#------------------------------------------------------------------------------
#$Date: 2020-12-06 23:26:35 +0200 (Sun, 06 Dec 2020) $
#$Revision: 259632 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/97/1559712.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_1559712
loop_
_publ_author_name
'Corfield, Peter W. R.'
'Dayrit, Joseph R.'
_publ_section_title
;
 Poly[1,3-Dimethyltetrahydropyrimidin-2(1H)-iminium
 [tri-µ2-cyanido-κ6C:N-dicuprate(I)]]
;
_journal_issue                   4
_journal_name_full               Molbank
_journal_page_first              M1170
_journal_paper_doi               10.3390/M1170
_journal_volume                  2020
_journal_year                    2020
_chemical_formula_moiety         'Cu2 C3 N3, C6 H14 N3'
_chemical_formula_sum            'C9 H14 Cu2 N6'
_chemical_formula_weight         333.34
_chemical_name_systematic
;
poly[1,3-dimethyltetrahydropyrimidin-2(1H)-iminium
[tri-μ₂-cyanido-κ⁶ C:N-dicuprate(I)]]
;
_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   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2017/1
_cell_angle_alpha                90
_cell_angle_beta                 108.570(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.5598(14)
_cell_length_b                   14.825(4)
_cell_length_c                   10.853(2)
_cell_measurement_reflns_used    3008
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     1305.5(5)
_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
'   ORTEP III (Burnett & Johnson, 1996);  Farrugia, 2012     '
_computing_publication_material  'publCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2015)'
_diffrn_ambient_temperature      300(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.987
_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  0.0312
_diffrn_reflns_av_unetI/netI     0.0352
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            3190
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         27.673
_diffrn_reflns_theta_min         2.410
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.249
_exptl_absorpt_correction_T_max  .6
_exptl_absorpt_correction_T_min  .4
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   '(Otwinowski & Minor,1997)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.698
_exptl_crystal_density_meas      1.692(8)
_exptl_crystal_density_method
;
flotation in mixtures of 1,2-dibromethane and 1,2,3-trichloropropane
;
_exptl_crystal_description       block
_exptl_crystal_F_000             672
_exptl_crystal_preparation       'mounted on glass fibre in air'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.371
_refine_diff_density_min         -0.295
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     178
_refine_ls_number_reflns         3009
_refine_ls_number_restraints     48
_refine_ls_restrained_S_all      1.075
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0470P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0893
_refine_ls_wR_factor_ref         0.0932
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2120
_reflns_number_total             3009
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            s5.cif
_cod_data_source_block           ajdmpdav4
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               1559712
_shelx_shelxl_version_number     2017/1
_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   0.563
_shelx_estimated_absorpt_t_max   0.624
_publcif_funding_html
;
;
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_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 0.73308(4) 0.89970(3) 0.20386(3) 0.06187(15) Uani 1 1 d . . . . .
Cu2 Cu 0.77580(4) 0.57251(3) 0.31676(3) 0.06149(15) Uani 1 1 d . . . . .
C1 C 0.4646(3) 0.46669(17) 0.3102(2) 0.0610(6) Uani 0.5 1 d . . P . .
N1A N 0.4646(3) 0.46669(17) 0.3102(2) 0.0610(6) Uani 0.5 1 d . . P . .
N1 N 0.5833(3) 0.50636(16) 0.3195(2) 0.0578(6) Uani 0.5 1 d . . P . .
C1A C 0.5833(3) 0.50636(16) 0.3195(2) 0.0578(6) Uani 0.5 1 d . . P . .
C2 C 1.0279(3) 1.00418(16) 0.1727(2) 0.0563(6) Uani 0.5 1 d . . P . .
N2A N 1.0279(3) 1.00418(16) 0.1727(2) 0.0563(6) Uani 0.5 1 d . . P . .
N2 N 0.9158(3) 0.96215(17) 0.1756(2) 0.0602(6) Uani 0.5 1 d . . P . .
C2A C 0.9158(3) 0.96215(17) 0.1756(2) 0.0602(6) Uani 0.5 1 d . . P . .
C3 C 0.7616(3) 0.6998(2) 0.2834(3) 0.0702(7) Uani 0.5 1 d . . P . .
