#------------------------------------------------------------------------------
#$Date: 2022-11-15 11:57:11 +0200 (Tue, 15 Nov 2022) $
#$Revision: 279290 $
#$URL: file:///home/coder/svn-repositories/cod/cif/8/10/60/8106096.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_8106096
loop_
_publ_author_name
'Xiangqing, Fang'
'Jiajia, Xu'
'Qi, Wu'
'Liguo, Yang'
'Ya, Li'
_publ_section_title
;
 Crystal structure of catena-poly[(μ 2-dicyanamido-κ 2 N:N′)-(μ
 2-2-(pyridin-2-yl)ethan-1-olato-κ 3 N,O:O′)copper(II)], C9H8CuN4O
;
_journal_issue                   2
_journal_name_full
'Zeitschrift für Kristallographie - New Crystal Structures'
_journal_page_first              193
_journal_page_last               194
_journal_paper_doi               10.1515/ncrs-2017-0186
_journal_volume                  233
_journal_year                    2018
_chemical_formula_sum            'C18 H16 Cu2 N8 O2'
_chemical_formula_weight         503.47
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_cell_angle_alpha                109.201(2)
_cell_angle_beta                 106.6290(10)
_cell_angle_gamma                105.4100(10)
_cell_formula_units_Z            1
_cell_length_a                   7.6740(6)
_cell_length_b                   8.6401(8)
_cell_length_c                   8.8869(9)
_cell_measurement_reflns_used    991
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.563
_cell_measurement_theta_min      2.661
_cell_volume                     489.21(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0265
_diffrn_reflns_av_unetI/netI     0.0547
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            2520
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.661
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.207
_exptl_absorpt_correction_T_max  0.7623
_exptl_absorpt_correction_T_min  0.6665
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.709
_exptl_crystal_description       block
_exptl_crystal_F_000             254
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.130
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.293
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.971
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1710
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.971
_refine_ls_R_factor_all          0.0537
_refine_ls_R_factor_gt           0.0406
_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)+(0.0516P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0928
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1351
_reflns_number_total             1710
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            suppl_ncrs-2017-0186_suppl.cif
_cod_data_source_block           1
_cod_database_code               8106096
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_min   0.667
_shelx_estimated_absorpt_t_max   0.762
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu1 Cu 0.51395(7) 0.44079(6) 0.32654(7) 0.0417(2) Uani 1 1 d . . . . .
O1 O 0.3834(4) 0.3509(3) 0.4552(4) 0.0432(7) Uani 1 1 d . . . . .
N1 N 0.7298(5) 0.5400(5) 0.2647(5) 0.0492(9) Uani 1 1 d . . . . .
C1 C 0.3281(6) 0.1747(5) 0.4360(6) 0.0445(10) Uani 1 1 d . . . . .
H1A H 0.1846 0.1155 0.3835 0.053 Uiso 1 1 calc R U . . .
H1B H 0.3760 0.1764 0.5503 0.053 Uiso 1 1 calc R U . . .
N2 N 1.0708(6) 0.6740(5) 0.3067(6) 0.0778(14) Uani 1 1 d . . . . .
C2 C 0.4104(7) 0.0707(6) 0.3236(6) 0.0473(11) Uani 1 1 d . . . . .
H2A H 0.5539 0.1297 0.3776 0.057 Uiso 1 1 calc R U . . .
H2B H 0.3749 -0.0476 0.3193 0.057 Uiso 1 1 calc R U . . .
N3 N 1.2734(6) 0.5396(5) 0.1896(6) 0.0601(10) Uani 1 1 d . . . . .
C3 C 0.3371(6) 0.0525(5) 0.1400(5) 0.0408(9) Uani 1 1 d . . . . .
N4 N 0.3865(5) 0.2047(4) 0.1219(4) 0.0387(8) Uani 1 1 d . . . . .
C4 C 0.2245(7) -0.1099(6) -0.0036(6) 0.0568(12) Uani 1 1 d . . . . .
H4 H 0.1889 -0.2141 0.0106 0.068 Uiso 1 1 calc R U . . .
C5 C 0.1641(7) -0.1177(7) -0.1701(6) 0.0628(13) Uani 1 1 d . . . . .
H5 H 0.0869 -0.2266 -0.2682 0.075 Uiso 1 1 calc R U . . .
C6 C 0.2197(7) 0.0368(6) -0.1874(6) 0.0532(12) Uani 1 1 d . . . . .
H6 H 0.1837 0.0350 -0.2973 0.064 Uiso 1 1 calc R U . . .
C7 C 0.3298(6) 0.1950(6) -0.0393(6) 0.0464(11) Uani 1 1 d . . . . .
H7 H 0.3668 0.3003 -0.0513 0.056 Uiso 1 1 calc R U . . .
C8 C 0.8893(6) 0.5934(5) 0.2791(6) 0.0449(10) Uani 1 1 d . . . . .
