#------------------------------------------------------------------------------
#$Date: 2016-03-26 00:44:48 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180094 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/40/7054023.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_7054023
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         'C10 H12 Cu N4 O4'
_chemical_formula_sum            'C10 H12 Cu N4 O4'
_chemical_formula_weight         315.78
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.762(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2518(2)
_cell_length_b                   8.3493(3)
_cell_length_c                   20.4560(7)
_cell_measurement_reflns_used    6253
_cell_measurement_temperature    295.0(2)
_cell_measurement_theta_max      29.1415
_cell_measurement_theta_min      3.4588
_cell_volume                     1238.45(7)
_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 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            11694
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         3.72
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_time  22.00
_diffrn_standards_number         7
_exptl_absorpt_coefficient_mu    1.780
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81061
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CrysAlis RED, (2005)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.694
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             644
_exptl_crystal_size_max          0.199
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.306
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     174
_refine_ls_number_reflns         2187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.067
_refine_ls_R_factor_all          0.0316
_refine_ls_R_factor_gt           0.0265
_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)+(0.0375P)²+0.7658P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0700
_refine_ls_wR_factor_ref         0.0723
_reflns_number_gt                1965
_reflns_number_total             2187
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3nj01541f2.cif
_cod_data_source_block           cu99
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7054023
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
C1 C 0.3853(3) 0.6274(3) 0.28448(13) 0.0328(6) Uani 1 1 d .
C2 C 0.4472(3) 0.5922(3) 0.34696(14) 0.0384(6) Uani 1 1 d .
C3 C 0.3111(3) 0.5026(3) 0.37466(12) 0.0355(6) Uani 1 1 d .
C4 C 0.2936(5) 0.4288(4) 0.44098(15) 0.0610(9) Uani 1 1 d .
C5 C 0.1509(4) 0.4725(3) 0.07187(12) 0.0401(6) Uani 1 1 d .
C6 C 0.2914(4) 0.3935(3) 0.04021(13) 0.0435(7) Uani 1 1 d .
C7 C 0.4207(3) 0.3600(3) 0.08762(12) 0.0337(6) Uani 1 1 d .
C8 C 0.6043(4) 0.2799(4) 0.08494(15) 0.0506(8) Uani 1 1 d .
C9 C -0.2199(3) 0.8281(3) 0.22376(12) 0.0270(5) Uani 1 1 d .
C10 C -0.2553(3) 0.7600(3) 0.15402(12) 0.0331(6) Uani 1 1 d .
Cu1 Cu 0.04320(4) 0.60340(3) 0.201400(13) 0.02639(12) Uani 1 1 d .
H1 H 0.4501 0.6880 0.2543 0.039 Uiso 1 1 calc R
H2 H 0.5585 0.6231 0.3662 0.046 Uiso 1 1 calc R
H2A H 0.0763 0.4366 0.3356 0.036 Uiso 1 1 calc R
H4 H 0.4124 0.4102 0.1806 0.034 Uiso 1 1 calc R
H4A H 0.2574 0.5093 0.4718 0.092 Uiso 1 1 calc R
H4B H 0.4101 0.3840 0.4543 0.092 Uiso 1 1 calc R
H4C H 0.2021 0.3458 0.4394 0.092 Uiso 1 1 calc R
H5 H 0.0443 0.5105 0.0514 0.048 Uiso 1 1 calc R
H6 H 0.2969 0.3684 -0.0040 0.052 Uiso 1 1 calc R
H8A H 0.6888 0.3330 0.1142 0.076 Uiso 1 1 calc R
H8B H 0.6501 0.2854 0.0412 0.076 Uiso 1 1 calc R
H8C H 0.5920 0.1698 0.0977 0.076 Uiso 1 1 calc R
N1 N 0.2204(3) 0.5629(2) 0.27340(9) 0.0270(4) Uani 1 1 d .
N2 N 0.1775(3) 0.4879(2) 0.32954(9) 0.0296(5) Uani 1 1 d .
N3 N 0.1880(3) 0.4872(2) 0.13538(9) 0.0304(5) Uani 1 1 d .
N4 N 0.3552(3) 0.4171(2) 0.14364(10) 0.0284(4) Uani 1 1 d .
O1 O -0.1366(2) 0.6600(2) 0.13463(8) 0.0367(4) Uani 1 1 d .
