#------------------------------------------------------------------------------
#$Date: 2019-11-28 13:50:34 +0200 (Thu, 28 Nov 2019) $
#$Revision: 243896 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/70/25/7702534.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_7702534
loop_
_publ_author_name
'Gao, En-Qing'
'Zhao, Qi-Hua'
'Tang, Jin-Kui'
'Liao, Dai-Zheng'
'Jiang, Zong-Hui'
'Yan, Shi-Ping'
_publ_section_title
;
 A new one-dimensional coordination polymer and a new supramolecular dimer
 made of trinuclear copper(II) complexes: crystal structure and magnetic
 properties
;
_journal_issue                   9
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              1537
_journal_paper_doi               10.1039/b100142f
_journal_year                    2001
_chemical_formula_sum            'C19 H40 Cl2 Cu3 N6 O17'
_chemical_formula_weight         886.09
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P c a 21'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.2818(11)
_cell_length_b                   12.8206(7)
_cell_length_c                   12.6462(7)
_cell_measurement_reflns_used    6911
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      2.45
_cell_volume                     3450.5(3)
_computing_cell_refinement       SAINT
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       ω
_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  0.0368
_diffrn_reflns_av_sigmaI/netI    0.0369
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13935
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        4.04
_exptl_absorpt_coefficient_mu    2.065
_exptl_absorpt_correction_T_max  0.6829
_exptl_absorpt_correction_T_min  0.6263
_exptl_absorpt_correction_type   sadabs
_exptl_crystal_colour            'greenish blue'
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1812
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.990
_refine_diff_density_min         -0.332
_refine_diff_density_rms         0.077
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.005(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     424
_refine_ls_number_reflns         5353
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0668P)²+0.1306P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0989
_refine_ls_wR_factor_ref         0.1069
_reflns_number_gt                4552
_reflns_number_total             5353
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b100142f.txt
_cod_data_source_block           1
_cod_original_sg_symbol_H-M      Pca2(1)
_cod_database_code               7702534
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, 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 0.54050(3) 0.25570(5) 0.90119(6) 0.04400(18) Uani 1 1 d .
Cu2 Cu 0.65671(3) 0.16077(5) 0.55441(5) 0.04219(17) Uani 1 1 d .
Cu3 Cu 0.40722(3) 0.32158(5) 1.23557(6) 0.04070(17) Uani 1 1 d .
O1 O 0.6007(2) 0.1492(3) 0.8521(3) 0.0506(11) Uani 1 1 d .
O2 O 0.5329(2) 0.1973(3) 1.0464(4) 0.0586(12) Uani 1 1 d .
N1 N 0.54560(19) 0.3089(3) 0.7587(3) 0.0335(10) Uani 1 1 d .
N2 N 0.4810(2) 0.3595(4) 0.9488(4) 0.0391(10) Uani 1 1 d .
O3 O 0.65296(18) 0.1129(3) 0.7046(3) 0.0472(10) Uani 1 1 d .
O4 O 0.59411(19) 0.2633(3) 0.6006(3) 0.0470(10) Uani 1 1 d .
N3 N 0.6727(2) 0.2363(4) 0.4162(4) 0.0473(12) Uani 1 1 d .
N4 N 0.7346(2) 0.0751(4) 0.5233(4) 0.0434(11) Uani 1 1 d .
O5 O 0.4817(2) 0.2377(4) 1.1950(3) 0.0604(12) Uani 1 1 d .
O6 O 0.42041(18) 0.3903(3) 1.0985(3) 0.0447(9) Uani 1 1 d .
O7 O 0.5491(2) 0.5284(3) 0.8309(4) 0.0581(11) Uani 1 1 d .
H7A H 0.5668 0.5574 0.7813 0.087 Uiso 1 1 calc R
N5 N 0.3175(2) 0.3686(4) 1.2421(5) 0.0572(13) Uani 1 1 d .
N6 N 0.3905(3) 0.2331(4) 1.3636(4) 0.0520(13) Uani 1 1 d .
O8 O 0.5800(3) 0.0455(5) 0.5061(5) 0.0849(17) Uani 1 1 d .
C1 C 0.6146(3) 0.1628(4) 0.7571(5) 0.0411(14) Uani 1 1 d .
C2 C 0.5820(2) 0.2530(4) 0.6987(4) 0.0341(12) Uani 1 1 d .
C3 C 0.5094(3) 0.3964(4) 0.7141(4) 0.0395(12) Uani 1 1 d .
