#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:49:25 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179079 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/41/4304198.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_4304198
loop_
_publ_author_name
'Alexander M. Kirillov'
'Yauhen Y. Karabach'
'Matti Haukka'
'M. Fátima C. Guedes da Silva'
'Joaquin Sanchiz'
'Maximilian N. Kopylovich'
'Armando J. L. Pombeiro'
_publ_section_title
;
Self-Assembled Copper(II) Coordination Polymers Derived from
Aminopolyalcohols and Benzenepolycarboxylates: Structural and Magnetic
Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              162
_journal_page_last               175
_journal_paper_doi               10.1021/ic701669x
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C21 H35 Cu2 N2 Na O14, 6(H2 O)'
_chemical_formula_sum            'C21 H47 Cu2 N2 Na O20'
_chemical_formula_weight         797.68
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   mixed
_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                   14.6973(2)
_cell_length_b                   17.7243(5)
_cell_length_c                   12.4624(3)
_cell_measurement_reflns_used    13074
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     3246.45(13)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Bruker AXS BV, 1997-2004)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'Diamond v.3.1d (Brandenburg, 2006)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '95mm CCD camera on κ-goniostat'
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'φ scans and ω scans with κ offset'
_diffrn_radiation_monochromator  'horizontally mounted graphite crystal'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0734
_diffrn_reflns_av_sigmaI/netI    0.0333
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            52474
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         2.82
_exptl_absorpt_coefficient_mu    1.409
_exptl_absorpt_correction_T_max  0.9445
_exptl_absorpt_correction_T_min  0.8070
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v.2.10 (Sheldrick, 2003)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.632
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.539
_refine_diff_density_min         -0.499
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         3713
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0510
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0332P)²+3.1912P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0724
_refine_ls_wR_factor_ref         0.0803
_reflns_number_gt                2908
_reflns_number_total             3713
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic701669x-file001_2.cif
_cod_data_source_block           structure_3
_cod_database_code               4304198
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.070845(16) 0.230816(15) 0.32680(2) 0.01148(9) Uani 1 1 d . . .
Na1 Na 0.0000 0.07151(7) 0.2500 0.0201(3) Uani 1 2 d S . .
O1 O 0.11828(10) 0.10061(9) 0.37029(13) 0.0170(3) Uani 1 1 d D . .
H1D H 0.1051(17) 0.1112(15) 0.4447(10) 0.025 Uiso 1 1 d D . .
O2 O 0.05703(9) 0.20168(9) 0.17661(12) 0.0133(3) Uani 1 1 d . . .
O3 O 0.09403(10) 0.36137(9) 0.28276(14) 0.0203(4) Uani 1 1 d D . .
H3D H 0.0681(17) 0.4089(9) 0.302(2) 0.030 Uiso 1 1 d D . .
O4 O 0.07461(10) 0.26130(9) 0.47798(12) 0.0146(3) Uani 1 1 d . . .
O5 O 0.05744(11) 0.15035(9) 0.56112(13) 0.0189(3) Uani 1 1 d . . .
O6 O 0.02355(10) 0.50014(9) 0.83504(13) 0.0192(4) Uani 1 1 d . . .
O7 O -0.10064(12) -0.02818(10) 0.29997(14) 0.0248(4) Uani 1 1 d D . .
H7D H -0.0840(19) -0.0700(12) 0.347(2) 0.037 Uiso 1 1 d D . .
H7E H -0.1529(13) -0.0044(16) 0.332(2) 0.037 Uiso 1 1 d D . .
O8 O 0.23614(12) 0.03791(11) 0.08457(15) 0.0291(4) Uani 1 1 d D . .
H8D H 0.2003(17) 0.0473(18) 0.0208(15) 0.044 Uiso 1 1 d D . .
H8E H 0.2888(14) 0.0113(16) 0.059(2) 0.044 Uiso 1 1 d D . .
O9 O -0.11520(12) 0.07307(10) 0.57625(16) 0.0284(4) Uani 1 1 d D . .
H9D H -0.0571(12) 0.0966(17) 0.565(3) 0.043 Uiso 1 1 d D . .
H9E H -0.110(2) 0.0491(17) 0.6454(14) 0.043 Uiso 1 1 d D . .
O10 O 0.11503(11) 0.45117(11) 1.02058(15) 0.0287(4) Uani 1 1 d D . .
H10D H 0.0688(16) 0.4559(19) 1.0757(18) 0.043 Uiso 1 1 d D . .
H10E H 0.0878(19) 0.4655(18) 0.9531(14) 0.043 Uiso 1 1 d D . .
