#------------------------------------------------------------------------------
#$Date: 2016-03-25 23:02:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 180023 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/17/7031745.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_7031745
loop_
_publ_author_name
'Dai, Yuan'
'Wang, Yin-Ge'
'Geng, Jiao'
'Peng, Yu-Xin'
'Huang, Wei'
_publ_section_title
;
 Dinuclear Cu(ii) complexes based on two flexible Schiff-base ligands and
 one unusual in situ formed diphenolate 2,6-piperidin-4-one derivative.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13831
_journal_page_last               13834
_journal_paper_doi               10.1039/c4dt01014k
_journal_volume                  43
_journal_year                    2014
_chemical_formula_moiety         'C50 H50 Cl8 Cu2 N6 O8, 2 (H2 O)'
_chemical_formula_sum            'C50 H54 Cl8 Cu2 N6 O10'
_chemical_formula_weight         1309.67
_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                 99.404(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.722(7)
_cell_length_b                   18.004(13)
_cell_length_c                   18.378(14)
_cell_measurement_reflns_used    2477
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      20.271
_cell_measurement_theta_min      2.436
_cell_volume                     2847(4)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (BRUKER 2000)'
_computing_data_reduction        'SAINT (BRUKER 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (BRUKER 2000)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'BRUKER Smart Apex CCD area detector'
_diffrn_measurement_method       'φ and ω scans'
_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  0.1176
_diffrn_reflns_av_sigmaI/netI    0.1344
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13440
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.26
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_T_max  0.8909
_exptl_absorpt_correction_T_min  0.8333
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, BRUKER(2000)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1340
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.420
_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.871
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         4936
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.871
_refine_ls_R_factor_all          0.1325
_refine_ls_R_factor_gt           0.0628
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0713P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1491
_refine_ls_wR_factor_ref         0.1700
_reflns_number_gt                2309
_reflns_number_total             4936
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4dt01014k2.cif
_cod_data_source_block           complex_3
_cod_depositor_comments
'Adding full bibliography for 7031743--7031745.cif.'
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7031745
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
Cu1 Cu 0.18186(7) 0.12970(4) 1.00283(4) 0.0654(3) Uani 1 1 d .
C1 C 0.0941(7) 0.0753(3) 0.8551(3) 0.0674(15) Uani 1 1 d .
C2 C -0.0028(7) 0.1350(3) 0.8284(3) 0.0674(15) Uani 1 1 d .
C3 C -0.1065(7) 0.1310(4) 0.7642(3) 0.0775(17) Uani 1 1 d .
H3 H -0.1657 0.1724 0.7474 0.093 Uiso 1 1 calc R
C4 C -0.1234(8) 0.0662(4) 0.7246(3) 0.0850(18) Uani 1 1 d .
C5 C -0.0356(8) 0.0058(4) 0.7475(3) 0.0827(18) Uani 1 1 d .
H5 H -0.0468 -0.0377 0.7199 0.099 Uiso 1 1 calc R
C6 C 0.0693(7) 0.0093(4) 0.8113(3) 0.0786(17) Uani 1 1 d .
C7 C 0.0232(6) 0.2094(3) 0.8692(3) 0.0661(14) Uani 1 1 d .
H7 H -0.0607 0.2432 0.8484 0.079 Uiso 1 1 calc R
C8 C 0.0976(8) 0.2284(3) 1.1138(4) 0.0752(16) Uani 1 1 d .
C9 C 0.0036(7) 0.2736(3) 1.0634(3) 0.0714(15) Uani 1 1 d .
C10 C -0.1020(8) 0.3221(3) 1.0882(4) 0.0873(18) Uani 1 1 d .
H10 H -0.1637 0.3526 1.0546 0.105 Uiso 1 1 calc R
C11 C -0.1157(9) 0.3251(4) 1.1614(4) 0.091(2) Uani 1 1 d .
C12 C -0.0262(9) 0.2810(4) 1.2125(4) 0.093(2) Uani 1 1 d .
H12 H -0.0358 0.2838 1.2621 0.112 Uiso 1 1 calc R
C13 C 0.0792(8) 0.2320(3) 1.1890(3) 0.0810(17) Uani 1 1 d .
C14 C 0.0262(7) 0.2770(3) 0.9843(3) 0.0719(15) Uani 1 1 d .
