#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:44:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180094 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/40/7054025.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_7054025
loop_
_publ_author_name
'Świtlicka-Olszewska, Anna'
'Machura, Barbara'
'Mroziński, Jerzy'
'Kalińska, Bożena'
'Kruszynski, Rafał'
'Penkala, Mateusz'
_publ_section_title
;
 Effect of N-donor ancillary ligands on structural and magnetic properties
 of oxalate copper(ii) complexes
;
_journal_issue                   4
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1611
_journal_paper_doi               10.1039/c3nj01541f
_journal_volume                  38
_journal_year                    2014
_chemical_formula_moiety         '2(C18 H16 Cu2 N8 O8), 7(H2 O)'
_chemical_formula_sum            'C36 H46 Cu4 N16 O23'
_chemical_formula_weight         1325.05
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                87.214(4)
_cell_angle_beta                 85.536(5)
_cell_angle_gamma                75.414(5)
_cell_formula_units_Z            1
_cell_length_a                   9.1374(6)
_cell_length_b                   11.7993(7)
_cell_length_c                   12.2790(6)
_cell_measurement_reflns_used    5102
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      29.1275
_cell_measurement_theta_min      3.5629
_cell_volume                     1276.73(13)
_computing_cell_refinement       'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_collection       'CrysAlis CCD v. 1.163 (UNIL IC & KUMA 2000)'
_computing_data_reduction        'CrysAlis RED v. 1.163 (UNIL IC & KUMA 2000)'
_computing_molecular_graphics
;XP in SHELXTL/PC (Sheldrick, 1990b)
 ORTEP-3 W v. 1.062 (Farrugia 1997)
;
_computing_publication_material
;SHELXL-97 (Sheldrick, 1997) and
 PLATON (Spek, 1990)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295.0(2)
_diffrn_detector_area_resol_mean 12.8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Gemini A Ultra'
_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  0.0340
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            13783
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.57
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  22.00
_diffrn_standards_number         7
_exptl_absorpt_coefficient_mu    1.741
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.38231
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.723
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             674
_exptl_crystal_size_max          0.581
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.233
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.597
_refine_diff_density_rms         0.127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.171
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         4504
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.171
_refine_ls_R_factor_all          0.0547
_refine_ls_R_factor_gt           0.0397
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0708P)²+1.4194P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1212
_refine_ls_wR_factor_ref         0.1426
_reflns_number_gt                3829
_reflns_number_total             4504
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01541f2.cif
_cod_data_source_block           cu61
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054025
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -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
C1 C -0.1375(6) 0.2571(5) 0.6532(5) 0.0553(13) Uani 1 1 d .
C2 C -0.1698(7) 0.1885(5) 0.7392(5) 0.0686(17) Uani 1 1 d .
C3 C -0.0621(7) 0.0857(5) 0.7336(4) 0.0605(15) Uani 1 1 d .
C4 C 0.1631(6) 0.0125(4) 0.6012(4) 0.0485(12) Uani 1 1 d .
C5 C 0.4224(6) 0.0050(4) 0.6612(4) 0.0569(14) Uani 1 1 d .
C6 C 0.5195(7) 0.0750(5) 0.6415(5) 0.0642(15) Uani 1 1 d .
C7 C 0.4421(6) 0.1672(4) 0.5768(4) 0.0523(12) Uani 1 1 d .
C8 C 0.5005(5) 0.3518(4) -0.0635(4) 0.0427(10) Uani 1 1 d .
C9 C 0.5056(6) 0.4250(5) -0.1553(4) 0.0572(13) Uani 1 1 d .
C10 C 0.3921(6) 0.4129(4) -0.2158(4) 0.0485(12) Uani 1 1 d .
C11 C 0.1941(5) 0.2959(4) -0.1861(3) 0.0397(10) Uani 1 1 d .
C12 C -0.0643(6) 0.4128(4) -0.1172(5) 0.0529(14) Uani 1 1 d .
C13 C -0.1400(6) 0.4197(4) -0.0173(5) 0.0580(14) Uani 1 1 d .
C14 C -0.0457(5) 0.3464(4) 0.0517(4) 0.0479(11) Uani 1 1 d .
C15 C 0.2574(5) 0.2878(3) 0.2742(3) 0.0329(9) Uani 1 1 d .
C16 C 0.1833(5) 0.1824(3) 0.2671(3) 0.0333(9) Uani 1 1 d .
C17 C 0.5524(5) 0.0174(3) 0.0407(3) 0.0348(9) Uani 1 1 d .