N1 N 0.20677(12) 0.23722(11) 0.29432(15) 0.0141(4) Uani 1 1 d . . .
C1 C 0.21432(15) 0.10101(13) 0.35219(19) 0.0179(5) Uani 1 1 d . . .
H1A H 0.2270 0.0807 0.2797 0.021 Uiso 1 1 calc R . .
H1B H 0.2441 0.0675 0.4052 0.021 Uiso 1 1 calc R . .
C2 C 0.25488(15) 0.17992(13) 0.36132(19) 0.0179(5) Uani 1 1 d . . .
H2A H 0.2527 0.1960 0.4373 0.021 Uiso 1 1 calc R . .
H2B H 0.3196 0.1780 0.3394 0.021 Uiso 1 1 calc R . .
C3 C 0.12855(14) 0.23519(13) 0.11585(18) 0.0161(5) Uani 1 1 d . . .
H3A H 0.1175 0.2899 0.1073 0.019 Uiso 1 1 calc R . .
H3B H 0.1317 0.2120 0.0437 0.019 Uiso 1 1 calc R . .
C4 C 0.21758(14) 0.22197(13) 0.17647(17) 0.0149(5) Uani 1 1 d . . .
H4A H 0.2374 0.1691 0.1659 0.018 Uiso 1 1 calc R . .
H4B H 0.2653 0.2554 0.1469 0.018 Uiso 1 1 calc R . .
C5 C 0.18883(15) 0.37583(14) 0.2705(2) 0.0211(5) Uani 1 1 d . . .
H5A H 0.2045 0.4250 0.3035 0.025 Uiso 1 1 calc R . .
H5B H 0.2047 0.3780 0.1934 0.025 Uiso 1 1 calc R . .
C6 C 0.24158(15) 0.31314(13) 0.32473(19) 0.0184(5) Uani 1 1 d . . .
H6A H 0.3065 0.3170 0.3045 0.022 Uiso 1 1 calc R . .
H6B H 0.2372 0.3192 0.4035 0.022 Uiso 1 1 calc R . .
C7 C 0.05487(14) 0.22148(13) 0.55844(18) 0.0136(5) Uani 1 1 d . . .
C8 C 0.02622(14) 0.26337(13) 0.65798(17) 0.0132(4) Uani 1 1 d . . .
C9 C 0.02465(14) 0.34211(13) 0.65776(17) 0.0143(4) Uani 1 1 d . . .
H9 H 0.0404 0.3690 0.5945 0.017 Uiso 1 1 calc R . .
C10 C 0.0000 0.38122(18) 0.7500 0.0146(6) Uani 1 2 d S . .
C11 C 0.0000 0.46647(19) 0.7500 0.0155(7) Uani 1 2 d S . .
C12 C 0.0000 0.22423(18) 0.7500 0.0133(6) Uani 1 2 d S . .
H12 H 0.0000 0.1706 0.7500 0.016 Uiso 1 2 calc SR . .
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'
Na Na 0.0362 0.0249 '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
_geom_angle_publ_flag
O2 Cu1 O2 78.97(7) 4 . ?
O2 Cu1 O4 96.96(6) 4 . ?
O2 Cu1 O4 175.61(6) . . yes
O2 Cu1 N1 162.51(7) 4 . ?
O2 Cu1 N1 85.78(7) . . ?
O4 Cu1 N1 98.49(7) . . ?
O2 Cu1 O3 112.76(6) 4 . ?
O2 Cu1 O3 92.89(6) . . yes
O4 Cu1 O3 87.14(6) . . ?
N1 Cu1 O3 76.25(6) . . yes
O2 Cu1 Cu1 43.57(4) 4 4 ?
O2 Cu1 Cu1 43.50(4) . 4 ?
O4 Cu1 Cu1 132.15(5) . 4 ?
N1 Cu1 Cu1 125.89(5) . 4 ?
O3 Cu1 Cu1 87.12(4) . 4 ?
O2 Cu1 Na1 55.86(5) 4 . ?
O2 Cu1 Na1 55.85(5) . . ?
O4 Cu1 Na1 123.16(5) . . ?
N1 Cu1 Na1 108.20(5) . . ?
O3 Cu1 Na1 147.01(4) . . ?
Cu1 Cu1 Na1 63.397(12) 4 . ?
O1 Na1 O1 154.68(10) . 4 ?
O1 Na1 O7 116.99(6) . . ?
O1 Na1 O7 82.57(6) 4 . ?
