#------------------------------------------------------------------------------
#$Date: 2024-05-04 03:49:46 +0200 (Sat 04 de May de 2024) $
#$Revision: 291489 $
#$URL: svn://www.crystallography.net/cod/cif/2/31/24/2312479.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_2312479
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 (C3 H9 N1 O1)2]'
_chemical_formula_moiety         'C10 H18 Cu3 N6 O2'
_chemical_formula_sum            'C10 H18 Cu3 N6 O2'
_chemical_formula_weight         444.94
_chemical_name_systematic
;
Poly[bis(2-aminopropanol)tetra-μ-cyanido-tricopper(I,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                 112.134(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.3903(4)
_cell_length_b                   8.9608(4)
_cell_length_c                   9.7986(4)
_cell_measurement_reflns_used    1863
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     763.74(6)
_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  0.084
_diffrn_reflns_av_unetI/netI     0.074
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19192
_diffrn_reflns_theta_full        25.016
_diffrn_reflns_theta_max         25.016
_diffrn_reflns_theta_min         2.341
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    4.150
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.75
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
(Otwinowski & Minor,1997)
;
_exptl_crystal_density_diffrn    1.935
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             446
_exptl_crystal_size_max          0.150
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.836
_refine_diff_density_min         -0.480
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1350
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.144
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0335
_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)+(0.0480P)²+1.2000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0813
_refine_ls_wR_factor_ref         0.1133
_reflns_number_gt                855
_reflns_number_total             1350
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            dg3052.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2312479
_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   0.575
_shelx_estimated_absorpt_t_max   0.922
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 0.45669(8) -0.02366(8) -0.14833(8) 0.0433(3) Uani d 1 . .
Cu Cu2 0.000000 0.000000 0.000000 0.0405(3) Uani d 1 . .
C C1 0.2964(7) -0.0113(5) -0.0678(6) 0.0394(13) Uani d 1 . .
N N1 0.1857(6) -0.0090(5) -0.0474(5) 0.0416(11) Uani d 1 . .
C C2 0.4991(6) 0.2789(6) -0.2877(6) 0.0482(14) Uani d 0.5 . .
N N2 0.4823(6) 0.1628(6) -0.2454(6) 0.0425(13) Uani d 0.5 . .
N C2N 0.4991(6) 0.2789(6) -0.2877(6) 0.0482(14) Uani d 0.5 . .
C N2C 0.4823(6) 0.1628(6) -0.2454(6) 0.0425(13) Uani d 0.5 . .
O O11A 0.121(10) 0.212(11) 0.196(7) 0.055(9) Uani d 0.537(8) A 1
H H11A 0.190(14) 0.272(13) 0.207(16) 0.065 Uiso d 0.537(8) A 1
C C12A 0.222(2) 0.126(2) 0.325(2) 0.053(3) Uani d 0.463(8) A 1
H H12A 0.315574 0.094938 0.312100 0.080 Uiso calc 0.463(8) A 1