C18 C -0.0536(5) 0.4916(3) 0.4564(3) 0.0318(9) Uani 1 1 d .
Cu1 Cu 0.12944(6) 0.26326(4) 0.48586(4) 0.03270(18) Uani 1 1 d .
Cu2 Cu 0.29325(6) 0.20945(4) 0.05030(4) 0.03154(18) Uani 1 1 d .
H1 H -0.1946 0.3324 0.6375 0.066 Uiso 1 1 calc R
H2 H -0.2502 0.2082 0.7918 0.082 Uiso 1 1 calc R
H3 H -0.0543 0.0210 0.7812 0.073 Uiso 1 1 calc R
H4A H 0.1736 -0.0619 0.6408 0.058 Uiso 1 1 calc R
H4B H 0.1506 0.0004 0.5253 0.058 Uiso 1 1 calc R
H5 H 0.4395 -0.0640 0.7036 0.068 Uiso 1 1 calc R
H6 H 0.6162 0.0637 0.6659 0.077 Uiso 1 1 calc R
H7 H 0.4798 0.2307 0.5517 0.063 Uiso 1 1 calc R
H8 H 0.5656 0.3422 -0.0073 0.051 Uiso 1 1 calc R
H9 H 0.5724 0.4722 -0.1718 0.069 Uiso 1 1 calc R
H10 H 0.3662 0.4507 -0.2824 0.058 Uiso 1 1 calc R
H11A H 0.1638 0.3253 -0.2583 0.048 Uiso 1 1 calc R
H11B H 0.2205 0.2110 -0.1865 0.048 Uiso 1 1 calc R
H12 H -0.0987 0.4534 -0.1808 0.063 Uiso 1 1 calc R
H13 H -0.2369 0.4653 0.0008 0.070 Uiso 1 1 calc R
H14 H -0.0690 0.3346 0.1258 0.057 Uiso 1 1 calc R
H97A H 0.1969 0.6766 0.6384 0.233 Uiso 1 1 d R
H97B H 0.2541 0.7231 0.7284 0.233 Uiso 1 1 d R
H98A H 0.3109 0.8473 0.8469 0.285 Uiso 1 1 d R
H98B H 0.1607 0.8983 0.8839 0.285 Uiso 1 1 d R
H99A H 0.5670 0.3874 0.4021 0.228 Uiso 1 1 d R
H99B H 0.4112 0.4071 0.4016 0.228 Uiso 1 1 d R
N1 N -0.0134(4) 0.2024(3) 0.5943(3) 0.0423(9) Uani 1 1 d .
N2 N 0.0306(4) 0.0961(3) 0.6459(3) 0.0412(9) Uani 1 1 d .
N3 N 0.3095(5) 0.1538(3) 0.5556(3) 0.0417(9) Uani 1 1 d .
N4 N 0.2977(4) 0.0530(3) 0.6086(3) 0.0395(8) Uani 1 1 d .
N5 N 0.3913(4) 0.2982(3) -0.0667(3) 0.0340(8) Uani 1 1 d .
N6 N 0.3245(4) 0.3360(3) -0.1613(3) 0.0358(8) Uani 1 1 d .
N7 N 0.0826(4) 0.2948(3) -0.0018(3) 0.0376(8) Uani 1 1 d .
N8 N 0.0698(4) 0.3362(3) -0.1063(3) 0.0377(8) Uani 1 1 d .
O1 O 0.2609(4) 0.3223(3) 0.3696(2) 0.0457(8) Uani 1 1 d .
O2 O 0.1205(4) 0.1491(3) 0.3512(2) 0.0435(7) Uani 1 1 d .
O3 O 0.3060(4) 0.3285(3) 0.1888(2) 0.0411(7) Uani 1 1 d .
O4 O 0.1922(4) 0.1392(2) 0.1745(2) 0.0437(8) Uani 1 1 d .
O5 O -0.1406(4) 0.5795(3) 0.4183(2) 0.0437(8) Uani 1 1 d .
O6 O -0.0471(4) 0.3878(3) 0.4333(3) 0.0492(8) Uani 1 1 d .
O7 O 0.5015(4) 0.1137(2) 0.0869(2) 0.0448(8) Uani 1 1 d .
O8 O 0.6764(4) -0.0513(3) 0.0545(3) 0.0508(9) Uani 1 1 d .
O96 O 0.0000 0.0000 0.0000 0.173(5) Uani 1 2 d S
O97 O 0.2636(8) 0.7143(6) 0.6598(7) 0.155(3) Uani 1 1 d .