O1 Na1 O7 82.57(6) . 4 ?
O1 Na1 O7 116.99(6) 4 4 ?
O7 Na1 O7 84.50(10) . 4 ?
O1 Na1 O2 78.05(6) . . yes
O1 Na1 O2 79.68(6) 4 . ?
O7 Na1 O2 160.27(6) . . yes
O7 Na1 O2 111.26(5) 4 . ?
O1 Na1 O2 79.68(6) . 4 ?
O1 Na1 O2 78.05(6) 4 4 ?
O7 Na1 O2 111.26(5) . 4 ?
O7 Na1 O2 160.27(6) 4 4 ?
O2 Na1 O2 56.53(7) . 4 ?
O1 Na1 Cu1 50.75(4) . . ?
O1 Na1 Cu1 103.93(6) 4 . ?
O7 Na1 Cu1 141.92(5) . . ?
O7 Na1 Cu1 122.45(4) 4 . ?
O2 Na1 Cu1 38.08(4) . . ?
O2 Na1 Cu1 38.02(4) 4 . ?
O1 Na1 Cu1 103.93(6) . 4 ?
O1 Na1 Cu1 50.75(4) 4 4 ?
O7 Na1 Cu1 122.45(4) . 4 ?
O7 Na1 Cu1 141.91(5) 4 4 ?
O2 Na1 Cu1 38.02(4) . 4 ?
O2 Na1 Cu1 38.08(4) 4 4 ?
Cu1 Na1 Cu1 53.21(2) . 4 ?
C1 O1 Na1 129.06(14) . . ?
C1 O1 H1D 110.4(16) . . ?
Na1 O1 H1D 120.4(16) . . ?
C3 O2 Cu1 126.09(13) . 4 ?
C3 O2 Cu1 108.81(13) . . ?
Cu1 O2 Cu1 92.93(6) 4 . ?
C3 O2 Na1 142.04(13) . . ?
Cu1 O2 Na1 86.13(5) 4 . ?
Cu1 O2 Na1 86.07(5) . . ?
C5 O3 Cu1 109.66(13) . . ?
C5 O3 H3D 105.0(17) . . ?
Cu1 O3 H3D 137.4(17) . . ?
C7 O4 Cu1 127.13(14) . . ?
Na1 O7 H7D 124.3(17) . . ?
Na1 O7 H7E 106.2(19) . . ?
H7D O7 H7E 106(3) . . ?
H8D O8 H8E 104(3) . . ?
H9D O9 H9E 104(3) . . ?
H10D O10 H10E 108(3) . . ?
C6 N1 C2 108.05(17) . . ?
C6 N1 C4 112.05(18) . . ?
C2 N1 C4 111.99(17) . . ?
C6 N1 Cu1 109.63(13) . . ?
C2 N1 Cu1 108.35(13) . . ?
C4 N1 Cu1 106.70(13) . . ?
O1 C1 C2 112.27(18) . . ?
O1 C1 H1A 109.1 . . ?
C2 C1 H1A 109.1 . . ?
O1 C1 H1B 109.1 . . ?
C2 C1 H1B 109.1 . . ?
H1A C1 H1B 107.9 . . ?
N1 C2 C1 113.40(18) . . ?
N1 C2 H2A 108.9 . . ?
C1 C2 H2A 108.9 . . ?
N1 C2 H2B 108.9 . . ?
C1 C2 H2B 108.9 . . ?
H2A C2 H2B 107.7 . . ?
O2 C3 C4 107.75(17) . . ?
O2 C3 H3A 110.2 . . ?
C4 C3 H3A 110.2 . . ?
O2 C3 H3B 110.2 . . ?
C4 C3 H3B 110.2 . . ?
H3A C3 H3B 108.5 . . ?
N1 C4 C3 111.42(17) . . ?
N1 C4 H4A 109.3 . . ?
C3 C4 H4A 109.3 . . ?
N1 C4 H4B 109.3 . . ?
C3 C4 H4B 109.3 . . ?
H4A C4 H4B 108.0 . . ?
O3 C5 C6 108.71(18) . . ?
O3 C5 H5A 109.9 . . ?
C6 C5 H5A 109.9 . . ?
O3 C5 H5B 109.9 . . ?
C6 C5 H5B 109.9 . . ?
H5A C5 H5B 108.3 . . ?
N1 C6 C5 111.96(18) . . ?
N1 C6 H6A 109.2 . . ?
C5 C6 H6A 109.2 . . ?
N1 C6 H6B 109.2 . . ?
C5 C6 H6B 109.2 . . ?