H3A H 0.4705 0.3697 0.6847 0.047 Uiso 1 1 calc R
H3B H 0.5332 0.4276 0.6569 0.047 Uiso 1 1 calc R
C4 C 0.4943(3) 0.4789(4) 0.7945(5) 0.0453(14) Uani 1 1 d .
H4A H 0.4702 0.5325 0.7569 0.054 Uiso 1 1 calc R
C5 C 0.4535(3) 0.4447(4) 0.8876(5) 0.0468(14) Uani 1 1 d .
H5A H 0.4468 0.5040 0.9340 0.056 Uiso 1 1 calc R
H5B H 0.4128 0.4229 0.8611 0.056 Uiso 1 1 calc R
C6 C 0.4620(2) 0.3414(4) 1.0437(5) 0.0359(12) Uani 1 1 d .
C7 C 0.4955(3) 0.2507(5) 1.1004(5) 0.0490(15) Uani 1 1 d .
C8 C 0.7358(3) 0.2014(5) 0.3804(5) 0.0508(15) Uani 1 1 d .
H8A H 0.7680 0.2434 0.4142 0.061 Uiso 1 1 calc R
H8B H 0.7394 0.2105 0.3045 0.061 Uiso 1 1 calc R
C9 C 0.7452(3) 0.0884(5) 0.4084(5) 0.0516(14) Uani 1 1 d .
H9A H 0.7158 0.0454 0.3690 0.062 Uiso 1 1 calc R
H9B H 0.7875 0.0669 0.3901 0.062 Uiso 1 1 calc R
C10 C 0.6727(5) 0.3517(6) 0.4296(8) 0.087(3) Uani 1 1 d .
H10A H 0.6806 0.3844 0.3626 0.130 Uiso 1 1 calc R
H10B H 0.7050 0.3712 0.4788 0.130 Uiso 1 1 calc R
H10C H 0.6326 0.3739 0.4561 0.130 Uiso 1 1 calc R
C11 C 0.6247(4) 0.2045(8) 0.3354(7) 0.086(3) Uani 1 1 d .
H11A H 0.6327 0.2405 0.2703 0.128 Uiso 1 1 calc R
H11B H 0.5835 0.2219 0.3606 0.128 Uiso 1 1 calc R
H11C H 0.6273 0.1306 0.3239 0.128 Uiso 1 1 calc R
C12 C 0.7874(3) 0.1133(7) 0.5877(6) 0.074(2) Uani 1 1 d .
H12A H 0.8242 0.0725 0.5729 0.111 Uiso 1 1 calc R
H12B H 0.7770 0.1073 0.6613 0.111 Uiso 1 1 calc R
H12C H 0.7955 0.1851 0.5709 0.111 Uiso 1 1 calc R
C13 C 0.7254(3) -0.0374(4) 0.5482(7) 0.0660(19) Uani 1 1 d .
H13A H 0.7632 -0.0751 0.5324 0.099 Uiso 1 1 calc R
H13B H 0.6915 -0.0645 0.5063 0.099 Uiso 1 1 calc R
H13C H 0.7156 -0.0451 0.6218 0.099 Uiso 1 1 calc R
C14 C 0.3239(5) 0.2543(10) 1.3908(12) 0.146(6) Uani 1 1 d .
H14A H 0.2996 0.1930 1.3719 0.175 Uiso 1 1 calc R
H14B H 0.3212 0.2617 1.4670 0.175 Uiso 1 1 calc R
C15 C 0.2959(5) 0.3370(12) 1.3475(9) 0.129(5) Uani 1 1 d .
H15A H 0.3014 0.3957 1.3949 0.155 Uiso 1 1 calc R
H15B H 0.2512 0.3227 1.3433 0.155 Uiso 1 1 calc R
C16 C 0.4340(6) 0.2572(7) 1.4497(7) 0.097(3) Uani 1 1 d .
H16A H 0.4248 0.2136 1.5094 0.146 Uiso 1 1 calc R
H16B H 0.4296 0.3291 1.4694 0.146 Uiso 1 1 calc R
H16C H 0.4764 0.2446 1.4266 0.146 Uiso 1 1 calc R
C17 C 0.3966(5) 0.1194(5) 1.3427(8) 0.090(3) Uani 1 1 d .