H14 H -0.0565 0.3078 0.9571 0.086 Uiso 1 1 calc R
C15 C 0.3357(6) -0.0153(4) 1.0249(3) 0.0659(14) Uani 1 1 d .
H15 H 0.3180 -0.0241 0.9743 0.079 Uiso 1 1 calc R
C16 C 0.4014(7) -0.0324(4) 1.1421(4) 0.0893(19) Uani 1 1 d .
H16 H 0.4372 -0.0541 1.1877 0.107 Uiso 1 1 calc R
C17 C 0.3482(8) 0.0359(4) 1.1301(4) 0.094(2) Uani 1 1 d .
H17 H 0.3405 0.0705 1.1669 0.112 Uiso 1 1 calc R
C18 C -0.4167(6) 0.1435(3) 0.9414(3) 0.0783(17) Uani 1 1 d .
H18A H -0.4247 0.1490 0.9931 0.094 Uiso 1 1 calc R
H18B H -0.5135 0.1605 0.9125 0.094 Uiso 1 1 calc R
C19 C -0.2838(6) 0.1910(3) 0.9237(3) 0.0700(15) Uani 1 1 d .
H19A H -0.2961 0.2414 0.9404 0.084 Uiso 1 1 calc R
H19B H -0.2866 0.1922 0.8707 0.084 Uiso 1 1 calc R
C20 C -0.1262(6) 0.1601(3) 0.9614(3) 0.0619(13) Uani 1 1 d .
H20A H -0.1273 0.1584 1.0140 0.074 Uiso 1 1 calc R
H20B H -0.1182 0.1092 0.9449 0.074 Uiso 1 1 calc R
C21 C 0.1777(7) 0.2445(3) 0.8582(3) 0.0786(17) Uani 1 1 d .
H21A H 0.2613 0.2096 0.8740 0.094 Uiso 1 1 calc R
H21B H 0.1754 0.2545 0.8062 0.094 Uiso 1 1 calc R
C22 C 0.1823(7) 0.3114(3) 0.9767(4) 0.0868(18) Uani 1 1 d .
H22A H 0.1869 0.3614 0.9967 0.104 Uiso 1 1 calc R
H22B H 0.2646 0.2827 1.0056 0.104 Uiso 1 1 calc R
C23 C 0.2092(8) 0.3145(4) 0.9003(4) 0.0900(19) Uani 1 1 d .
C24 C 0.4241(15) 0.4004(9) 0.9348(7) 0.245(7) Uani 1 1 d .
H24A H 0.3529 0.4413 0.9254 0.368 Uiso 1 1 calc R
H24B H 0.5217 0.4139 0.9209 0.368 Uiso 1 1 calc R
H24C H 0.4395 0.3885 0.9864 0.368 Uiso 1 1 calc R
C25 C 0.1057(15) 0.3911(7) 0.7990(5) 0.199(5) Uani 1 1 d .
H25A H 0.2104 0.3996 0.7911 0.298 Uiso 1 1 calc R
H25B H 0.0456 0.4355 0.7877 0.298 Uiso 1 1 calc R
H25C H 0.0607 0.3515 0.7676 0.298 Uiso 1 1 calc R
Cl1 Cl -0.2579(3) 0.05957(13) 0.64436(11) 0.1406(8) Uani 1 1 d .
Cl2 Cl 0.1784(2) -0.06880(9) 0.84220(9) 0.1060(6) Uani 1 1 d .
Cl3 Cl -0.2474(3) 0.38631(12) 1.18988(12) 0.1358(8) Uani 1 1 d .
Cl4 Cl 0.1919(2) 0.17788(10) 1.25197(9) 0.1019(6) Uani 1 1 d .
N1 N 0.3059(5) 0.0491(3) 1.0562(3) 0.0705(12) Uani 1 1 d .
N2 N 0.3933(5) -0.0646(3) 1.0749(3) 0.0707(12) Uani 1 1 d .
N3 N 0.0168(5) 0.1999(2) 0.9496(2) 0.0604(11) Uani 1 1 d .
O1 O 0.1957(5) 0.0770(2) 0.9156(2) 0.0771(11) Uani 1 1 d .
O3 O 0.2010(5) 0.1822(2) 1.0933(2) 0.0811(11) Uani 1 1 d .
O5 O 0.1062(7) 0.3723(3) 0.8704(3) 0.1337(19) Uani 1 1 d .