C9 C 1.1695(6) 0.5913(6) 0.2379(6) 0.0450(10) 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'
O O 0.0106 0.0060 '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'
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
O1 Cu1 O1 77.74(12) 2_666 .
O1 Cu1 N1 93.14(13) 2_666 .
O1 Cu1 N1 158.99(14) . .
O1 Cu1 N4 170.07(11) 2_666 .
O1 Cu1 N4 92.38(12) . .
N1 Cu1 N4 95.87(14) . .
O1 Cu1 N3 91.22(13) 2_666 1_455
O1 Cu1 N3 99.06(13) . 1_455
N1 Cu1 N3 100.03(14) . 1_455
N4 Cu1 N3 91.31(14) . 1_455
O1 Cu1 Cu1 39.01(7) 2_666 2_666
O1 Cu1 Cu1 38.73(8) . 2_666
N1 Cu1 Cu1 129.52(11) . 2_666
N4 Cu1 Cu1 131.10(9) . 2_666
N3 Cu1 Cu1 96.61(10) 1_455 2_666
C1 O1 Cu1 124.7(2) . 2_666
C1 O1 Cu1 124.5(2) . .
Cu1 O1 Cu1 102.26(12) 2_666 .
C8 N1 Cu1 156.3(4) . .
O1 C1 C2 111.7(3) . .
O1 C1 H1A 109.3 . .
C2 C1 H1A 109.3 . .
O1 C1 H1B 109.3 . .
C2 C1 H1B 109.3 . .
H1A C1 H1B 107.9 . .
C8 N2 C9 122.9(4) . .
C3 C2 C1 113.6(3) . .
C3 C2 H2A 108.8 . .
C1 C2 H2A 108.8 . .
C3 C2 H2B 108.8 . .
C1 C2 H2B 108.8 . .
H2A C2 H2B 107.7 . .
C9 N3 Cu1 129.4(4) . 1_655
N4 C3 C4 120.9(4) . .
N4 C3 C2 116.5(4) . .
C4 C3 C2 122.6(4) . .
C7 N4 C3 118.7(4) . .
C7 N4 Cu1 119.5(3) . .
C3 N4 Cu1 121.4(3) . .
C3 C4 C5 119.8(4) . .
C3 C4 H4 120.1 . .
C5 C4 H4 120.1 . .
C6 C5 C4 119.0(4) . .
C6 C5 H5 120.5 . .
C4 C5 H5 120.5 . .
C5 C6 C7 118.7(4) . .
C5 C6 H6 120.7 . .
C7 C6 H6 120.7 . .
N4 C7 C6 123.0(4) . .
N4 C7 H7 118.5 . .
C6 C7 H7 118.5 . .
N1 C8 N2 172.6(5) . .
N3 C9 N2 171.6(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 O1 1.923(3) 2_666
Cu1 O1 1.934(2) .
Cu1 N1 1.964(3) .
Cu1 N4 1.977(3) .
Cu1 N3 2.420(4) 1_455
Cu1 Cu1 3.0029(10) 2_666
O1 C1 1.404(5) .
O1 Cu1 1.923(3) 2_666
N1 C8 1.139(5) .
C1 C2 1.509(6) .
C1 H1A 0.9700 .
C1 H1B 0.9700 .
N2 C8 1.289(5) .
N2 C9 1.313(6) .
C2 C3 1.504(6) .
C2 H2A 0.9700 .
C2 H2B 0.9700 .
N3 C9 1.131(5) .
N3 Cu1 2.419(4) 1_655
C3 N4 1.344(5) .
C3 C4 1.375(6) .
N4 C7 1.339(5) .
C4 C5 1.391(6) .
C4 H4 0.9300 .
C5 C6 1.363(6) .
C5 H5 0.9300 .
C6 C7 1.371(6) .
C6 H6 0.9300 .
C7 H7 0.9300 .
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
Cu1 O1 C1 C2 -133.3(3) 2_666 . . .
Cu1 O1 C1 C2 8.8(5) . . . .
O1 C1 C2 C3 -61.7(5) . . . .
C1 C2 C3 N4 63.1(5) . . . .
C1 C2 C3 C4 -116.6(4) . . . .
C4 C3 N4 C7 -2.3(6) . . . .
C2 C3 N4 C7 178.0(4) . . . .
C4 C3 N4 Cu1 171.0(3) . . . .
C2 C3 N4 Cu1 -8.8(5) . . . .
N4 C3 C4 C5 1.3(7) . . . .
C2 C3 C4 C5 -179.0(4) . . . .
C3 C4 C5 C6 0.6(7) . . . .
C4 C5 C6 C7 -1.4(7) . . . .
C3 N4 C7 C6 1.4(6) . . . .
Cu1 N4 C7 C6 -171.9(3) . . . .
C5 C6 C7 N4 0.4(7) . . . .
