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#$Date: 2023-01-19 10:27:24 +0200 (Thu, 19 Jan 2023) $
#$Revision: 280431 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/64/8106490.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_8106490
loop_
_publ_author_name
'Brito, Iván'
'Cárdenas, Alejandro'
'Bolte, Michael'
'Llanos, Jaime'
_publ_section_title
;
 Crystal structure of
 catena-poly[diaqua-bis(μ2-ethane-1,2-diyl-bis(pyridine-3-carboxylate-κ2
 N:N′))copper(II)] dinitrate, C28H28CuN6O16
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              225
_journal_page_last               226
_journal_paper_doi               10.1515/ncrs-2016-0215
_journal_volume                  232
_journal_year                    2017
_chemical_formula_moiety         'C28 H28 Cu N4 O10, 2(N O3)'
_chemical_formula_sum            'C28 H28 Cu N6 O16'
_chemical_formula_weight         768.10
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                92.109(7)
_cell_angle_beta                 105.804(7)
_cell_angle_gamma                98.416(7)
_cell_formula_units_Z            1
_cell_length_a                   7.3118(7)
_cell_length_b                   10.0597(8)
_cell_length_c                   11.2579(10)
_cell_measurement_reflns_used    6034
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.9
_cell_measurement_theta_min      3.5
_cell_volume                     785.63(12)
_computing_cell_refinement       'X-Area (Stoe & Cie, 2001)'
_computing_data_collection       'X-Area (Stoe & Cie, 2001)'
_computing_data_reduction        'X-Area (Stoe & Cie, 2001)'
_computing_molecular_graphics    'XP (Sheldrick, 2008)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008) '
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008) '
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'STOE IPDS II two-circle-diffractometer'
_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  0.0655
_diffrn_reflns_av_sigmaI/netI    0.0753
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8041
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.62
_diffrn_reflns_theta_min         3.46
_diffrn_standards_interval_count .
_diffrn_standards_interval_time  .
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.784
_exptl_absorpt_correction_T_max  0.9328
_exptl_absorpt_correction_T_min  0.8282
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULABS (Spek, 2003; Blessing, 1995)'
_exptl_crystal_colour            'light blue'
_exptl_crystal_density_diffrn    1.624
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             395
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.424
_refine_diff_density_rms         0.071
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.936
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2918
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.937
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0419
_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)+(0.0450P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0905
_refine_ls_wR_factor_ref         0.0954
_reflns_number_gt                2226
_reflns_number_total             2918
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            suppl_ncrs-2016-0215_suppl.cif
_cod_data_source_block           ib13
_cod_original_sg_symbol_H-M      'P-1 '
_cod_database_code               8106490
_publcif_info_exptl_table_max_cols 4
_publcif_info_exptl_table_use_headnotes n
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.5000 0.0000 0.0000 0.02006(16) Uani 1 2 d S . .
C1 C 0.2579(4) 0.2108(3) 0.3625(3) 0.0244(6) Uani 1 1 d . . .
O1 O 0.0967(3) 0.1960(2) 0.2954(2) 0.0377(6) Uani 1 1 d . . .
O2 O 0.3206(3) 0.2916(2) 0.4681(2) 0.0271(5) Uani 1 1 d . . .
C2 C 0.1811(5) 0.3675(3) 0.4964(3) 0.0310(7) Uani 1 1 d . . .
H2A H 0.0840 0.3076 0.5246 0.037 Uiso 1 1 calc R . .
H2B H 0.1140 0.4095 0.4222 0.037 Uiso 1 1 calc R . .
C3 C 0.2928(5) 0.4739(3) 0.5973(3) 0.0279(7) Uani 1 1 d . . .
H3A H 0.3963 0.5291 0.5710 0.033 Uiso 1 1 calc R . .
H3B H 0.2066 0.5340 0.6158 0.033 Uiso 1 1 calc R . .
O3 O 0.3749(3) 0.40688(19) 0.7058(2) 0.0264(5) Uani 1 1 d . . .
O4 O 0.5727(4) 0.5992(2) 0.7885(3) 0.0469(7) Uani 1 1 d . . .
C4 C 0.5167(5) 0.4820(3) 0.7940(3) 0.0254(7) Uani 1 1 d . . .
C11 C 0.4137(4) 0.1429(3) 0.3400(3) 0.0198(6) Uani 1 1 d . . .
C12 C 0.3929(4) 0.0949(3) 0.2188(3) 0.0220(6) Uani 1 1 d . . .
H12 H 0.2796 0.1050 0.1564 0.026 Uiso 1 1 calc R . .
N13 N 0.5269(4) 0.0348(2) 0.1865(2) 0.0219(5) Uani 1 1 d . . .
C14 C 0.6839(4) 0.0180(3) 0.2770(3) 0.0239(6) Uani 1 1 d . . .
H14 H 0.7777 -0.0269 0.2559 0.029 Uiso 1 1 calc R . .
C15 C 0.7138(5) 0.0635(3) 0.3991(3) 0.0257(6) Uani 1 1 d . . .
H15 H 0.8258 0.0491 0.4605 0.031 Uiso 1 1 calc R . .