O6 O 0.3593(7) 0.3350(3) 0.8914(3) 0.143(2) Uani 1 1 d .
O7 O 0.4735(10) 0.7789(6) 0.8885(7) 0.308(6) Uani 1 1 d .
H7A H 0.5052 0.7909 0.9332 0.462 Uiso 1 1 d R
H7B H 0.5490 0.7796 0.8646 0.462 Uiso 1 1 d R
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 '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'
Cl Cl 0.1484 0.1585 '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'
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
O1 Cu1 O3 171.39(18) . .
O1 Cu1 N1 86.94(19) . .
O3 Cu1 N1 88.18(19) . .
O1 Cu1 N3 92.42(16) . .
O3 Cu1 N3 93.76(17) . .
N1 Cu1 N3 168.63(17) . .
O1 C1 C2 124.4(5) . .
O1 C1 C6 121.2(5) . .
C2 C1 C6 114.3(6) . .
C3 C2 C1 122.5(6) . .
C3 C2 C7 119.4(5) . .
C1 C2 C7 117.7(5) . .
C2 C3 C4 120.1(6) . .
C2 C3 H3 120.0 . .
C4 C3 H3 120.0 . .
C5 C4 C3 120.7(6) . .
C5 C4 Cl1 118.6(6) . .
C3 C4 Cl1 120.6(5) . .
C4 C5 C6 119.7(6) . .
C4 C5 H5 120.2 . .
C6 C5 H5 120.2 . .
C5 C6 C1 122.6(6) . .
C5 C6 Cl2 119.8(5) . .
C1 C6 Cl2 117.6(5) . .
N3 C7 C21 110.6(4) . .
N3 C7 C2 110.8(4) . .
C21 C7 C2 111.1(4) . .
N3 C7 H7 108.1 . .
C21 C7 H7 108.1 . .
C2 C7 H7 108.1 . .
O3 C8 C9 122.1(6) . .
O3 C8 C13 119.7(6) . .
C9 C8 C13 118.2(6) . .
C8 C9 C10 119.7(6) . .
C8 C9 C14 120.8(5) . .
C10 C9 C14 119.2(6) . .
C11 C10 C9 120.8(6) . .
C11 C10 H10 119.6 . .
C9 C10 H10 119.6 . .
C10 C11 C12 121.2(6) . .
C10 C11 Cl3 119.3(7) . .
C12 C11 Cl3 119.5(6) . .
C11 C12 C13 119.0(6) . .
C11 C12 H12 120.5 . .
C13 C12 H12 120.5 . .
C12 C13 C8 121.1(7) . .
C12 C13 Cl4 119.4(5) . .
C8 C13 Cl4 119.5(5) . .
C9 C14 C22 111.5(5) . .
C9 C14 N3 111.2(4) . .
C22 C14 N3 108.6(4) . .
C9 C14 H14 108.5 . .
C22 C14 H14 108.5 . .
N3 C14 H14 108.5 . .
N2 C15 N1 111.3(5) . .
N2 C15 H15 124.4 . .
N1 C15 H15 124.4 . .
C17 C16 N2 106.3(6) . .
C17 C16 H16 126.8 . .
N2 C16 H16 126.8 . .
C16 C17 N1 111.0(6) . .
C16 C17 H17 124.5 . .
N1 C17 H17 124.5 . .
N2 C18 C19 111.3(4) 3_557 .
N2 C18 H18A 109.4 3_557 .
C19 C18 H18A 109.4 . .
N2 C18 H18B 109.4 3_557 .
C19 C18 H18B 109.4 . .
H18A C18 H18B 108.0 . .
C18 C19 C20 111.0(4) . .
C18 C19 H19A 109.4 . .
C20 C19 H19A 109.4 . .
C18 C19 H19B 109.4 . .
C20 C19 H19B 109.4 . .
H19A C19 H19B 108.0 . .
N3 C20 C19 118.0(4) . .
N3 C20 H20A 107.8 . .
C19 C20 H20A 107.8 . .
N3 C20 H20B 107.8 . .
C19 C20 H20B 107.8 . .
H20A C20 H20B 107.1 . .
C23 C21 C7 112.0(5) . .
C23 C21 H21A 109.2 . .
C7 C21 H21A 109.2 . .
C23 C21 H21B 109.2 . .
C7 C21 H21B 109.2 . .
H21A C21 H21B 107.9 . .
