#------------------------------------------------------------------------------
#$Date: 2019-11-07 22:12:49 +0200 (Thu, 07 Nov 2019) $
#$Revision: 223731 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/23/23/7232348.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_7232348
loop_
_publ_author_name
'Ishikawa, Ryuta'
'Ueno, Shunya'
'Hamatake, Yumi'
'Horii, Yoji'
'Miyazaki, Yuji'
'Nakano, Motohiro'
'Noda, Takeshi'
'Uematsu, Mikoto'
'Kawata, Satoshi'
_publ_section_title
;
 Versatile coordination architectures of products generated by the in situ
 reaction of a doubly bis(2-pyridyl)pyrazolate bridged dinuclear
 copper(ii) complex with tetracyanoethylene
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              1886
_journal_paper_doi               10.1039/C9CE00036D
_journal_volume                  21
_journal_year                    2019
_chemical_formula_moiety         'C38 H28 Cu2 N12 O4'
_chemical_formula_sum            'C38 H28 Cu2 N12 O4'
_chemical_formula_weight         843.81
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_update_record
;
2018-12-22 deposited with the CCDC.    2019-02-13 downloaded from the CCDC.
;
_cell_angle_alpha                108.3940(19)
_cell_angle_beta                 95.407(2)
_cell_angle_gamma                108.6530(14)
_cell_formula_units_Z            1
_cell_length_a                   8.1083(5)
_cell_length_b                   10.3884(6)
_cell_length_c                   11.9430(8)
_cell_measurement_reflns_used    7270
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.54
_cell_measurement_theta_min      3.23
_cell_volume                     882.88(10)
_computing_cell_refinement       'RAPID AUTO'
_computing_data_collection       'RAPID AUTO (Rigaku, ????)'
_computing_data_reduction        'RAPID AUTO'
_computing_molecular_graphics    'CrystalStructure 4.0'
_computing_publication_material  'CrystalStructure 4.0 (Rigaku, 2010)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'Il Milione (Burla, et al., 2007)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 10.000
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID'
_diffrn_measurement_method       ω
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0270
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            8849
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.266
_exptl_absorpt_correction_T_max  0.881
_exptl_absorpt_correction_T_min  0.718
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.587
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             430.00
_exptl_crystal_preparation       'Magnetic properties'
_exptl_crystal_recrystallization_method
'Liquid-liquid slow diffusion technique'
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.400
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_number_parameters     254
_refine_ls_number_reflns         4047
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[σ²(Fo²)+(0.0278P)²+0.8604P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0826
_reflns_number_gt                3372
_reflns_number_total             4047
_reflns_threshold_expression     F²>2.0σ(F²)
_cod_data_source_file            c9ce00036d2.cif
_cod_data_source_block           Cu2_bpypz2_DCNE2
_cod_depositor_comments
'Adding full bibliography for 7232348--7232350.cif.'
_cod_original_cell_volume        882.89(9)
_cod_database_code               7232348
loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 +X,+Y,+Z
2 -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
Cu1 Cu 1.10939(4) 0.61213(3) 0.17751(2) 0.01795(9) Uani 1.0 2 d .
O1 O 1.0116(2) 1.11445(18) 0.15972(15) 0.0239(4) Uani 1.0 2 d .
O2 O 1.2575(3) 1.32116(18) 0.22522(16) 0.0264(4) Uani 1.0 2 d .
N1 N 0.9767(3) 0.5994(2) 0.31597(17) 0.0202(4) Uani 1.0 2 d .
N2 N 0.8659(3) 0.4927(2) 0.08376(17) 0.0178(4) Uani 1.0 2 d .
N3 N 0.7914(3) 0.4249(2) -0.03395(16) 0.0181(4) Uani 1.0 2 d .
N4 N 0.6155(3) 0.2794(2) -0.25533(17) 0.0196(4) Uani 1.0 2 d .
N5 N 1.1076(3) 0.8359(3) 0.2086(2) 0.0265(5) Uani 1.0 2 d .
N6 N 1.6007(3) 1.2127(3) 0.3542(2) 0.0350(6) Uani 1.0 2 d .
C1 C 1.0418(4) 0.6559(3) 0.4352(3) 0.0298(6) Uani 1.0 2 d .
C2 C 0.9356(4) 0.6593(3) 0.5192(3) 0.0342(7) Uani 1.0 2 d .
C3 C 0.7525(4) 0.6000(3) 0.4793(3) 0.0275(6) Uani 1.0 2 d .
C4 C 0.6815(3) 0.5376(3) 0.3562(2) 0.0225(5) Uani 1.0 2 d .
C5 C 0.7959(3) 0.5391(3) 0.2771(2) 0.0178(5) Uani 1.0 2 d .
C6 C 0.7351(3) 0.4740(3) 0.1462(2) 0.0172(5) Uani 1.0 2 d .