H H12B 0.248953 0.182727 0.415081 0.080 Uiso calc 0.463(8) A 1
C C13A 0.1207(13) -0.0068(11) 0.3227(11) 0.0373(19) Uani d 0.537(8) A 1
H H13A 0.017617 0.026093 0.312321 0.056 Uiso calc 0.537(8) A 1
N N14A 0.1135(5) -0.1060(5) 0.1972(5) 0.0448(12) Uani d 0.537(8) A 1
H H14A 0.064638 -0.190114 0.200746 0.067 Uiso calc 0.537(8) A 1
H H14B 0.208310 -0.129292 0.204899 0.067 Uiso calc 0.537(8) A 1
C C15A 0.199(3) -0.092(4) 0.467(4) 0.075(7) Uani d 0.537(8) A 1
H H15A 0.204104 -0.029338 0.548490 0.113 Uiso calc 0.537(8) A 1
H H15B 0.140548 -0.180008 0.466991 0.113 Uiso calc 0.537(8) A 1
H H15C 0.300891 -0.119842 0.476832 0.113 Uiso calc 0.537(8) A 1
O O11B 0.132(12) 0.213(13) 0.175(8) 0.055(9) Uani d 0.463(8) A 2
H H11B 0.211(14) 0.232(17) 0.162(16) 0.065 Uiso d 0.463(8) A 2
C C12B 0.1572(18) 0.137(2) 0.316(2) 0.053(3) Uani d 0.537(8) A 2
H H12C 0.060844 0.130492 0.330578 0.080 Uiso calc 0.537(8) A 2
H H12D 0.228706 0.194823 0.396615 0.080 Uiso calc 0.537(8) A 2
C C13B 0.2200(15) -0.0148(12) 0.3157(13) 0.0373(19) Uani d 0.463(8) A 2
H H13B 0.312585 -0.002539 0.293205 0.056 Uiso calc 0.463(8) A 2
N N14B 0.1135(5) -0.1060(5) 0.1972(5) 0.0448(12) Uani d 0.463(8) A 2
H H14C 0.043546 -0.143775 0.228563 0.067 Uiso calc 0.463(8) A 2
H H14D 0.165766 -0.182183 0.180980 0.067 Uiso calc 0.463(8) A 2
C C15B 0.271(3) -0.088(4) 0.464(5) 0.075(7) Uani d 0.463(8) A 2
H H15D 0.310254 -0.185476 0.458921 0.113 Uiso calc 0.463(8) A 2
H H15E 0.349447 -0.028548 0.534644 0.113 Uiso calc 0.463(8) A 2
H H15F 0.184552 -0.096094 0.493930 0.113 Uiso calc 0.463(8) 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 C2 . 4_655 117.8(2) ?
C1 Cu1 N2 . . 113.5(2) ?
C2 Cu1 N2 4_655 . 121.7(2) ?
C1 Cu1 C1 . 3_655 105.1(2) ?
C2 Cu1 C1 4_655 3_655 98.19(19) ?
N2 Cu1 C1 . 3_655 93.39(19) ?
C1 Cu1 Cu1 . 3_655 61.80(18) ?
C2 Cu1 Cu1 4_655 3_655 117.51(16) ?
N2 Cu1 Cu1 . 3_655 109.72(16) ?
C1 Cu1 Cu1 3_655 3_655 43.34(13) ?
N1 Cu2 N1 3 . 180.0(2) ?
N1 Cu2 N14A 3 3 90.66(18) ?
N1 Cu2 N14A . 3 89.34(18) ?
N1 Cu2 N14B 3 . 89.34(18) ?
N1 Cu2 N14B . . 90.66(18) ?
N1 Cu2 N14A 3 . 89.34(18) ?
N1 Cu2 N14A . . 90.66(18) ?
N14A Cu2 N14A 3 . 180.0 ?
N1 Cu2 O11A 3 . 89(2) ?
N1 Cu2 O11A . . 91(2) ?
N14A Cu2 O11A 3 . 106.4(8) ?
N14A Cu2 O11A . . 73.6(8) ?
N1 Cu2 O11B 3 . 93(3) ?
N1 Cu2 O11B . . 87(3) ?
N14B Cu2 O11B . . 76.5(8) ?
N1 C1 Cu1 . . 167.2(6) ?
N1 C1 Cu1 . 3_655 118.0(5) ?
Cu1 C1 Cu1 . 3_655 74.9(2) ?
C1 N1 Cu2 . . 176.5(5) ?
N2 C2 Cu1 . 4_665 176.0(5) ?
C2 N2 Cu1 . . 172.6(5) ?
C12A O11A Cu2 . . 102(5) ?
C12A O11A H11A . . 91(10) ?
Cu2 O11A H11A . . 132(10) ?
C13A C12A O11A . . 101(4) ?
C13A C12A H12A . . 111.5 ?
O11A C12A H12A . . 111.5 ?
C13A C12A H12B . . 111.5 ?
O11A C12A H12B . . 111.5 ?
H12A C12A H12B . . 109.3 ?
N14A C13A C12A . . 108.0(10) ?
N14A C13A C15A . . 108.8(14) ?
C12A C13A C15A . . 107.4(14) ?
N14A C13A H13A . . 110.9 ?
C12A C13A H13A . . 110.9 ?
C15A C13A H13A . . 110.9 ?
C13A N14A Cu2 . . 110.2(5) ?
C13A N14A H14A . . 109.6 ?
Cu2 N14A H14A . . 109.6 ?
C13A N14A H14B . . 109.6 ?
Cu2 N14A H14B . . 109.6 ?