H17A H 0.3885 0.0813 1.4066 0.134 Uiso 1 1 calc R
H17B H 0.4384 0.1045 1.3186 0.134 Uiso 1 1 calc R
H17C H 0.3669 0.0991 1.2895 0.134 Uiso 1 1 calc R
C18 C 0.3098(3) 0.4863(6) 1.2332(8) 0.078(2) Uani 1 1 d .
H18A H 0.2660 0.5039 1.2368 0.117 Uiso 1 1 calc R
H18B H 0.3268 0.5097 1.1670 0.117 Uiso 1 1 calc R
H18C H 0.3318 0.5196 1.2903 0.117 Uiso 1 1 calc R
C19 C 0.2818(4) 0.3230(7) 1.1567(9) 0.092(3) Uani 1 1 d .
H19A H 0.2390 0.3463 1.1607 0.138 Uiso 1 1 calc R
H19B H 0.2831 0.2484 1.1623 0.138 Uiso 1 1 calc R
H19C H 0.2996 0.3440 1.0903 0.138 Uiso 1 1 calc R
Cl1 Cl 0.64740(8) 0.42392(13) 1.06474(16) 0.0629(4) Uani 1 1 d .
O9 O 0.6363(3) 0.3772(5) 0.9634(4) 0.0826(16) Uani 1 1 d .
O10 O 0.5985(5) 0.4047(17) 1.1293(11) 0.289(11) Uani 1 1 d .
O11 O 0.6697(10) 0.5159(8) 1.0620(12) 0.315(11) Uani 1 1 d .
O12 O 0.6940(6) 0.3647(8) 1.1159(8) 0.164(4) Uani 1 1 d .
Cl2 Cl 0.87332(10) 0.83496(14) 0.79894(18) 0.0735(5) Uani 1 1 d .
O16 O 0.8522(4) 0.7808(9) 0.8916(11) 0.171(4) Uani 1 1 d .
O15 O 0.8271(5) 0.9024(7) 0.7732(7) 0.163(4) Uani 1 1 d .
O14 O 0.9290(4) 0.8829(7) 0.8259(8) 0.151(4) Uani 1 1 d .
O13 O 0.8863(4) 0.7585(7) 0.7256(8) 0.154(4) Uani 1 1 d .
O17 O 0.9777(4) 0.9850(6) 0.6239(10) 0.186(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'
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'
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_3
N1 Cu1 N2 94.84(18) .
N1 Cu1 O1 85.07(17) .
N2 Cu1 O1 179.6(2) .
N1 Cu1 O2 178.0(2) .
N2 Cu1 O2 85.32(17) .
O1 Cu1 O2 94.75(16) .
N1 Cu1 O9 91.49(18) .
N2 Cu1 O9 90.4(2) .
O1 Cu1 O9 90.0(2) .
O2 Cu1 O9 90.5(2) .
O4 Cu2 O3 83.99(16) .
O4 Cu2 N3 92.90(18) .
O3 Cu2 N3 166.8(2) .
O4 Cu2 N4 167.61(19) .
O3 Cu2 N4 92.91(17) .
N3 Cu2 N4 87.39(18) .
O4 Cu2 O8 91.59(19) .
O3 Cu2 O8 91.5(2) .
N3 Cu2 O8 101.4(2) .
N4 Cu2 O8 100.5(2) .
O6 Cu3 O5 84.30(16) .
O6 Cu3 N5 92.1(2) .
O5 Cu3 N5 159.3(2) .
O6 Cu3 N6 171.8(2) .
O5 Cu3 N6 92.54(19) .
N5 Cu3 N6 88.1(2) .
O6 Cu3 O7 91.60(17) 2_665
O5 Cu3 O7 104.47(19) 2_665
N5 Cu3 O7 96.0(2) 2_665
N6 Cu3 O7 96.52(19) 2_665
C1 O1 Cu1 111.1(4) .
C7 O2 Cu1 110.5(4) .
C2 N1 C3 120.5(4) .
C2 N1 Cu1 112.6(3) .
C3 N1 Cu1 126.6(3) .
C6 N2 C5 120.1(4) .
C6 N2 Cu1 111.9(4) .
C5 N2 Cu1 127.8(4) .
C1 O3 Cu2 112.3(4) .
C2 O4 Cu2 111.0(3) .
C8 N3 C10 109.4(5) .
C8 N3 C11 109.0(5) .
C10 N3 C11 110.4(7) .
C8 N3 Cu2 105.7(4) .
C10 N3 Cu2 112.1(4) .