C7 C 0.5711(3) 0.3908(3) 0.0664(2) 0.0188(5) Uani 1.0 2 d .
C8 C 0.6137(3) 0.3630(3) -0.0468(2) 0.0171(5) Uani 1.0 2 d .
C9 C 0.5140(3) 0.2780(3) -0.1710(2) 0.0181(5) Uani 1.0 2 d .
C10 C 0.3317(3) 0.1982(3) -0.2017(3) 0.0239(5) Uani 1.0 2 d .
C11 C 0.2503(4) 0.1144(3) -0.3214(3) 0.0277(6) Uani 1.0 2 d .
C12 C 0.3528(4) 0.1138(3) -0.4079(3) 0.0277(6) Uani 1.0 2 d .
C13 C 0.5338(4) 0.1977(3) -0.3710(3) 0.0261(6) Uani 1.0 2 d .
C14 C 1.1788(3) 0.9582(3) 0.2262(2) 0.0214(5) Uani 1.0 2 d .
C15 C 1.4535(4) 1.1675(3) 0.3075(3) 0.0229(5) Uani 1.0 2 d .
C16 C 1.2697(3) 1.1076(3) 0.2506(2) 0.0201(5) Uani 1.0 2 d .
C17 C 1.1858(3) 1.1931(3) 0.2124(2) 0.0198(5) Uani 1.0 2 d .
C18 C 0.9153(4) 1.1892(3) 0.1131(3) 0.0304(6) Uani 1.0 2 d .
C19 C 0.7253(4) 1.0856(3) 0.0648(3) 0.0301(6) Uani 1.0 2 d .
H1 H 1.1675 0.6957 0.4638 0.0358 Uiso 1.0 2 calc R
H2 H 0.9878 0.7019 0.6033 0.0411 Uiso 1.0 2 calc R
H3 H 0.6767 0.6021 0.5353 0.0330 Uiso 1.0 2 calc R
H4 H 0.5560 0.4943 0.3264 0.0270 Uiso 1.0 2 calc R
H7 H 0.4568 0.3602 0.0848 0.0225 Uiso 1.0 2 calc R
H10 H 0.2638 0.2012 -0.1410 0.0286 Uiso 1.0 2 calc R
H11 H 0.1260 0.0582 -0.3440 0.0333 Uiso 1.0 2 calc R
H12 H 0.3001 0.0569 -0.4908 0.0332 Uiso 1.0 2 calc R
H13 H 0.6033 0.1972 -0.4308 0.0313 Uiso 1.0 2 calc R
H18A H 0.9665 1.2163 0.0481 0.0365 Uiso 1.0 2 calc R
H18B H 0.9227 1.2792 0.1783 0.0365 Uiso 1.0 2 calc R
H19A H 0.6753 1.0619 0.1306 0.0361 Uiso 1.0 2 calc R
H19B H 0.7202 0.9960 0.0020 0.0361 Uiso 1.0 2 calc R
H19C H 0.6560 1.1313 0.0302 0.0361 Uiso 1.0 2 calc R
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 for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
N N 0.0061 0.0033
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
C C 0.0033 0.0016
;
International Tables for Crystallography
(1992, Vol. C, Tables 4.2.6.8 and 6.1.1.4)
;
H H 0.0000 0.0000
;
International Tables for Crystallography
(1992, Vol. C, Table 6.1.1.4)
;
O O 0.0106 0.0060
;
International Tables for Crystallography
(1992, 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_publ_flag
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Cu1 N2 79.75(8) yes . .
N1 Cu1 N3 166.72(8) yes . 2_765
N1 Cu1 N4 107.75(8) yes . 2_765
N1 Cu1 N5 90.46(9) yes . .
N2 Cu1 N3 92.35(8) yes . 2_765
N2 Cu1 N4 170.81(9) yes . 2_765
N2 Cu1 N5 100.17(9) yes . .
N3 Cu1 N4 79.26(8) yes 2_765 2_765
N3 Cu1 N5 101.52(10) yes 2_765 .
N4 Cu1 N5 85.31(9) yes 2_765 .
C17 O1 C18 115.9(2) yes . .
Cu1 N1 C1 129.23(17) yes . .
Cu1 N1 C5 113.01(16) yes . .
C1 N1 C5 117.3(3) yes . .
Cu1 N2 N3 134.51(16) yes . .
Cu1 N2 C6 117.13(14) yes . .
N3 N2 C6 108.32(17) yes . .
Cu1 N3 N2 132.77(15) yes 2_765 .
Cu1 N3 C8 118.45(14) yes 2_765 .
N2 N3 C8 108.50(19) yes . .
Cu1 N4 C9 112.62(14) yes 2_765 .
Cu1 N4 C13 129.16(18) yes 2_765 .
C9 N4 C13 117.47(19) yes . .
Cu1 N5 C14 151.7(3) yes . .
N1 C1 C2 123.4(3) yes . .
N1 C1 H1 118.4 yes . .