H14A N14A H14B . . 108.1 ?
C13A C15A H15A . . 109.5 ?
C13A C15A H15B . . 109.5 ?
H15A C15A H15B . . 109.5 ?
C13A C15A H15C . . 109.5 ?
H15A C15A H15C . . 109.5 ?
H15B C15A H15C . . 109.5 ?
C12B O11B Cu2 . . 99(6) ?
C12B O11B H11B . . 114(10) ?
Cu2 O11B H11B . . 106(10) ?
O11B C12B C13B . . 110(5) ?
O11B C12B H12C . . 109.6 ?
C13B C12B H12C . . 109.6 ?
O11B C12B H12D . . 109.6 ?
C13B C12B H12D . . 109.6 ?
H12C C12B H12D . . 108.1 ?
C15B C13B C12B . . 112.3(18) ?
C15B C13B N14B . . 113.5(16) ?
C12B C13B N14B . . 111.1(10) ?
C15B C13B H13B . . 106.5 ?
C12B C13B H13B . . 106.5 ?
N14B C13B H13B . . 106.5 ?
C13B N14B Cu2 . . 116.5(5) ?
C13B N14B H14C . . 108.2 ?
Cu2 N14B H14C . . 108.2 ?
C13B N14B H14D . . 108.2 ?
Cu2 N14B H14D . . 108.2 ?
H14C N14B H14D . . 107.3 ?
C13B C15B H15D . . 109.5 ?
C13B C15B H15E . . 109.5 ?
H15D C15B H15E . . 109.5 ?
C13B C15B H15F . . 109.5 ?
H15D C15B H15F . . 109.5 ?
H15E C15B H15F . . 109.5 ?
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 . 1.948(6) ?
Cu1 C2 4_655 1.973(5) ?
Cu1 N2 . 1.982(5) ?
Cu1 C1 3_655 2.502(6) ?
Cu1 Cu1 3_655 2.7403(14) ?
Cu2 N1 . 1.969(5) ?
Cu2 N14B . 2.054(5) ?
Cu2 N14A . 2.054(5) ?
Cu2 O11A . 2.64(11) ?
Cu2 O11B . 2.56(13) ?
C1 N1 . 1.130(8) ?
C2 N2 . 1.152(7) ?
O11A C12A . 1.47(3) ?
O11A H11A . 0.82(2) ?
C12A C13A . 1.52(2) ?
C12A H12A . 0.9700 ?
C12A H12B . 0.9700 ?
C13A N14A . 1.497(10) ?
C13A C15A . 1.53(4) ?
C13A H13A . 0.9800 ?
N14A H14A . 0.8900 ?
N14A H14B . 0.8900 ?
C15A H15A . 0.9600 ?
C15A H15B . 0.9600 ?
C15A H15C . 0.9600 ?
O11B C12B . 1.47(3) ?
O11B H11B . 0.82(2) ?
C12B C13B . 1.49(2) ?
C12B H12C . 0.9700 ?
C12B H12D . 0.9700 ?
C13B C15B . 1.50(4) ?
C13B N14B . 1.463(13) ?
C13B H13B . 0.9800 ?
N14B H14C . 0.8900 ?
N14B H14D . 0.8900 ?
C15B H15D . 0.9600 ?
C15B H15E . 0.9600 ?
C15B H15F . 0.9600 ?
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
N14A H14A O11A 4_556 0.89 2.48 3.21(11) 140.1 yes
O11B H11B N2 2 0.82(2) 2.54(13) 3.28(11) 150(13) yes
C12A H12A C2N 2 0.97 2.54 3.29(2) 134.1 yes
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
Cu2 O11A C12A C13A . . . . -42(4) ?
O11A C12A C13A N14A . . . . 73(4) ?
O11A C12A C13A C15A . . . . -169(5) ?
C12A C13A N14A Cu2 . . . . -66.5(10) ?
C15A C13A N14A Cu2 . . . . 177.3(10) ?
Cu2 O11B C12B C13B . . . . 46(5) ?
O11B C12B C13B C15B . . . . 171(5) ?
O11B C12B C13B N14B . . . . -61(5) ?
C15B C13B N14B Cu2 . . . . 166.7(14) ?
C12B C13B N14B Cu2 . . . . 39.0(12) ?