C11 N3 Cu2 110.1(4) .
C12 N4 C9 112.9(5) .
C12 N4 C13 107.8(6) .
C9 N4 C13 109.8(5) .
C12 N4 Cu2 109.7(4) .
C9 N4 Cu2 104.6(4) .
C13 N4 Cu2 112.1(4) .
C7 O5 Cu3 111.4(4) .
C6 O6 Cu3 110.8(3) .
C19 N5 C15 113.7(8) .
C19 N5 C18 106.9(7) .
C15 N5 C18 107.9(8) .
C19 N5 Cu3 110.4(5) .
C15 N5 Cu3 104.6(5) .
C18 N5 Cu3 113.4(4) .
C16 N6 C14 113.3(9) .
C16 N6 C17 106.5(7) .
C14 N6 C17 107.7(8) .
C16 N6 Cu3 111.6(4) .
C14 N6 Cu3 104.7(5) .
C17 N6 Cu3 113.2(5) .
O3 C1 O1 127.0(5) .
O3 C1 C2 115.6(5) .
O1 C1 C2 117.4(5) .
O4 C2 N1 129.3(5) .
O4 C2 C1 117.0(4) .
N1 C2 C1 113.7(5) .
N1 C3 C4 112.9(5) .
O7 C4 C3 111.3(5) .
O7 C4 C5 110.4(5) .
C3 C4 C5 116.1(4) .
N2 C5 C4 113.2(4) .
O6 C6 N2 129.1(5) .
O6 C6 C7 115.8(5) .
N2 C6 C7 115.1(4) .
O5 C7 O2 127.0(6) .
O5 C7 C6 116.1(5) .
O2 C7 C6 116.9(5) .
N3 C8 C9 109.8(5) .
N4 C9 C8 108.7(5) .
C15 C14 N6 118.4(8) .
C14 C15 N5 117.0(9) .
O11 Cl1 O10 118.4(13) .
O11 Cl1 O12 104.5(9) .
O10 Cl1 O12 99.6(10) .
O11 Cl1 O9 115.1(7) .
O10 Cl1 O9 109.8(6) .
O12 Cl1 O9 107.5(5) .
Cl1 O9 Cu1 129.0(3) .
O15 Cl2 O13 116.1(6) .
O15 Cl2 O14 113.6(6) .
O13 Cl2 O14 108.1(6) .
O15 Cl2 O16 106.2(6) .
O13 Cl2 O16 105.6(7) .
O14 Cl2 O16 106.5(7) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N1 1.930(4) .
Cu1 N2 1.933(4) .
Cu1 O1 1.973(4) .
Cu1 O2 1.989(5) .
Cu1 O9 2.684(6) .
Cu2 O4 1.961(4) .
Cu2 O3 1.998(4) .
Cu2 N3 2.027(5) .
Cu2 N4 2.028(4) .
Cu2 O8 2.285(5) .
Cu3 O6 1.964(4) .
Cu3 O5 1.984(4) .
Cu3 N5 2.004(5) .
Cu3 N6 2.009(5) .
Cu3 O7 2.453(4) 2_665
O1 C1 1.250(7) .
O2 C7 1.253(7) .
N1 C2 1.299(7) .
N1 C3 1.473(6) .
N2 C6 1.288(7) .
N2 C5 1.462(7) .
O3 C1 1.231(7) .
O4 C2 1.273(6) .
N3 C8 1.486(7) .
N3 C10 1.489(9) .
N3 C11 1.500(9) .
N4 C12 1.471(8) .
N4 C9 1.481(8) .
N4 C13 1.490(8) .
O5 C7 1.242(7) .
O6 C6 1.287(6) .
O7 C4 1.406(8) .
N5 C19 1.444(10) .
N5 C15 1.467(11) .
N5 C18 1.522(9) .
N6 C16 1.462(11) .
N6 C14 1.484(10) .
N6 C17 1.487(9) .
C1 C2 1.538(7) .
C3 C4 1.502(7) .
C4 C5 1.528(8) .
C6 C7 1.541(7) .
C8 C9 1.505(8) .
C14 C15 1.334(14) .
Cl1 O11 1.272(10) .
Cl1 O10 1.345(12) .
Cl1 O12 1.406(9) .
Cl1 O9 1.434(6) .
Cl2 O15 1.349(7) .
Cl2 O13 1.377(7) .
Cl2 O14 1.378(8) .
Cl2 O16 1.434(11) .