C16 C 0.5796(4) 0.1302(3) 0.4313(3) 0.0245(6) Uani 1 1 d . . .
H16 H 0.6006 0.1664 0.5139 0.029 Uiso 1 1 calc R . .
C21 C 0.5991(4) 0.4043(3) 0.8991(3) 0.0221(6) Uani 1 1 d . . .
C22 C 0.5277(4) 0.2696(3) 0.9040(3) 0.0224(6) Uani 1 1 d . . .
H22 H 0.4199 0.2270 0.8391 0.027 Uiso 1 1 calc R . .
N23 N 0.6048(3) 0.1977(2) 0.9966(2) 0.0214(5) Uani 1 1 d . . .
C24 C 0.7577(4) 0.2598(3) 1.0881(3) 0.0270(7) Uani 1 1 d . . .
H24 H 0.8149 0.2091 1.1537 0.032 Uiso 1 1 calc R . .
C25 C 0.8345(5) 0.3940(3) 1.0905(3) 0.0299(7) Uani 1 1 d . . .
H25 H 0.9403 0.4349 1.1573 0.036 Uiso 1 1 calc R . .
C26 C 0.7553(4) 0.4676(3) 0.9944(3) 0.0254(7) Uani 1 1 d . . .
H26 H 0.8065 0.5598 0.9934 0.030 Uiso 1 1 calc R . .
N11 N -0.0596(4) 0.2595(3) -0.2635(3) 0.0363(7) Uani 1 1 d . . .
O11 O 0.0037(5) 0.2673(3) -0.1473(2) 0.0526(7) Uani 1 1 d . . .
O12 O -0.1320(4) 0.3540(2) -0.3170(3) 0.0503(7) Uani 1 1 d . . .
O13 O -0.0446(5) 0.1571(3) -0.3224(3) 0.0568(8) Uani 1 1 d . . .
O1W O 0.1524(5) 0.0474(3) -0.0595(2) 0.0481(7) Uani 1 1 d D . .
H1WA H 0.094(5) 0.111(3) -0.092(4) 0.072 Uiso 1 1 d D . .
H1WB H 0.0843 0.0018 -0.0116 0.072 Uiso 0.50 1 d PR A 1
H1WC H 0.0885 -0.0116 -0.1145 0.072 Uiso 0.50 1 d PR A 2
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
N23 Cu1 N23 180.0 2_656 1_554
N23 Cu1 N13 91.09(9) 2_656 .
N23 Cu1 N13 88.91(9) 1_554 .
N23 Cu1 N13 88.91(9) 2_656 2_655
N23 Cu1 N13 91.09(9) 1_554 2_655
N13 Cu1 N13 180.0 . 2_655
O1 C1 O2 124.1(3) . .
O1 C1 C11 124.6(3) . .
O2 C1 C11 111.3(2) . .
C1 O2 C2 115.8(2) . .
O2 C2 C3 106.4(2) . .
O2 C2 H2A 110.5 . .
C3 C2 H2A 110.5 . .
O2 C2 H2B 110.5 . .
C3 C2 H2B 110.5 . .
H2A C2 H2B 108.6 . .
O3 C3 C2 107.9(2) . .
O3 C3 H3A 110.1 . .
C2 C3 H3A 110.1 . .
O3 C3 H3B 110.1 . .
C2 C3 H3B 110.1 . .
H3A C3 H3B 108.4 . .
C4 O3 C3 115.9(2) . .
O4 C4 O3 124.0(3) . .
O4 C4 C21 123.5(3) . .
O3 C4 C21 112.5(2) . .
C16 C11 C12 119.1(3) . .
C16 C11 C1 123.7(3) . .
C12 C11 C1 117.1(3) . .
N13 C12 C11 122.6(3) . .
N13 C12 H12 118.7 . .
C11 C12 H12 118.7 . .
C12 N13 C14 117.8(3) . .
C12 N13 Cu1 118.0(2) . .
C14 N13 Cu1 123.6(2) . .
N13 C14 C15 122.6(3) . .
N13 C14 H14 118.7 . .
C15 C14 H14 118.7 . .
C14 C15 C16 119.5(3) . .
C14 C15 H15 120.3 . .
C16 C15 H15 120.3 . .
C15 C16 C11 118.3(3) . .
C15 C16 H16 120.8 . .
C11 C16 H16 120.8 . .
C22 C21 C26 119.1(3) . .
C22 C21 C4 122.0(3) . .
C26 C21 C4 118.9(2) . .
N23 C22 C21 122.4(3) . .
N23 C22 H22 118.8 . .
C21 C22 H22 118.8 . .
C22 N23 C24 118.0(2) . .
C22 N23 Cu1 121.55(19) . 1_556
C24 N23 Cu1 120.4(2) . 1_556
N23 C24 C25 122.8(3) . .
N23 C24 H24 118.6 . .
C25 C24 H24 118.6 . .
C26 C25 C24 119.0(3) . .
C26 C25 H25 120.5 . .
C24 C25 H25 120.5 . .
C25 C26 C21 118.6(3) . .
C25 C26 H26 120.7 . .
C21 C26 H26 120.7 . .