C2 C1 H1 118.3 yes . .
C1 C2 C3 119.0(3) yes . .
C2 C3 C4 118.8(3) yes . .
C3 C4 C5 119.1(3) yes . .
C3 C2 H2 120.4 yes . .
C1 C2 H2 120.5 yes . .
C2 C3 H3 120.7 yes . .
C4 C3 H3 120.6 yes . .
C5 C4 H4 120.5 yes . .
C5 C4 H4 120.5 yes . .
C3 C4 H4 120.4 yes . .
C8 C7 H7 128.2 yes . .
C6 C7 H7 128.1 yes . .
C9 C10 H10 120.3 yes . .
C11 C10 H10 120.4 yes . .
C11 C10 H10 120.4 yes . .
C10 C11 H11 120.5 yes . .
C10 C11 H11 120.5 yes . .
C12 C11 H11 120.6 yes . .
C11 C12 H12 120.6 yes . .
C13 C12 H12 120.7 yes . .
N1 C5 C4 122.4(2) yes . .
N1 C5 C6 114.1(2) yes . .
C4 C5 C6 123.4(2) yes . .
N2 C6 C5 114.95(18) yes . .
N2 C6 C7 109.7(2) yes . .
C5 C6 C7 135.3(3) yes . .
C6 C7 C8 103.7(2) yes . .
N3 C8 C7 109.72(18) yes . .
N3 C8 C9 115.0(2) yes . .
C7 C8 C9 135.1(2) yes . .
N4 C9 C8 114.30(18) yes . .
N4 C9 C10 122.27(19) yes . .
C8 C9 C10 123.4(3) yes . .
C9 C10 C11 119.3(3) yes . .
C10 C11 C12 118.9(2) yes . .
C11 C12 C13 118.7(3) yes . .
N4 C13 C12 123.3(3) yes . .
N5 C14 C16 178.3(3) yes . .
N6 C15 C16 178.2(4) yes . .
N4 C13 H13 118.4 yes . .
C12 C13 H13 118.3 yes . .
C14 C16 C15 116.7(3) yes . .
C14 C16 C17 122.0(2) yes . .
C15 C16 C17 121.2(3) yes . .
O1 C17 O2 122.7(3) yes . .
O1 C17 C16 111.3(2) yes . .
O2 C17 C16 125.9(2) yes . .
O1 C18 C19 106.9(3) yes . .
N4 C13 H13 118.4 yes . .
O1 C18 H18A 110.3 yes . .
O1 C18 H18B 110.3 yes . .
C19 C18 H18A 110.4 yes . .
C19 C18 H18B 110.3 yes . .
H18A C18 H18B 108.6 yes . .
C18 C19 H19A 109.5 yes . .
C18 C19 H19B 109.5 yes . .
C18 C19 H19B 109.4 yes . .
H19A C19 H19B 109.5 yes . .
H19A C19 H19C 109.5 yes . .
H19B C19 H19C 109.5 yes . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
_geom_bond_site_symmetry_2
Cu1 N1 2.072(3) yes .
Cu1 N2 1.9575(17) yes .
Cu1 N3 1.943(2) yes 2_765
Cu1 N4 2.1095(18) yes 2_765
Cu1 N5 2.241(3) yes .
O1 C17 1.352(3) yes .
O1 C18 1.450(4) yes .
O2 C17 1.221(3) yes .
N1 C1 1.336(3) yes .
N1 C5 1.363(3) yes .
N2 N3 1.334(3) yes .
N2 C6 1.352(4) yes .
N3 C8 1.348(3) yes .
N4 C9 1.360(4) yes .
N4 C13 1.340(3) yes .
N5 C14 1.153(4) yes .
N6 C15 1.143(4) yes .
C1 C2 1.382(5) yes .
C1 H1 0.9500 yes .
C2 C3 1.381(4) yes .
C2 H2 0.9500 yes .
C3 C4 1.383(4) yes .
C3 H3 0.9500 yes .
C4 C5 1.386(4) yes .
C4 H4 0.9500 yes .
C5 C6 1.455(3) yes .
C6 C7 1.389(3) yes .
C7 C8 1.391(4) yes .
C7 H7 0.9500 yes .
C8 C9 1.458(3) yes .
C9 C10 1.389(3) yes .
C10 C11 1.380(4) yes .
C10 H10 0.9500 yes .
C11 C12 1.385(4) yes .
C11 H11 0.9500 yes .
C12 C13 1.388(4) yes .
C12 H12 0.9500 yes .
C13 H13 0.9500 yes .
C14 C16 1.407(4) yes .
C15 C16 1.421(4) yes .
C16 C17 1.429(5) yes .
C18 C19 1.498(4) yes .
C18 H18A 0.9800 yes .
C18 H18B 0.9800 yes .
C19 H19A 0.9800 yes .
C19 H19B 0.9800 yes .
C19 H19C 0.9800 yes .
