#------------------------------------------------------------------------------
#$Date: 2025-08-19 13:52:15 +0200 (Tue 19 de Aug de 2025) $
#$Revision: 301804 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/41/2214137.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_2214137
loop_
_publ_author_name
'Jiao, Rui'
'Wang, Li'
'Xu, Feng'
'Huang, Wei'
_publ_section_title
;A triclinic polymorph of
 bis(2,2'-bipyridine-κ²N,N')(dicyanamido-κN)copper(II)
 perchlorate
;
_journal_coeditor_code           CV2256
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1823
_journal_page_last               m1823
_journal_paper_doi               10.1107/S1600536807026876
_journal_volume                  63
_journal_year                    2007
_chemical_formula_iupac          '[Cu (C2 N3) (C10 H8 N2)2] Cl O4'
_chemical_formula_moiety         'C22 H16 Cu N7, Cl O4'
_chemical_formula_sum            'C22 H16 Cl Cu N7 O4'
_chemical_formula_weight         541.41
_chemical_name_systematic
;
bis(2,2'-bipyridine-κ²N,N')(dicyanamido-\kN)copper(II) perchlorate
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_cell_angle_alpha                79.953(4)
_cell_angle_beta                 78.131(3)
_cell_angle_gamma                67.468(3)
_cell_formula_units_Z            2
_cell_length_a                   7.6881(12)
_cell_length_b                   9.0059(14)
_cell_length_c                   17.737(3)
_cell_measurement_reflns_used    999
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20.061
_cell_measurement_theta_min      2.360
_cell_volume                     1103.9(3)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (Bruker, 2000)'
_computing_data_reduction        'SAINT (Bruker, 2000)'
_computing_molecular_graphics    SHELXTL
_computing_publication_material  SHELXTL
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Bruker, 2000)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker 1K CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0653
_diffrn_reflns_av_sigmaI/netI    0.1001
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5551
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  0.8930
_exptl_absorpt_correction_T_min  0.8365
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.629
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.646
_refine_diff_density_min         -0.380
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     317
_refine_ls_number_reflns         3839
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0689
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0664P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1532
_refine_ls_wR_factor_ref         0.1683
_reflns_number_gt                2781
_reflns_number_total             3839
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            cv2256.cif
_cod_data_source_block           I
_cod_database_code               2214137
_cod_database_fobs_code          2214137
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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_refinement_flags
_atom_site_occupancy
Cu Cu1 0.19003(9) 0.56335(8) 0.25165(4) 0.0435(3) Uani d . 1
C C1 0.3784(8) 0.6567(7) 0.3548(3) 0.0448(14) Uani d . 1
C C2 0.4336(10) 0.7407(9) 0.3973(3) 0.0578(17) Uani d . 1
H H2 0.5328 0.6874 0.4260 0.069 Uiso calc R 1
C C3 0.3381(11) 0.9058(10) 0.3964(4) 0.071(2) Uani d . 1
H H3 0.3694 0.9651 0.4259 0.085 Uiso calc R 1