O13 N11 O12 121.5(3) . .
O13 N11 O11 118.0(3) . .
O12 N11 O11 120.4(3) . .
H1WA O1W H1WB 109.3 . .
H1WA O1W H1WC 95.0 . .
H1WB O1W H1WC 83.8 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N23 2.030(2) 2_656
Cu1 N23 2.030(2) 1_554
Cu1 N13 2.066(2) .
Cu1 N13 2.066(2) 2_655
C1 O1 1.199(4) .
C1 O2 1.345(4) .
C1 C11 1.484(4) .
O2 C2 1.453(4) .
C2 C3 1.500(4) .
C2 H2A 0.9900 .
C2 H2B 0.9900 .
C3 O3 1.445(4) .
C3 H3A 0.9900 .
C3 H3B 0.9900 .
O3 C4 1.336(4) .
O4 C4 1.199(4) .
C4 C21 1.482(4) .
C11 C16 1.385(4) .
C11 C12 1.391(4) .
C12 N13 1.345(4) .
C12 H12 0.9500 .
N13 C14 1.348(4) .
C14 C15 1.381(4) .
C14 H14 0.9500 .
C15 C16 1.384(4) .
C15 H15 0.9500 .
C16 H16 0.9500 .
C21 C22 1.387(4) .
C21 C26 1.390(4) .
C22 N23 1.335(4) .
C22 H22 0.9500 .
N23 C24 1.350(4) .
N23 Cu1 2.030(2) 1_556
C24 C25 1.380(4) .
C24 H24 0.9500 .
C25 C26 1.377(5) .
C25 H25 0.9500 .
C26 H26 0.9500 .
N11 O13 1.240(4) .
N11 O12 1.250(4) .
N11 O11 1.258(4) .
O1W H1WA 0.864(10) .
O1W H1WB 0.9206 .
O1W H1WC 0.8292 .
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
O1W H1WA O11 0.864(10) 1.852(13) 2.708(4) 171(4) .
O1W H1WB O1W 0.92 2.10 2.961(6) 155.1 2
O1W H1WC O1 0.83 2.63 3.456(4) 176.4 2
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
O1 C1 O2 C2 -2.4(4) . . . .
C11 C1 O2 C2 177.6(2) . . . .
C1 O2 C2 C3 -166.0(2) . . . .
O2 C2 C3 O3 -64.5(3) . . . .
C2 C3 O3 C4 163.8(3) . . . .
C3 O3 C4 O4 2.2(4) . . . .
C3 O3 C4 C21 -177.2(2) . . . .
O1 C1 C11 C16 -161.4(3) . . . .
O2 C1 C11 C16 18.7(4) . . . .
O1 C1 C11 C12 21.4(4) . . . .
O2 C1 C11 C12 -158.5(2) . . . .
C16 C11 C12 N13 0.9(4) . . . .
C1 C11 C12 N13 178.2(2) . . . .
C11 C12 N13 C14 1.9(4) . . . .
C11 C12 N13 Cu1 -169.14(19) . . . .
N23 Cu1 N13 C12 -102.42(19) 2_656 . . .
N23 Cu1 N13 C12 77.58(19) 1_554 . . .
N23 Cu1 N13 C14 87.1(2) 2_656 . . .
N23 Cu1 N13 C14 -92.9(2) 1_554 . . .
C12 N13 C14 C15 -2.0(4) . . . .
Cu1 N13 C14 C15 168.5(2) . . . .
N13 C14 C15 C16 -0.6(4) . . . .
C14 C15 C16 C11 3.3(4) . . . .
C12 C11 C16 C15 -3.4(4) . . . .
C1 C11 C16 C15 179.4(2) . . . .
O4 C4 C21 C22 178.3(3) . . . .
O3 C4 C21 C22 -2.2(4) . . . .
O4 C4 C21 C26 -3.1(5) . . . .
O3 C4 C21 C26 176.4(3) . . . .
C26 C21 C22 N23 -0.7(5) . . . .
C4 C21 C22 N23 177.9(3) . . . .
C21 C22 N23 C24 0.1(4) . . . .
C21 C22 N23 Cu1 -179.0(2) . . . 1_556
C22 N23 C24 C25 1.0(5) . . . .
Cu1 N23 C24 C25 -179.9(3) 1_556 . . .
N23 C24 C25 C26 -1.4(5) . . . .
C24 C25 C26 C21 0.8(5) . . . .
C22 C21 C26 C25 0.3(4) . . . .
C4 C21 C26 C25 -178.4(3) . . . .
loop_
_publcif_info_datablock.id
_publcif_info_datablock.publ_exptl
_publcif_info_datablock.publ_geom
_publcif_info_datablock.structure
{9d99ffef-84c8-434f-8ef9-27154260bbde} y y y
loop_
_publcif_info_exptl_table_extra_item
sin_theta_over_lambda_max
loop_
_publcif_info_tables.block_id
_publcif_info_tables.reference_item
{9d99ffef-84c8-434f-8ef9-27154260bbde} '_publcif_info_datablock.publ_exptl'
{9d99ffef-84c8-434f-8ef9-27154260bbde} '_geom_hbond_atom_site_label_D'