H6A C6 H6B 107.9 . . ?
O4 C7 O5 125.0(2) . . ?
O4 C7 C8 116.33(19) . . ?
O5 C7 C8 118.6(2) . . ?
C12 C8 C9 119.6(2) . . ?
C12 C8 C7 120.6(2) . . ?
C9 C8 C7 119.7(2) . . ?
C10 C9 C8 120.1(2) . . ?
C10 C9 H9 120.0 . . ?
C8 C9 H9 120.0 . . ?
C9 C10 C9 120.2(3) 4_556 . ?
C9 C10 C11 119.91(15) 4_556 . ?
C9 C10 C11 119.91(15) . . ?
O6 C11 O6 123.7(3) . 4_556 ?
O6 C11 C10 118.16(15) . . ?
O6 C11 C10 118.16(15) 4_556 . ?
C8 C12 C8 120.3(3) . 4_556 ?
C8 C12 H12 119.8 . . ?
C8 C12 H12 119.8 4_556 . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cu1 O2 1.9495(14) 4 yes
Cu1 O2 1.9521(15) . yes
Cu1 O4 1.9609(15) . yes
Cu1 N1 2.0415(18) . yes
Cu1 O3 2.4024(16) . yes
Cu1 Cu1 2.8285(5) 4 yes
Cu1 Na1 3.1580(12) . yes
Na1 O1 2.3528(16) . yes
Na1 O1 2.3528(16) 4 yes
Na1 O7 2.387(2) . yes
Na1 O7 2.387(2) 4 yes
Na1 O2 2.6196(19) . yes
Na1 O2 2.6196(19) 4 yes
Na1 Cu1 3.1580(12) 4 yes
O1 C1 1.429(3) . ?
O1 H1D 0.966(10) . ?
O2 C3 1.425(3) . ?
O2 Cu1 1.9495(14) 4 ?
O3 C5 1.425(3) . ?
O3 H3D 0.955(10) . ?
O4 C7 1.260(3) . ?
O5 C7 1.262(3) . ?
O6 C11 1.265(2) . ?
O7 H7D 0.973(10) . ?
O7 H7E 0.965(10) . ?
O8 H8D 0.969(10) . ?
O8 H8E 0.962(10) . ?
O9 H9D 0.960(10) . ?
O9 H9E 0.964(10) . ?
O10 H10D 0.970(10) . ?
O10 H10E 0.965(10) . ?
N1 C6 1.489(3) . ?
N1 C2 1.493(3) . ?
N1 C4 1.502(3) . ?
C1 C2 1.525(3) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C2 H2A 0.9900 . ?
C2 H2B 0.9900 . ?
C3 C4 1.529(3) . ?
C3 H3A 0.9900 . ?
C3 H3B 0.9900 . ?
C4 H4A 0.9900 . ?
C4 H4B 0.9900 . ?
C5 C6 1.514(3) . ?
C5 H5A 0.9900 . ?
C5 H5B 0.9900 . ?
C6 H6A 0.9900 . ?
C6 H6B 0.9900 . ?
C7 C8 1.506(3) . ?
C8 C12 1.395(3) . ?
C8 C9 1.396(3) . ?
C9 C10 1.390(3) . ?
C9 H9 0.9500 . ?
C10 C9 1.390(3) 4_556 ?
C10 C11 1.511(5) . ?
C11 O6 1.265(2) 4_556 ?
C12 C8 1.395(3) 4_556 ?
C12 H12 0.9500 . ?
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
_geom_hbond_publ_flag
O1 H1D O5 0.966(10) 1.754(13) 2.689(2) 162(2) . yes
O3 H3D O6 0.955(10) 1.789(10) 2.743(2) 178(3) 8_565 yes
O7 H7D O5 0.973(10) 1.871(10) 2.844(2) 177(3) 5_556 yes
O7 H7E O8 0.965(10) 1.769(12) 2.722(3) 169(3) 4 yes
O8 H8D O9 0.969(10) 1.798(12) 2.750(3) 167(3) 4 yes
O8 H8E O10 0.962(10) 1.833(11) 2.790(3) 173(3) 7_654 yes
O9 H9D O5 0.960(10) 1.935(11) 2.890(2) 172(3) . yes
O9 H9E O7 0.964(10) 1.966(13) 2.907(3) 165(3) 8_556 yes
O10 H10D O6 0.970(10) 1.920(15) 2.851(2) 160(3) 5_567 yes
O10 H10E O6 0.965(10) 1.853(11) 2.812(2) 172(3) . yes