C23 C22 C14 113.0(5) . .
C23 C22 H22A 109.0 . .
C14 C22 H22A 109.0 . .
C23 C22 H22B 109.0 . .
C14 C22 H22B 109.0 . .
H22A C22 H22B 107.8 . .
O6 C23 O5 107.8(5) . .
O6 C23 C22 115.1(6) . .
O5 C23 C22 102.0(6) . .
O6 C23 C21 105.1(6) . .
O5 C23 C21 111.6(6) . .
C22 C23 C21 115.1(5) . .
O6 C24 H24A 109.5 . .
O6 C24 H24B 109.5 . .
H24A C24 H24B 109.5 . .
O6 C24 H24C 109.5 . .
H24A C24 H24C 109.5 . .
H24B C24 H24C 109.5 . .
O5 C25 H25A 109.5 . .
O5 C25 H25B 109.5 . .
H25A C25 H25B 109.5 . .
O5 C25 H25C 109.5 . .
H25A C25 H25C 109.5 . .
H25B C25 H25C 109.5 . .
C15 N1 C17 103.7(5) . .
C15 N1 Cu1 123.5(4) . .
C17 N1 Cu1 131.2(4) . .
C15 N2 C16 107.7(5) . .
C15 N2 C18 124.0(5) . 3_557
C16 N2 C18 127.5(5) . 3_557
C20 N3 C7 111.5(4) . .
C20 N3 C14 111.6(4) . .
C7 N3 C14 107.5(4) . .
C20 N3 Cu1 100.1(3) . .
C7 N3 Cu1 114.0(3) . .
C14 N3 Cu1 112.2(3) . .
C1 O1 Cu1 127.5(3) . .
C8 O3 Cu1 126.5(4) . .
C25 O5 C23 117.3(8) . .
C23 O6 C24 115.4(7) . .
H7A O7 H7B 109.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.883(4) .
Cu1 O3 1.897(4) .
Cu1 N1 1.973(5) .
Cu1 N3 2.041(4) .
C1 O1 1.305(7) .
C1 C2 1.405(7) .
C1 C6 1.432(8) .
C2 C3 1.366(8) .
C2 C7 1.534(7) .
C3 C4 1.372(8) .
C3 H3 0.9300 .
C4 C5 1.357(8) .
C4 Cl1 1.732(7) .
C5 C6 1.366(8) .
C5 H5 0.9300 .
C6 Cl2 1.740(6) .
C7 N3 1.498(6) .
C7 C21 1.531(7) .
C7 H7 0.9800 .
C8 O3 1.326(7) .
C8 C9 1.393(8) .
C8 C13 1.419(8) .
C9 C10 1.398(8) .
C9 C14 1.500(7) .
C10 C11 1.371(8) .
C10 H10 0.9300 .
C11 C12 1.371(9) .
C11 Cl3 1.734(7) .
C12 C13 1.392(9) .
C12 H12 0.9300 .
C13 Cl4 1.698(7) .
C14 C22 1.523(7) .
C14 N3 1.524(6) .
C14 H14 0.9800 .
C15 N2 1.316(6) .
C15 N1 1.339(7) .
C15 H15 0.9300 .
C16 C17 1.320(8) .
C16 N2 1.357(7) .
C16 H16 0.9300 .
C17 N1 1.368(7) .
C17 H17 0.9300 .
C18 N2 1.472(7) 3_557
C18 C19 1.517(7) .
C18 H18A 0.9700 .
C18 H18B 0.9700 .
C19 C20 1.539(7) .
C19 H19A 0.9700 .
C19 H19B 0.9700 .
C20 N3 1.485(6) .
C20 H20A 0.9700 .
C20 H20B 0.9700 .
C21 C23 1.481(8) .
C21 H21A 0.9700 .
C21 H21B 0.9700 .
C22 C23 1.461(8) .
C22 H22A 0.9700 .
C22 H22B 0.9700 .
C23 O6 1.396(8) .
C23 O5 1.425(8) .
C24 O6 1.483(14) .
C24 H24A 0.9600 .
C24 H24B 0.9600 .
C24 H24C 0.9600 .
C25 O5 1.355(9) .
C25 H25A 0.9600 .
C25 H25B 0.9600 .
C25 H25C 0.9600 .
N2 C18 1.472(7) 3_557
O7 H7A 0.8500 .
O7 H7B 0.8500 .
