#------------------------------------------------------------------------------
#$Date: 2024-05-04 04:49:46 +0300 (Sat, 04 May 2024) $
#$Revision: 291489 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/31/24/2312480.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2312480
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Elsayed, Ahmed'
'DaCunha, Tristan'
'Bender, Christopher'
_publ_section_title
;
 Crystal structures, electron spin resonance, and thermogravimetric
 analysis of three mixed-valence copper cyanide polymers.
;
_journal_coeditor_code           DG3052
_journal_issue                   6
_journal_name_full
'Acta crystallographica. Section C, Structural chemistry'
_journal_paper_doi               10.1107/S2053229624003371
_journal_volume                  80
_journal_year                    2024
_chemical_formula_iupac          '[Cu3 (C N)4 (C2 H7 N1 O1)2]'
_chemical_formula_moiety         'C8 H14 Cu3 N6 O2'
_chemical_formula_sum            'C8 H14 Cu3 N6 O2'
_chemical_formula_weight         416.88
_chemical_name_systematic
;
Poly[bis(2-aminoethanol)tetra-μ-cyanido-tricopper(II)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 117.3580(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5158(2)
_cell_length_b                   8.8022(2)
_cell_length_c                   9.3589(2)
_cell_measurement_reflns_used    2164
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      28.8
_cell_measurement_theta_min      1.0
_cell_volume                     696.22(3)
_computing_cell_refinement
;
SCALEPACK (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
KappaCCD Server Software (Nonius, 1997)
;
_computing_data_reduction
;
DENZO and SCALEPACK (Otwinowski & Minor,1997)
;
_computing_molecular_graphics
;
ORTEPIII (Burnett & Johnson, 1996) and ORTEP-3 for Windows (Farrugia,
2012)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius KappaCCD'
_diffrn_measurement_method       'combination of ω and φ scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_unetI/netI     0.0222
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            27010
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         28.810
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.545
_exptl_absorpt_correction_T_max  0.59
_exptl_absorpt_correction_T_min  0.48
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Otwinowski & Minor,1997)
;
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             414
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.22
_refine_diff_density_max         1.065
_refine_diff_density_min         -0.533
_refine_ls_extinction_coef       0.0030(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method
;
SHELXL2018 (Sheldrick, 2015b)
;
_refine_ls_goodness_of_fit_ref   1.156
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     118
_refine_ls_number_reflns         1740
_refine_ls_number_restraints     26
_refine_ls_restrained_S_all      1.180
_refine_ls_R_factor_all          0.0570
_refine_ls_R_factor_gt           0.0236
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0263P)²+0.6300P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0541
_refine_ls_wR_factor_ref         0.0769
_reflns_number_gt                1049
_reflns_number_total             1740
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            dg3052.cif
_cod_data_source_block           3
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312480
_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   0.284
_shelx_estimated_absorpt_t_max   0.435
loop_
_space_group_symop_operation_xyz
'x, y, z'
'x, -y+1/2, z+1/2'
'-x, -y, -z'
'-x, y-1/2, -z-1/2'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cu Cu1 0.43137(4) -0.00194(4) -0.16664(4) 0.03507(14) Uani d 1 . .
Cu Cu2 0.000000 0.000000 0.000000 0.02951(14) Uani d 1 . .
C C1 0.2785(3) 0.0024(3) -0.0860(3) 0.0351(5) Uani d 1 . .
N N1 0.1773(3) 0.0056(3) -0.0525(3) 0.0369(5) Uani d 1 . .
C C2 0.5179(3) 0.3029(3) -0.2702(3) 0.0378(6) Uani d 0.5 . .
N N2 0.4816(3) 0.1875(3) -0.2405(3) 0.0398(6) Uani d 0.5 . .
N N2C 0.5179(3) 0.3029(3) -0.2702(3) 0.0378(6) Uani d 0.5 . .
C C2N 0.4816(3) 0.1875(3) -0.2405(3) 0.0398(6) Uani d 0.5 . .