N3A N 0.7616(3) 0.6998(2) 0.2834(3) 0.0702(7) Uani 0.5 1 d . . P . .
N3 N 0.7504(3) 0.7748(2) 0.2550(3) 0.0704(7) Uani 0.5 1 d . . P . .
C3A C 0.7504(3) 0.7748(2) 0.2550(3) 0.0704(7) Uani 0.5 1 d . . P . .
N10 N 0.8203(4) 0.33915(19) 0.4668(3) 0.0963(9) Uani 1 1 d . . . . .
H10A H 0.892705 0.348057 0.428428 0.145 Uiso 1 1 calc R U . . .
H10B H 0.773102 0.384325 0.489967 0.145 Uiso 1 1 calc R U . . .
N11 N 0.8575(3) 0.18874(17) 0.4526(2) 0.0617(6) Uani 1 1 d . . . . .
C12 C 0.7814(3) 0.25578(17) 0.4902(2) 0.0508(6) Uani 1 1 d . . . . .
N13 N 0.6698(3) 0.24101(19) 0.5465(2) 0.0737(7) Uani 1 1 d D . . . .
C14A C 0.6398(12) 0.1528(4) 0.5909(8) 0.087(2) Uani 0.650(14) 1 d D U P A 1
H14A H 0.528057 0.148687 0.594101 0.131 Uiso 0.650(14) 1 calc R U P A 1
H14B H 0.715764 0.140859 0.677058 0.131 Uiso 0.650(14) 1 calc R U P A 1
C15A C 0.6650(13) 0.0883(7) 0.4971(15) 0.106(4) Uani 0.650(14) 1 d D U P A 1
H15A H 0.650515 0.027616 0.525146 0.158 Uiso 0.650(14) 1 calc R U P A 1
H15B H 0.581783 0.098188 0.413444 0.158 Uiso 0.650(14) 1 calc R U P A 1
C14B C 0.5847(15) 0.1540(6) 0.5179(18) 0.100(3) Uani 0.350(14) 1 d D U P A 2
H14C H 0.511795 0.154633 0.428786 0.151 Uiso 0.350(14) 1 calc R U P A 2
H14D H 0.517051 0.146672 0.573938 0.151 Uiso 0.350(14) 1 calc R U P A 2
C15B C 0.695(3) 0.0765(11) 0.535(3) 0.105(5) Uani 0.350(14) 1 d D U P A 2
H15C H 0.741661 0.062723 0.627357 0.158 Uiso 0.350(14) 1 calc R U P A 2
H15D H 0.633780 0.024218 0.492285 0.158 Uiso 0.350(14) 1 calc R U P A 2
C16 C 0.8308(5) 0.0954(2) 0.4813(4) 0.0926(11) Uani 1 1 d D . . . .
H16A H 0.914780 0.076524 0.560472 0.139 Uiso 1 1 calc R U . A 1
H16B H 0.837050 0.056774 0.410906 0.139 Uiso 1 1 calc R U . A 1
C17 C 0.5936(5) 0.3146(3) 0.5947(4) 0.1215(16) Uani 1 1 d . . . . .
H17A H 0.675716 0.358740 0.635772 0.182 Uiso 1 1 calc R U . . .
H17B H 0.544742 0.291725 0.656694 0.182 Uiso 1 1 calc R U . . .
H17C H 0.509989 0.341947 0.523533 0.182 Uiso 1 1 calc R U . . .
C18 C 0.9840(4) 0.2049(3) 0.3909(3) 0.1096(14) Uani 1 1 d . . . . .
H18A H 0.937103 0.238221 0.311952 0.164 Uiso 1 1 calc R U . . .
H18B H 1.025001 0.148147 0.371544 0.164 Uiso 1 1 calc R U . . .
H18C H 1.072785 0.238766 0.448861 0.164 Uiso 1 1 calc R U . . .
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'
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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
N2 Cu1 N3 121.11(10) . . ?
N2 Cu1 C1 118.53(11) . 4_666 ?
N3 Cu1 C1 120.27(10) . 4_666 ?
N1 Cu2 C3 120.06(10) . . ?
N1 Cu2 C2 117.64(11) . 4_756 ?
C3 Cu2 C2 121.87(10) . 4_756 ?