C C4 0.1994(11) 0.9799(9) 0.3522(4) 0.070(2) Uani d . 1
H H4 0.1364 1.0913 0.3503 0.084 Uiso calc R 1
C C5 0.1504(9) 0.8919(8) 0.3100(4) 0.0582(17) Uani d . 1
H H5 0.0536 0.9448 0.2801 0.070 Uiso calc R 1
C C6 0.4731(7) 0.4797(7) 0.3503(3) 0.0439(14) Uani d . 1
C C7 0.6032(8) 0.3794(9) 0.3970(3) 0.0582(17) Uani d . 1
H H7 0.6396 0.4219 0.4327 0.070 Uiso calc R 1
C C8 0.6785(9) 0.2178(9) 0.3909(4) 0.0660(19) Uani d . 1
H H8 0.7659 0.1494 0.4227 0.079 Uiso calc R 1
C C9 0.6260(8) 0.1568(8) 0.3387(4) 0.0591(17) Uani d . 1
H H9 0.6778 0.0467 0.3335 0.071 Uiso calc R 1
C C10 0.4953(9) 0.2600(7) 0.2937(3) 0.0553(16) Uani d . 1
H H10 0.4581 0.2182 0.2580 0.066 Uiso calc R 1
C C11 0.2155(8) 0.6974(6) 0.0944(3) 0.0424(13) Uani d . 1
C C12 0.2918(9) 0.7448(7) 0.0211(3) 0.0547(16) Uani d . 1
H H12 0.2116 0.8091 -0.0141 0.066 Uiso calc R 1
C C13 0.4845(10) 0.6975(8) 0.0002(4) 0.0653(19) Uani d . 1
H H13 0.5366 0.7294 -0.0492 0.078 Uiso calc R 1
C C14 0.5998(9) 0.6028(8) 0.0526(4) 0.0612(17) Uani d . 1
H H14 0.7316 0.5699 0.0396 0.073 Uiso calc R 1
C C15 0.5196(8) 0.5572(8) 0.1239(3) 0.0534(16) Uani d . 1
H H15 0.5991 0.4919 0.1592 0.064 Uiso calc R 1
C C16 0.0109(8) 0.7505(7) 0.1246(3) 0.0437(14) Uani d . 1
C C17 -0.1305(9) 0.8438(7) 0.0818(3) 0.0550(16) Uani d . 1
H H17 -0.1008 0.8732 0.0292 0.066 Uiso calc R 1
C C18 -0.3177(10) 0.8934(8) 0.1180(4) 0.0618(18) Uani d . 1
H H18 -0.4157 0.9558 0.0899 0.074 Uiso calc R 1
C C19 -0.3571(9) 0.8500(8) 0.1951(4) 0.0613(18) Uani d . 1
H H19 -0.4820 0.8847 0.2206 0.074 Uiso calc R 1
C C20 -0.2115(9) 0.7551(8) 0.2341(4) 0.0599(17) Uani d . 1
H H20 -0.2389 0.7246 0.2867 0.072 Uiso calc R 1
C C21 0.0205(8) 0.4107(8) 0.3986(4) 0.0504(14) Uani d U 1
C C22 0.1100(10) 0.2596(9) 0.5108(4) 0.0620(14) Uani d U 1
Cl Cl1 0.0782(2) 0.2387(2) 0.14516(10) 0.0672(5) Uani d . 1
N N1 0.2396(6) 0.7306(6) 0.3109(3) 0.0447(11) Uani d . 1
N N2 0.4187(6) 0.4198(6) 0.2993(3) 0.0446(11) Uani d . 1
N N3 0.3321(7) 0.6019(6) 0.1455(3) 0.0457(11) Uani d . 1
N N4 -0.0303(6) 0.7041(5) 0.1998(2) 0.0435(11) Uani d . 1
N N5 0.0378(7) 0.4750(6) 0.3393(3) 0.0571(14) Uani d . 1
N N6 -0.0215(8) 0.3402(7) 0.4665(3) 0.0688(13) Uani d U 1
N N7 0.2105(9) 0.1878(8) 0.5522(3) 0.0827(19) Uani d . 1
O O1 0.140(2) 0.0985(10) 0.1153(5) 0.238(6) Uani d . 1
O O2 0.0414(9) 0.3627(8) 0.0838(3) 0.127(2) Uani d . 1
O O3 -0.0722(9) 0.2517(12) 0.1995(5) 0.202(5) Uani d . 1
O O4 0.2253(10) 0.2385(12) 0.1770(4) 0.167(3) Uani d . 1
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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'
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_publ_flag
N4 Cu1 N5 95.2(2) ?
N4 Cu1 N2 177.48(18) y
N5 Cu1 N2 86.8(2) y
N4 Cu1 N3 81.29(18) y
N5 Cu1 N3 161.8(2) y
N2 Cu1 N3 96.32(19) y
N4 Cu1 N1 102.75(18) y
N5 Cu1 N1 98.96(19) y
N2 Cu1 N1 78.38(18) y
N3 Cu1 N1 99.24(18) y
N1 C1 C2 122.2(6) ?
N1 C1 C6 114.6(5) ?
C2 C1 C6 123.1(6) ?
C1 C2 C3 118.5(6) ?
C1 C2 H2 120.8 ?
C3 C2 H2 120.8 ?
C4 C3 C2 119.2(6) ?
C4 C3 H3 120.4 ?
C2 C3 H3 120.4 ?
C3 C4 C5 120.4(7) ?
C3 C4 H4 119.8 ?
C5 C4 H4 119.8 ?
N1 C5 C4 121.4(6) ?
N1 C5 H5 119.3 ?
C4 C5 H5 119.3 ?
N2 C6 C7 120.6(6) ?
N2 C6 C1 115.8(5) ?
C7 C6 C1 123.6(5) ?
C8 C7 C6 119.8(6) ?
C8 C7 H7 120.1 ?
C6 C7 H7 120.1 ?
C9 C8 C7 119.8(6) ?
C9 C8 H8 120.1 ?
C7 C8 H8 120.1 ?
C8 C9 C10 118.7(6) ?
C8 C9 H9 120.6 ?
C10 C9 H9 120.6 ?
N2 C10 C9 122.3(6) ?
