 98.97(11) . . ?
O31 Cu2 Cl2 104.15(7) . . ?
N39 Cu2 Cl2 89.28(8) . . ?
N4 Cu2 Cl2 104.45(7) . . ?
N42 Cu2 Cl2 93.57(7) . . ?
N4 Cu3 N1 166.57(11) . . ?
N4 Cu3 O11 95.60(9) . . ?
N1 Cu3 O11 75.63(9) . . ?
N4 Cu3 O31 75.13(9) . . ?
N1 Cu3 O31 95.93(10) . . ?
O11 Cu3 O31 98.99(8) . . ?
N4 Cu3 Cl1 97.63(8) . . ?
N1 Cu3 Cl1 95.73(8) . . ?
O11 Cu3 Cl1 124.00(7) . . ?
O31 Cu3 Cl1 136.99(6) . . ?
Cu1 Cl2 Cu2 140.57(3) 2_556 . ?
O11 C12 C17 120.9(3) . . ?
O11 C12 C13 120.0(3) . . ?
C17 C12 C13 119.0(3) . . ?
C14 C13 C12 120.3(3) . . ?
C13 C14 C15 120.9(3) . . ?
C16 C15 C14 118.9(3) . . ?
C15 C16 C17 121.1(3) . . ?
C12 C17 C16 119.5(3) . . ?
C12 C17 C18 119.1(3) . . ?
C16 C17 C18 121.5(3) . . ?
N19 C18 C17 110.3(3) . . ?
N19 C20 C21 107.7(3) . . ?
N22 C21 C20 109.4(2) . . ?
O31 C32 C33 120.6(3) . . ?
O31 C32 C37 120.8(3) . . ?
C33 C32 C37 118.6(3) . . ?
C34 C33 C32 120.8(3) . . ?
C35 C34 C33 120.3(3) . . ?
C34 C35 C36 119.8(3) . . ?
C35 C36 C37 121.1(3) . . ?
C36 C37 C32 119.3(3) . . ?
C36 C37 C38 119.5(3) . . ?
C32 C37 C38 121.1(3) . . ?
N39 C38 C37 113.4(2) . . ?
N39 C40 C41 108.4(3) . . ?
N42 C41 C40 109.7(3) . . ?
C12 O11 Cu1 125.25(18) . . ?
C12 O11 Cu3 131.53(18) . . ?
Cu1 O11 Cu3 102.53(10) . . ?
C32 O31 Cu2 126.2(2) . . ?
C32 O31 Cu3 131.97(19) . . ?
Cu2 O31 Cu3 101.54(9) . . ?
N2 N1 Cu3 124.4(2) . . ?
N2 N1 Cu1 133.3(2) . . ?
Cu3 N1 Cu1 101.25(12) . . ?
N3 N2 N1 178.9(4) . . ?
N5 N4 Cu3 122.6(2) . . ?
N5 N4 Cu2 134.2(2) . . ?
Cu3 N4 Cu2 103.18(11) . . ?
N6 N5 N4 178.9(4) . . ?
C20 N19 C18 113.7(2) . . ?
C20 N19 Cu1 108.7(2) . . ?
C18 N19 Cu1 112.15(18) . . ?
C23 N22 C24 109.4(3) . . ?
C23 N22 C21 109.1(3) . . ?
C24 N22 C21 110.6(3) . . ?
C23 N22 Cu1 115.2(2) . . ?
C24 N22 Cu1 108.21(19) . . ?
C21 N22 Cu1 104.26(18) . . ?
C40 N39 C38 112.5(2) . . ?
C40 N39 Cu2 109.97(19) . . ?
C38 N39 Cu2 113.39(19) . . ?
C43 N42 C44 108.3(3) . . ?
C43 N42 C41 108.3(2) . . ?
C44 N42 C41 111.1(2) . . ?
C43 N42 Cu2 115.8(2) . . ?
C44 N42 Cu2 108.02(19) . . ?
C41 N42 Cu2 105.29(19) . . ?
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
Cu1 O11 1.914(2) . ?
Cu1 N19 2.014(2) . ?
Cu1 N22 2.031(2) . ?
Cu1 N1 2.031(3) . ?
Cu1 Cl2 2.5392(9) 2_546 ?
Cu2 O31 1.946(2) . ?
Cu2 N39 1.998(2) . ?
Cu2 N4 2.000(3) . ?
Cu2 N42 2.042(3) . ?
Cu2 Cl2 2.6470(9) . ?
Cu3 N4 1.993(3) . ?
Cu3 N1 2.002(3) . ?
Cu3 O11 2.080(2) . ?
Cu3 O31 2.091(2) . ?
Cu3 Cl1 2.2223(9) . ?
Cl2 Cu1 2.5391(9) 2_556 ?
C12 O11 1.336(4) . ?
C12 C17 1.392(4) . ?
C12 C13 1.392(4) . ?
C13 C14 1.372(4) . ?
C14 C15 1.380(4) . ?
C15 C16 1.375(4) . ?
C16 C17 1.389(4) . ?
C17 C18 1.500(4) . ?
C18 N19 1.480(4) . ?
C20 N19 1.476(4) . ?
C20 C21 1.501(4) . ?
C21 N22 1.484(4) . ?
C23 N22 1.471(4) . ?
C24 N22 1.481(4) . ?
C32 O31 1.342(3) . ?
C32 C33 1.396(4) . ?
C32 C37 1.406(4) . ?
C33 C34 1.379(4) . ?
C34 C35 1.377(5) . ?
C35 C36 1.372(5) . ?
C36 C37 1.394(4) . ?
C37 C38 1.483(4) . ?
C38 N39 1.474(4) . ?
C40 N39 1.470(4) . ?
C40 C41 1.507(4) . ?
C41 N42 1.478(4) . ?
C43 N42 1.471(4) . ?
C44 N42 1.480(4) . ?
N1 N2 1.190(4) . ?
N2 N3 1.142(4) . ?
N4 N5 1.218(3) . ?
N5 N6 1.137(4) . ?
