#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:44:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180094 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/40/7054027.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_7054027
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         'C20 H24 Cu3 N4 O14, 2(H2 O)'
_chemical_formula_sum            'C20 H28 Cu3 N4 O16'
_chemical_formula_weight         771.08
_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                98.405(6)
_cell_angle_beta                 90.733(5)
_cell_angle_gamma                101.710(6)
_cell_formula_units_Z            1
_cell_length_a                   7.6832(5)
_cell_length_b                   8.8480(6)
_cell_length_c                   10.4914(7)
_cell_measurement_reflns_used    2795
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      29.1877
_cell_measurement_theta_min      3.4100
_cell_volume                     690.21(8)
_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 0.997
_diffrn_measured_fraction_theta_max 0.997
_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  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5160
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         3.42
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  22.00
_diffrn_standards_number         7
_exptl_absorpt_coefficient_mu    2.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.70095
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.855
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             391
_exptl_crystal_size_max          0.189
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.004
_refine_diff_density_max         0.320
_refine_diff_density_min         -0.353
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     196
_refine_ls_number_reflns         2441
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0315
_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)+(0.0349P)²+0.0143P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0722
_refine_ls_wR_factor_ref         0.0761
_reflns_number_gt                2139
_reflns_number_total             2441
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01541f2.cif
_cod_data_source_block           cu59
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7054027
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 0.5256(3) 0.7922(3) 0.2528(3) 0.0334(7) Uani 1 1 d .
C2 C 0.6181(4) 0.9402(3) 0.2508(3) 0.0434(8) Uani 1 1 d .
C3 C 0.5472(4) 1.0631(4) 0.3065(3) 0.0474(9) Uani 1 1 d .
C4 C 0.3878(4) 1.0332(3) 0.3629(3) 0.0419(8) Uani 1 1 d .
C5 C 0.3020(4) 0.8811(3) 0.3654(3) 0.0331(7) Uani 1 1 d .
C6 C 0.1265(4) 0.8429(3) 0.4277(4) 0.0499(9) Uani 1 1 d .
C7 C -0.0168(4) 0.7409(3) 0.3367(4) 0.0485(9) Uani 1 1 d .
C8 C 0.1661(4) 0.2983(3) 0.0808(3) 0.0319(7) Uani 1 1 d .
C9 C 0.1070(3) 0.2256(3) 0.2036(3) 0.0285(6) Uani 1 1 d .
C10 C 0.4445(3) 0.5227(3) 0.5586(3) 0.0205(6) Uani 1 1 d .
Cu1 Cu 0.25290(4) 0.53646(3) 0.31599(3) 0.02316(13) Uani 1 1 d .
Cu2 Cu 0.0000 0.0000 0.0000 0.0516(2) Uani 1 2 d S
H1 H 0.5723 0.7093 0.2127 0.040 Uiso 1 1 calc R
H2 H 0.7273 0.9578 0.2123 0.052 Uiso 1 1 calc R
H2A H -0.0422 0.5362 0.2339 0.043 Uiso 1 1 calc R
H2B H -0.0532 0.5270 0.3701 0.043 Uiso 1 1 calc R
H3 H 0.6072 1.1654 0.3057 0.057 Uiso 1 1 calc R
H4 H 0.3370 1.1152 0.3998 0.050 Uiso 1 1 calc R
H6A H 0.1417 0.7904 0.5008 0.060 Uiso 1 1 calc R
H6B H 0.0893 0.9393 0.4600 0.060 Uiso 1 1 calc R
H7A H -0.1318 0.7424 0.3733 0.058 Uiso 1 1 calc R
H7B H -0.0158 0.7820 0.2559 0.058 Uiso 1 1 calc R
H7OA H -0.3488 0.0767 -0.0965 0.108 Uiso 1 1 d R
H7OB H -0.2837 0.1867 0.0308 0.108 Uiso 1 1 d R
H8OA H -0.2751 0.4462 0.0496 0.078 Uiso 1 1 d R
H8OB H -0.3788 0.4071 0.1705 0.078 Uiso 1 1 d R
N1 N 0.3701(3) 0.7605(2) 0.3101(2) 0.0253(5) Uani 1 1 d .
N2 N 0.0087(3) 0.5791(3) 0.3120(3) 0.0359(6) Uani 1 1 d .
O1 O 0.1346(2) 0.3079(2) 0.31010(19) 0.0308(5) Uani 1 1 d .
O2 O 0.2436(3) 0.4367(2) 0.09514(19) 0.0380(5) Uani 1 1 d .
O3 O 0.0325(3) 0.0826(2) 0.18301(19) 0.0370(5) Uani 1 1 d .
O4 O 0.1281(3) 0.2079(2) -0.0242(2) 0.0471(6) Uani 1 1 d .
O5 O 0.2994(2) 0.5559(2) 0.53527(18) 0.0280(4) Uani 1 1 d .
O6 O 0.5090(2) 0.5221(2) 0.66912(18) 0.0259(4) Uani 1 1 d .
O7 O -0.2899(4) 0.0925(3) -0.0112(3) 0.0720(8) Uani 1 1 d .
O8 O -0.2845(3) 0.3947(2) 0.1131(2) 0.0523(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'
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
N2 Cu1 O6 174.48(8) . 2_666
N2 Cu1 N1 93.43(9) . .
O6 Cu1 N1 91.15(7) 2_666 .