N2 C10 H10 118.9 ?
C9 C10 H10 118.9 ?
N3 C11 C12 120.0(5) ?
N3 C11 C16 115.3(5) ?
C12 C11 C16 124.6(5) ?
C13 C12 C11 120.2(6) ?
C13 C12 H12 119.9 ?
C11 C12 H12 119.9 ?
C12 C13 C14 119.1(6) ?
C12 C13 H13 120.5 ?
C14 C13 H13 120.5 ?
C15 C14 C13 119.1(6) ?
C15 C14 H14 120.5 ?
C13 C14 H14 120.5 ?
N3 C15 C14 122.8(6) ?
N3 C15 H15 118.6 ?
C14 C15 H15 118.6 ?
N4 C16 C17 121.0(5) ?
N4 C16 C11 114.5(5) ?
C17 C16 C11 124.4(5) ?
C16 C17 C18 119.0(6) ?
C16 C17 H17 120.5 ?
C18 C17 H17 120.5 ?
C19 C18 C17 119.3(6) ?
C19 C18 H18 120.3 ?
C17 C18 H18 120.3 ?
C20 C19 C18 119.0(6) ?
C20 C19 H19 120.5 ?
C18 C19 H19 120.5 ?
N4 C20 C19 122.4(6) ?
N4 C20 H20 118.8 ?
C19 C20 H20 118.8 ?
N5 C21 N6 172.9(7) ?
N7 C22 N6 174.5(8) ?
O3 Cl1 O1 110.9(7) ?
O3 Cl1 O4 109.8(6) ?
O1 Cl1 O4 106.1(7) ?
O3 Cl1 O2 113.1(4) ?
O1 Cl1 O2 107.6(5) ?
O4 Cl1 O2 109.1(5) ?
C1 N1 C5 118.3(5) ?
C1 N1 Cu1 112.6(4) ?
C5 N1 Cu1 129.1(4) ?
C6 N2 C10 118.8(5) ?
C6 N2 Cu1 117.6(4) ?
C10 N2 Cu1 122.3(4) ?
C15 N3 C11 118.9(5) ?
C15 N3 Cu1 127.7(4) ?
C11 N3 Cu1 113.1(4) ?
C20 N4 C16 119.2(5) ?
C20 N4 Cu1 125.1(4) ?
C16 N4 Cu1 115.7(4) ?
C21 N5 Cu1 151.6(5) ?
C21 N6 C22 121.1(6) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Cu1 N4 1.978(4) y
Cu1 N5 1.988(5) y
Cu1 N2 1.991(4) y
Cu1 N3 2.019(5) y
Cu1 N1 2.163(5) y
C1 N1 1.343(7) ?
C1 C2 1.377(8) ?
C1 C6 1.486(8) ?
C2 C3 1.383(9) ?
C2 H2 0.9300 ?
C3 C4 1.346(9) ?
C3 H3 0.9300 ?
C4 C5 1.372(9) ?
C4 H4 0.9300 ?
C5 N1 1.346(7) ?
C5 H5 0.9300 ?
C6 N2 1.336(7) ?
C6 C7 1.375(7) ?
C7 C8 1.359(9) ?
C7 H7 0.9300 ?
C8 C9 1.350(9) ?
C8 H8 0.9300 ?
C9 C10 1.366(8) ?
C9 H9 0.9300 ?
C10 N2 1.343(7) ?
C10 H10 0.9300 ?
C11 N3 1.355(7) ?
C11 C12 1.378(7) ?
C11 C16 1.469(7) ?
C12 C13 1.364(8) ?
C12 H12 0.9300 ?
C13 C14 1.364(9) ?
C13 H13 0.9300 ?
C14 C15 1.357(8) ?
C14 H14 0.9300 ?
C15 N3 1.329(7) ?
C15 H15 0.9300 ?
C16 N4 1.336(6) ?
C16 C17 1.372(7) ?
C17 C18 1.382(9) ?
C17 H17 0.9300 ?
C18 C19 1.359(8) ?
C18 H18 0.9300 ?
C19 C20 1.358(8) ?
C19 H19 0.9300 ?
C20 N4 1.334(7) ?
C20 H20 0.9300 ?
C21 N5 1.117(7) ?
C21 N6 1.299(7) ?
C22 N7 1.112(7) ?
C22 N6 1.317(8) ?
Cl1 O3 1.325(6) ?
Cl1 O1 1.331(8) ?
Cl1 O4 1.364(6) ?
Cl1 O2 1.405(6) ?
loop_
_cod_related_entry_id
_cod_related_entry_database
_cod_related_entry_code
1 PubChem 139058674