N1 C1 Cu1 179.5(3) . 4_656 ?
C1 N1 Cu2 174.4(2) . . ?
N2 C2 Cu2 175.2(2) . 4_766 ?
C2 N2 Cu1 171.9(2) . . ?
N3 C3 Cu2 175.6(3) . . ?
C3 N3 Cu1 178.7(3) . . ?
C12 N10 H10A 120.0 . . ?
C12 N10 H10B 120.0 . . ?
H10A N10 H10B 120.0 . . ?
C12 N11 C18 121.9(3) . . ?
C12 N11 C16 121.6(2) . . ?
C18 N11 C16 116.3(3) . . ?
N11 C12 N13 121.6(3) . . ?
N11 C12 N10 117.6(3) . . ?
N13 C12 N10 120.8(3) . . ?
C12 N13 C14A 122.8(4) . . ?
C12 N13 C14B 115.9(7) . . ?
C12 N13 C17 121.5(3) . . ?
C14A N13 C17 114.4(3) . . ?
C14B N13 C17 119.2(7) . . ?
N13 C14A C15A 106.2(6) . . ?
N13 C14A H14A 110.5 . . ?
C15A C14A H14A 110.5 . . ?
N13 C14A H14B 110.5 . . ?
C15A C14A H14B 110.5 . . ?
H14A C14A H14B 108.7 . . ?
C16 C15A C14A 113.1(8) . . ?
C16 C15A H15A 109.0 . . ?
C14A C15A H15A 109.0 . . ?
C16 C15A H15B 109.0 . . ?
C14A C15A H15B 109.0 . . ?
H15A C15A H15B 107.8 . . ?
N13 C14B C15B 114.0(14) . . ?
N13 C14B H14C 108.8 . . ?
C15B C14B H14C 108.8 . . ?
N13 C14B H14D 108.8 . . ?
C15B C14B H14D 108.8 . . ?
H14C C14B H14D 107.7 . . ?
C16 C15B C14B 110.8(12) . . ?
C16 C15B H15C 109.5 . . ?
C14B C15B H15C 109.5 . . ?
C16 C15B H15D 109.5 . . ?
C14B C15B H15D 109.5 . . ?
H15C C15B H15D 108.1 . . ?
N11 C16 C15B 117.5(6) . . ?
N11 C16 C15A 108.3(5) . . ?
N11 C16 H16A 110.0 . . ?
C15A C16 H16A 110.0 . . ?
N11 C16 H16B 110.0 . . ?
C15A C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
N13 C17 H17A 109.5 . . ?
N13 C17 H17B 109.5 . . ?
H17A C17 H17B 109.5 . . ?
N13 C17 H17C 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
N11 C18 H18A 109.5 . . ?
N11 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
N11 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
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 N2 1.924(2) . ?
Cu1 N3 1.926(3) . ?
Cu1 C1 1.926(3) 4_666 ?
Cu2 N1 1.926(2) . ?
Cu2 C3 1.918(3) . ?
Cu2 C2 1.934(2) 4_756 ?
C1 N1 1.150(3) . ?
C2 N2 1.153(3) . ?
C3 N3 1.149(4) . ?
N10 C12 1.325(4) . ?
N10 H10A 0.8600 . ?
N10 H10B 0.8600 . ?
N11 C12 1.322(3) . ?
N11 C18 1.462(4) . ?
N11 C16 1.451(4) . ?
C12 N13 1.306(3) . ?
N13 C14A 1.445(5) . ?
N13 C14B 1.465(7) . ?
N13 C17 1.451(4) . ?
C14A C15A 1.462(10) . ?
C14A H14A 0.9700 . ?
C14A H14B 0.9700 . ?
C15A C16 1.486(7) . ?
C15A H15A 0.9700 . ?
C15A H15B 0.9700 . ?
C14B C15B 1.464(11) . ?
C14B H14C 0.9700 . ?
C14B H14D 0.9700 . ?
C15B C16 1.483(9) . ?
C15B H15C 0.9700 . ?
C15B H15D 0.9700 . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 H17A 0.9600 . ?
C17 H17B 0.9600 . ?
C17 H17C 0.9600 . ?
C18 H18A 0.9600 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
loop_
_publcif_info_cif.paper_type
?