O98 O 0.2205(11) 0.8408(8) 0.8449(7) 0.190(4) Uani 1 1 d .
O99 O 0.4823(8) 0.4368(7) 0.4174(5) 0.152(3) 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'
Cu Cu 0.3201 1.2651 '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'
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 O6 87.68(15) . .
O1 Cu1 N1 175.70(13) . .
O6 Cu1 N1 89.78(15) . .
O1 Cu1 N3 93.27(15) . .
O6 Cu1 N3 171.77(13) . .
N1 Cu1 N3 89.74(16) . .
O1 Cu1 O2 79.63(12) . .
O6 Cu1 O2 91.66(12) . .
N1 Cu1 O2 96.98(14) . .
N3 Cu1 O2 96.56(13) . .
O1 Cu1 O5 85.94(12) . 2_566
O6 Cu1 O5 77.89(11) . 2_566
N1 Cu1 O5 96.92(14) . 2_566
N3 Cu1 O5 94.01(12) . 2_566
O2 Cu1 O5 162.54(11) . 2_566
O4 Cu2 N5 173.45(12) . .
O4 Cu2 O7 92.54(14) . .
N5 Cu2 O7 89.41(13) . .
O4 Cu2 N7 89.27(14) . .
N5 Cu2 N7 89.49(14) . .
O7 Cu2 N7 173.48(12) . .
O4 Cu2 O8 93.26(13) . 2_655
N5 Cu2 O8 93.26(13) . 2_655
O7 Cu2 O8 78.25(11) . 2_655
N7 Cu2 O8 95.41(13) . 2_655
O4 Cu2 O3 78.55(11) . .
N5 Cu2 O3 95.31(12) . .
O7 Cu2 O3 87.13(11) . .
N7 Cu2 O3 99.37(13) . .
O8 Cu2 O3 162.96(11) 2_655 .
C1 N1 N2 104.1(4) . .
C1 N1 Cu1 131.8(3) . .
N2 N1 Cu1 121.4(3) . .
C3 N2 N1 111.7(4) . .
C3 N2 C4 129.7(4) . .
N1 N2 C4 118.6(4) . .
C7 N3 N4 105.3(4) . .
C7 N3 Cu1 132.1(3) . .
N4 N3 Cu1 121.6(3) . .
C5 N4 N3 110.8(4) . .
C5 N4 C4 129.9(4) . .
N3 N4 C4 119.3(4) . .
C8 N5 N6 105.8(4) . .
C8 N5 Cu2 131.3(3) . .
N6 N5 Cu2 121.3(3) . .
C10 N6 N5 110.6(4) . .
C10 N6 C11 130.2(4) . .
N5 N6 C11 119.0(3) . .
C14 N7 N8 105.7(4) . .
C14 N7 Cu2 132.2(3) . .
N8 N7 Cu2 119.8(3) . .
C12 N8 N7 110.8(4) . .
C12 N8 C11 130.1(4) . .
N7 N8 C11 119.1(3) . .
N1 C1 C2 111.2(5) . .
N1 C1 H1 124.4 . .
C2 C1 H1 124.4 . .
C3 C2 C1 106.7(5) . .
C3 C2 H2 126.6 . .
C1 C2 H2 126.6 . .
N2 C3 C2 106.3(5) . .
N2 C3 H3 126.9 . .
C2 C3 H3 126.9 . .
N4 C4 N2 111.1(4) . .
N4 C4 H4A 109.4 . .
N2 C4 H4A 109.4 . .
N4 C4 H4B 109.4 . .
N2 C4 H4B 109.4 . .
H4A C4 H4B 108.0 . .
N4 C5 C6 107.7(5) . .
N4 C5 H5 126.1 . .
C6 C5 H5 126.1 . .
C5 C6 C7 104.5(5) . .
C5 C6 H6 127.7 . .
C7 C6 H6 127.7 . .
N3 C7 C6 111.6(5) . .
N3 C7 H7 124.2 . .
C6 C7 H7 124.2 . .
N5 C8 C9 110.9(4) . .
N5 C8 H8 124.6 . .
C9 C8 H8 124.6 . .
C10 C9 C8 105.4(5) . .
C10 C9 H9 127.3 . .
C8 C9 H9 127.3 . .
N6 C10 C9 107.2(4) . .
N6 C10 H10 126.4 . .
C9 C10 H10 126.4 . .
N8 C11 N6 110.5(3) . .
N8 C11 H11A 109.6 . .
N6 C11 H11A 109.6 . .
N8 C11 H11B 109.6 . .
N6 C11 H11B 109.6 . .
H11A C11 H11B 108.1 . .