O2 O -0.3896(3) 0.8062(3) 0.12290(10) 0.0633(7) Uani 1 1 d .
O3 O -0.0720(2) 0.77709(19) 0.25120(8) 0.0293(4) Uani 1 1 d .
O4 O -0.3306(2) 0.9217(2) 0.24703(9) 0.0401(4) 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'
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
O1 Cu1 O3 84.17(7) .
O1 Cu1 N1 175.03(7) .
O3 Cu1 N1 90.96(7) .
O1 Cu1 N3 89.82(7) .
O3 Cu1 N3 161.81(8) .
N1 Cu1 N3 94.55(8) .
O1 Cu1 O4 91.94(7) 2_445
O3 Cu1 O4 87.65(7) 2_445
N1 Cu1 O4 88.82(7) 2_445
N3 Cu1 O4 109.76(8) 2_445
C1 N1 N2 105.1(2) .
C1 N1 Cu1 129.37(17) .
N2 N1 Cu1 124.13(15) .
C3 N2 N1 111.88(19) .
C3 N2 H2A 124.1 .
N1 N2 H2A 124.1 .
C5 N3 N4 104.57(19) .
C5 N3 Cu1 127.63(17) .
N4 N3 Cu1 127.56(15) .
C7 N4 N3 112.0(2) .
C7 N4 H4 124.0 .
N3 N4 H4 124.0 .
C10 O1 Cu1 113.24(15) .
C9 O3 Cu1 112.25(14) .
C9 O4 Cu1 177.04(18) 2_455
N1 C1 C2 110.6(2) .
N1 C1 H1 124.7 .
C2 C1 H1 124.7 .
C3 C2 C1 105.8(2) .
C3 C2 H2 127.1 .
C1 C2 H2 127.1 .
N2 C3 C2 106.6(2) .
N2 C3 C4 121.3(2) .
C2 C3 C4 132.2(3) .
C3 C4 H4A 109.5 .
C3 C4 H4B 109.5 .
H4A C4 H4B 109.5 .
C3 C4 H4C 109.5 .
H4A C4 H4C 109.5 .
H4B C4 H4C 109.5 .
N3 C5 C6 111.2(2) .
N3 C5 H5 124.4 .
C6 C5 H5 124.4 .
C7 C6 C5 105.5(2) .
C7 C6 H6 127.2 .
C5 C6 H6 127.2 .
N4 C7 C6 106.7(2) .
N4 C7 C8 121.3(2) .
C6 C7 C8 132.0(2) .
C7 C8 H8A 109.5 .
C7 C8 H8B 109.5 .
H8A C8 H8B 109.5 .
C7 C8 H8C 109.5 .
H8A C8 H8C 109.5 .
H8B C8 H8C 109.5 .
O4 C9 O3 126.5(2) .
O4 C9 C10 119.4(2) .
O3 C9 C10 114.16(19) .
O2 C10 O1 125.9(2) .
O2 C10 C9 119.0(2) .
O1 C10 C9 115.1(2) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.9345(16) .
Cu1 O3 1.9651(15) .
Cu1 N1 1.9708(19) .
Cu1 N3 1.9766(19) .
Cu1 O4 2.4157(17) 2_445
N1 C1 1.329(3) .
N1 N2 1.348(3) .
N2 C3 1.335(3) .
N2 H2A 0.8600 .
N3 C5 1.329(3) .
N3 N4 1.355(3) .
N4 C7 1.334(3) .
N4 H4 0.8600 .
O1 C10 1.267(3) .
O2 C10 1.219(3) .
O3 C9 1.277(3) .
O4 C9 1.221(3) .
O4 Cu1 2.4157(17) 2_455
C1 C2 1.381(4) .
C1 H1 0.9300 .
C2 C3 1.367(4) .
C2 H2 0.9300 .
C3 C4 1.497(4) .
C4 H4A 0.9600 .
C4 H4B 0.9600 .
C4 H4C 0.9600 .
C5 C6 1.382(4) .
C5 H5 0.9300 .
C6 C7 1.369(4) .
C6 H6 0.9300 .
C7 C8 1.492(3) .
C8 H8A 0.9600 .
C8 H8B 0.9600 .
C8 H8C 0.9600 .
C9 C10 1.554(3) .