O O11A 0.1498(19) -0.1514(11) 0.241(2) 0.0534(15) Uani d 0.643(14) A 1
H H11A 0.202(8) -0.226(5) 0.243(10) 0.051(15) Uiso d 0.643(14) A 1
C C12A 0.2544(10) -0.0467(8) 0.3618(7) 0.0484(19) Uani d 0.643(14) A 1
H H12A 0.290950 -0.088854 0.468798 0.073 Uiso calc 0.643(14) A 1
H H12B 0.345489 -0.023671 0.345150 0.073 Uiso calc 0.643(14) A 1
C C13A 0.1569(11) 0.0924(7) 0.3410(6) 0.0475(19) Uani d 0.643(14) A 1
H H13A 0.063915 0.066997 0.353403 0.071 Uiso calc 0.643(14) A 1
H H13B 0.217945 0.167214 0.421944 0.071 Uiso calc 0.643(14) A 1
N N14A 0.1096(3) 0.1541(3) 0.1812(3) 0.0448(6) Uani d 0.643(14) A 1
H H14A 0.195028 0.189574 0.176700 0.067 Uiso calc 0.643(14) A 1
H H14B 0.044412 0.232000 0.165357 0.067 Uiso calc 0.643(14) A 1
O O11B 0.143(4) -0.189(2) 0.249(4) 0.0534(15) Uani d 0.357(14) A 2
H H11B 0.220(11) -0.197(13) 0.232(17) 0.051(15) Uiso d 0.357(14) A 2
C C12B 0.171(2) -0.0648(17) 0.3598(13) 0.058(3) Uani d 0.357(14) A 2
H H12C 0.241443 -0.100736 0.467296 0.087 Uiso calc 0.357(14) A 2
H H12D 0.071231 -0.039347 0.358141 0.087 Uiso calc 0.357(14) A 2
C C13B 0.2362(19) 0.0704(15) 0.3333(12) 0.050(3) Uani d 0.357(14) A 2
H H13C 0.327766 0.046259 0.317901 0.075 Uiso calc 0.357(14) A 2
H H13D 0.270322 0.136169 0.426513 0.075 Uiso calc 0.357(14) A 2
N N14B 0.1096(3) 0.1541(3) 0.1812(3) 0.0448(6) Uani d 0.357(14) A 2
H H14C 0.155966 0.225597 0.150299 0.067 Uiso calc 0.357(14) A 2
H H14D 0.038556 0.198626 0.204402 0.067 Uiso calc 0.357(14) A 2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Cu Cu 0.3201 1.2651 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 Cu1 N2 . . 118.41(12) ?
C1 Cu1 C2 . 4_655 118.33(12) ?
N2 Cu1 C2 . 4_655 120.78(11) ?
C1 Cu1 Cu1 . 3_655 66.96(9) ?
N2 Cu1 Cu1 . 3_655 108.86(8) ?
C2 Cu1 Cu1 4_655 3_655 107.33(8) ?
N1 Cu2 N1 . 3 180.0 ?
N1 Cu2 N14A . 3 88.76(10) ?
N1 Cu2 N14A 3 3 91.24(10) ?
N1 Cu2 N14A . . 91.24(10) ?
N1 Cu2 N14A 3 . 88.76(10) ?
N14A Cu2 N14A 3 . 180.0 ?
N1 Cu2 N14B . . 91.24(10) ?
N1 Cu2 N14B 3 . 88.76(10) ?
N1 Cu2 O11B . 3 85.3(7) ?
N1 Cu2 O11B 3 3 94.7(7) ?
N14A Cu2 O11B 3 3 80.1(7) ?
N14A Cu2 O11B . 3 99.9(7) ?
N14B Cu2 O11B . 3 99.9(7) ?
N1 Cu2 O11B . . 94.7(7) ?
N1 Cu2 O11B 3 . 85.3(7) ?
N14B Cu2 O11B . . 80.1(7) ?
O11B Cu2 O11B 3 . 180.0 ?
N1 Cu2 O11A . . 92.4(4) ?
N1 Cu2 O11A 3 . 87.6(4) ?
N14A Cu2 O11A 3 . 105.3(3) ?