N8 C12 C13 106.6(4) . .
N8 C12 H12 126.7 . .
C13 C12 H12 126.7 . .
C12 C13 C14 106.6(4) . .
C12 C13 H13 126.7 . .
C14 C13 H13 126.7 . .
N7 C14 C13 110.4(5) . .
N7 C14 H14 124.8 . .
C13 C14 H14 124.8 . .
O3 C15 O1 126.5(4) . .
O3 C15 C16 118.3(3) . .
O1 C15 C16 115.2(4) . .
O2 C16 O4 125.4(4) . .
O2 C16 C15 118.4(3) . .
O4 C16 C15 116.2(4) . .
O8 C17 O7 125.5(4) . .
O8 C17 C17 117.9(4) . 2_655
O7 C17 C17 116.6(4) . 2_655
O5 C18 O6 125.3(4) . .
O5 C18 C18 118.3(4) . 2_566
O6 C18 C18 116.4(4) . 2_566
C16 O4 Cu2 118.4(3) . .
C15 O3 Cu2 108.0(2) . .
C16 O2 Cu1 109.2(3) . .
C15 O1 Cu1 115.8(3) . .
C17 O7 Cu2 117.5(3) . .
C18 O6 Cu1 116.8(3) . .
C17 O8 Cu2 109.8(3) . 2_655
C18 O5 Cu1 108.5(2) . 2_566
H97A O97 H97B 111.4 . .
H98A O98 H98B 107.2 . .
H99A O99 H99B 108.3 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 2.006(3) .
Cu1 O6 2.014(3) .
Cu1 N1 2.025(4) .
Cu1 N3 2.037(4) .
Cu1 O2 2.202(3) .
Cu1 O5 2.273(3) 2_566
Cu2 O4 1.977(3) .
Cu2 N5 2.023(4) .
Cu2 O7 2.025(3) .
Cu2 N7 2.069(4) .
Cu2 O8 2.265(3) 2_655
Cu2 O3 2.285(3) .
N1 C1 1.332(6) .
N1 N2 1.359(5) .
N2 C3 1.338(7) .
N2 C4 1.444(6) .
N3 C7 1.308(7) .
N3 N4 1.352(5) .
N4 C5 1.338(6) .
N4 C4 1.438(6) .
N5 C8 1.313(6) .
N5 N6 1.357(4) .
N6 C10 1.347(6) .
N6 C11 1.446(6) .
N7 C14 1.318(6) .
N7 N8 1.353(5) .
N8 C12 1.338(6) .
N8 C11 1.442(6) .
C1 C2 1.359(8) .
C1 H1 0.9300 .
C2 C3 1.356(8) .
C2 H2 0.9300 .
C3 H3 0.9300 .
C4 H4A 0.9700 .
C4 H4B 0.9700 .
C5 C6 1.358(9) .
C5 H5 0.9300 .
C6 C7 1.390(7) .
C6 H6 0.9300 .
C7 H7 0.9300 .
C8 C9 1.391(7) .
C8 H8 0.9300 .
C9 C10 1.361(7) .
C9 H9 0.9300 .
C10 H10 0.9300 .
C11 H11A 0.9700 .
C11 H11B 0.9700 .
C12 C13 1.355(8) .
C12 H12 0.9300 .
C13 C14 1.369(7) .
C13 H13 0.9300 .
C14 H14 0.9300 .
C15 O3 1.230(5) .
C15 O1 1.264(5) .
C15 C16 1.567(6) .
C16 O2 1.238(5) .
C16 O4 1.258(5) .
C17 O8 1.234(5) .
C17 O7 1.259(5) .
C17 C17 1.572(8) 2_655
C18 O5 1.234(5) .
C18 O6 1.256(5) .
C18 C18 1.558(8) 2_566
O8 Cu2 2.265(3) 2_655
O5 Cu1 2.273(3) 2_566
O97 H97A 0.9006 .
O97 H97B 0.8487 .
O98 H98A 0.8512 .
O98 H98B 0.8902 .
O99 H99A 0.8575 .
O99 H99B 0.8500 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O97 H97A O6 0.90 2.00 2.891(7) 169.6 2_566
O97 H97B O98 0.85 1.99 2.728(12) 144.1 .
O98 H98B O96 0.89 2.14 3.010(11) 165.3 1_566
O99 H99B O1 0.85 1.96 2.811(6) 173.9 .
C3 H3 O4 0.93 2.54 3.289(6) 137.9 2_556
C4 H4A O97 0.97 2.56 3.460(8) 153.5 1_545