N2 Cu1 O1 86.68(9) . .
O6 Cu1 O1 88.93(7) 2_666 .
N1 Cu1 O1 176.55(8) . .
N2 Cu1 O5 99.22(9) . .
O6 Cu1 O5 77.34(7) 2_666 .
N1 Cu1 O5 94.27(8) . .
O1 Cu1 O5 89.12(7) . .
N2 Cu1 O2 94.50(9) . .
O6 Cu1 O2 87.77(8) 2_666 .
N1 Cu1 O2 99.63(8) . .
O1 Cu1 O2 76.93(7) . .
O5 Cu1 O2 159.83(7) . .
O3 Cu2 O3 180.00(12) 2 .
O3 Cu2 O4 95.30(8) 2 .
O3 Cu2 O4 84.70(8) . .
O3 Cu2 O4 84.70(8) 2 2
O3 Cu2 O4 95.30(8) . 2
O4 Cu2 O4 180.00(6) . 2
C1 N1 C5 118.1(2) . .
C1 N1 Cu1 119.28(18) . .
C5 N1 Cu1 122.62(17) . .
C7 N2 Cu1 119.90(17) . .
C7 N2 H2A 107.3 . .
Cu1 N2 H2A 107.3 . .
C7 N2 H2B 107.3 . .
Cu1 N2 H2B 107.3 . .
H2A N2 H2B 106.9 . .
N1 C1 C2 123.0(3) . .
N1 C1 H1 118.5 . .
C2 C1 H1 118.5 . .
C1 C2 C3 118.7(3) . .
C1 C2 H2 120.6 . .
C3 C2 H2 120.6 . .
C4 C3 C2 119.1(3) . .
C4 C3 H3 120.5 . .
C2 C3 H3 120.5 . .
C3 C4 C5 119.8(3) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
N1 C5 C4 121.3(3) . .
N1 C5 C6 117.2(2) . .
C4 C5 C6 121.5(3) . .
C7 C6 C5 112.8(3) . .
C7 C6 H6A 109.0 . .
C5 C6 H6A 109.0 . .
C7 C6 H6B 109.0 . .
C5 C6 H6B 109.0 . .
H6A C6 H6B 107.8 . .
N2 C7 C6 111.4(2) . .
N2 C7 H7A 109.4 . .
C6 C7 H7A 109.4 . .
N2 C7 H7B 109.4 . .
C6 C7 H7B 109.4 . .
H7A C7 H7B 108.0 . .
O2 C8 O4 126.6(3) . .
O2 C8 C9 118.0(3) . .
O4 C8 C9 115.4(2) . .
O1 C9 O3 125.6(2) . .
O1 C9 C8 119.4(2) . .
O3 C9 C8 115.0(3) . .
O5 C10 O6 125.4(2) . .
O5 C10 C10 117.3(3) . 2_666
O6 C10 C10 117.3(3) . 2_666
C9 O1 Cu1 117.65(17) . .
C8 O2 Cu1 107.96(17) . .
C9 O3 Cu2 112.47(17) . .
C8 O4 Cu2 112.27(17) . .
C10 O5 Cu1 109.53(16) . .
C10 O6 Cu1 118.49(16) . 2_666
H7OA O7 H7OB 112.9 . .
H8OA O8 H8OB 117.0 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 1.988(2) .
Cu1 O6 2.0104(17) 2_666
Cu1 N1 2.014(2) .
Cu1 O1 2.0336(17) .
Cu1 O5 2.2996(19) .
Cu1 O2 2.351(2) .
Cu2 O3 1.946(2) 2
Cu2 O3 1.946(2) .
Cu2 O4 1.9556(18) .
Cu2 O4 1.9556(18) 2
N1 C1 1.341(3) .
N1 C5 1.342(4) .
N2 C7 1.471(4) .
N2 H2A 0.9000 .
N2 H2B 0.9000 .
C1 C2 1.360(4) .
C1 H1 0.9300 .
C2 C3 1.373(5) .
C2 H2 0.9300 .
C3 C4 1.361(4) .
C3 H3 0.9300 .
C4 C5 1.377(4) .
C4 H4 0.9300 .
C5 C6 1.504(4) .
C6 C7 1.502(4) .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 H7A 0.9700 .
C7 H7B 0.9700 .
C8 O2 1.234(3) .
C8 O4 1.257(3) .
C8 C9 1.554(4) .
C9 O1 1.232(3) .
C9 O3 1.264(3) .
C10 O5 1.239(3) .
C10 O6 1.256(3) .
C10 C10 1.557(5) 2_666
O6 Cu1 2.0104(17) 2_666
O7 H7OA 0.9767 .
O7 H7OB 0.8752 .
O8 H8OA 0.8575 .
O8 H8OB 0.9611 .
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
N2 H2A O8 0.90 2.27 3.079(3) 148.9 .
O7 H7OB O8 0.88 1.92 2.790(4) 175.5 .
N2 H2B O5 0.90 2.19 3.018(3) 152.5 2_566
O8 H8OA O2 0.86 1.95 2.807(3) 177.7 2_565
O8 H8OB O6 0.96 2.05 2.977(3) 160.7 2_566
C1 H1 O6 0.93 2.52 2.975(3) 110.2 2_666
C2 H2 O3 0.93 2.42 3.305(3) 157.8 1_665
C7 H7B O4 0.97 2.59 3.494(4) 155.4 2_565