N14A Cu2 O11A . . 74.7(3) ?
N1 C1 Cu1 . . 173.7(3) ?
N1 C1 Cu1 . 3_655 114.4(2) ?
Cu1 C1 Cu1 . 3_655 71.84(9) ?
C1 N1 Cu2 . . 176.9(2) ?
N2 C2 Cu1 . 4_665 176.5(3) ?
C2 N2 Cu1 . . 174.0(3) ?
C12A O11A Cu2 . . 106.0(5) ?
C12A O11A H11A . . 108(6) ?
Cu2 O11A H11A . . 123(6) ?
C13A C12A O11A . . 104.9(8) ?
C13A C12A H12A . . 110.8 ?
O11A C12A H12A . . 110.8 ?
C13A C12A H12B . . 110.8 ?
O11A C12A H12B . . 110.8 ?
H12A C12A H12B . . 108.8 ?
N14A C13A C12A . . 108.7(6) ?
N14A C13A H13A . . 109.9 ?
C12A C13A H13A . . 109.9 ?
N14A C13A H13B . . 109.9 ?
C12A C13A H13B . . 109.9 ?
H13A C13A H13B . . 108.3 ?
C13A N14A Cu2 . . 113.8(3) ?
C13A N14A H14A . . 108.8 ?
Cu2 N14A H14A . . 108.8 ?
C13A N14A H14B . . 108.8 ?
Cu2 N14A H14B . . 108.8 ?
H14A N14A H14B . . 107.7 ?
C12B O11B Cu2 . . 90.3(10) ?
C12B O11B H11B . . 109(10) ?
Cu2 O11B H11B . . 91(9) ?
O11B C12B C13B . . 117.6(14) ?
O11B C12B H12C . . 107.9 ?
C13B C12B H12C . . 107.9 ?
O11B C12B H12D . . 107.9 ?
C13B C12B H12D . . 107.9 ?
H12C C12B H12D . . 107.2 ?
C12B C13B N14B . . 109.9(12) ?
C12B C13B H13C . . 109.7 ?
N14B C13B H13C . . 109.7 ?
C12B C13B H13D . . 109.7 ?
N14B C13B H13D . . 109.7 ?
H13C C13B H13D . . 108.2 ?
C13B N14B Cu2 . . 109.2(5) ?
C13B N14B H14C . . 109.8 ?
Cu2 N14B H14C . . 109.8 ?
C13B N14B H14D . . 109.8 ?
Cu2 N14B H14D . . 109.8 ?
H14C N14B H14D . . 108.3 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 C1 . 1.922(3) ?
Cu1 N2 . 1.947(3) ?
Cu1 C2 4_655 1.949(3) ?
Cu1 Cu1 3_655 2.7734(7) ?
Cu2 N1 . 1.963(2) ?
Cu2 N14A . 2.044(2) ?
Cu2 N14B . 2.044(2) ?
Cu2 O11B . 2.67(3) ?
Cu2 O11A . 2.439(14) ?
C1 N1 . 1.142(4) ?
C2 N2 . 1.147(4) ?
O11A C12A . 1.442(17) ?
O11A H11A . 0.817(10) ?
C12A C13A . 1.494(11) ?
C12A H12A . 0.9700 ?
C12A H12B . 0.9700 ?
C13A N14A . 1.454(6) ?
C13A H13A . 0.9700 ?
C13A H13B . 0.9700 ?
N14A H14A . 0.8900 ?
N14A H14B . 0.8900 ?
O11B C12B . 1.44(3) ?
O11B H11B . 0.819(10) ?
C12B C13B . 1.41(2) ?
C12B H12C . 0.9700 ?
C12B H12D . 0.9700 ?
C13B N14B . 1.563(12) ?
C13B H13C . 0.9700 ?
C13B H13D . 0.9700 ?
N14B H14C . 0.8900 ?
N14B H14D . 0.8900 ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N14B H14D O11B 4_566 0.89 2.20 3.09(3) 177.5 yes
O11B H11B N2C 3_655 0.819(10) 2.53(6) 3.30(3) 156(11) yes
