#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:25:48 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179969 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/63/7026334.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_7026334
loop_
_publ_author_name
'Xu, Feng'
'Huang, Wei'
'You, Xiao-Zeng'
_publ_section_title
;
 Novel cyano-bridged mixed-valent copper complexes formed by completely in
 situ synthetic method via the cleavage of C-C bond in acetonitrile.
;
_journal_issue                   44
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10652
_journal_page_last               10658
_journal_paper_doi               10.1039/c0dt00345j
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C21 H16 Cu N5, Cl O4'
_chemical_formula_sum            'C21 H16 Cl Cu N5 O4'
_chemical_formula_weight         501.38
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.524(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.304(3)
_cell_length_b                   11.451(2)
_cell_length_c                   14.804(3)
_cell_measurement_reflns_used    2259
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      21.266
_cell_measurement_theta_min      2.307
_cell_volume                     2112.1(7)
_computing_cell_refinement       SMART
_computing_data_collection       'SMART (BRUKER 2000)'
_computing_data_reduction        'SAINT (BRUKER 2000)'
_computing_molecular_graphics    'SHELXL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0583
_diffrn_reflns_av_sigmaI/netI    0.0596
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            10390
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.31
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.200
_exptl_absorpt_correction_T_max  0.8894
_exptl_absorpt_correction_T_min  0.8500
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, Bruker(2000)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.577
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1020
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.928
_refine_diff_density_min         -0.482
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.942
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     289
_refine_ls_number_reflns         3721
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.942
_refine_ls_R_factor_all          0.0973
_refine_ls_R_factor_gt           0.0637
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1212P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1747
_refine_ls_wR_factor_ref         0.1935
_reflns_number_gt                2247
_reflns_number_total             3721
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0dt00345j.txt
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7026334
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Cu1 Cu 0.76471(5) 0.47359(6) 0.00883(4) 0.0575(3) Uani 1 1 d .
C1 C 0.9098(5) 0.5498(5) 0.2151(4) 0.0758(17) Uani 1 1 d .
H1 H 0.8524 0.5952 0.2166 0.091 Uiso 1 1 calc R
C2 C 1.0021(6) 0.5463(6) 0.2952(5) 0.090(2) Uani 1 1 d .
H2 H 1.0058 0.5864 0.3509 0.108 Uiso 1 1 calc R
C3 C 1.0869(6) 0.4843(7) 0.2924(5) 0.091(2) Uani 1 1 d .
H3 H 1.1503 0.4841 0.3456 0.109 Uiso 1 1 calc R
C4 C 1.0807(5) 0.4222(6) 0.2127(5) 0.0804(18) Uani 1 1 d .
H4 H 1.1389 0.3784 0.2110 0.097 Uiso 1 1 calc R
C5 C 0.9852(4) 0.4252(5) 0.1329(4) 0.0600(13) Uani 1 1 d .
C6 C 0.9676(4) 0.3603(4) 0.0439(4) 0.0594(13) Uani 1 1 d .
C7 C 1.0458(5) 0.2931(5) 0.0290(5) 0.0764(17) Uani 1 1 d .
H7 H 1.1143 0.2890 0.0754 0.092 Uiso 1 1 calc R
C8 C 1.0204(6) 0.2318(6) -0.0565(6) 0.092(2) Uani 1 1 d .
H8 H 1.0709 0.1831 -0.0674 0.110 Uiso 1 1 calc R
C9 C 0.9220(6) 0.2430(5) -0.1241(5) 0.0848(19) Uani 1 1 d .
H9 H 0.9048 0.2040 -0.1827 0.102 Uiso 1 1 calc R
C10 C 0.8471(5) 0.3126(5) -0.1056(4) 0.0748(16) Uani 1 1 d .
H10 H 0.7792 0.3200 -0.1525 0.090 Uiso 1 1 calc R
C11 C 0.6956(4) 0.2301(5) 0.0640(4) 0.0701(15) Uani 1 1 d .
H11 H 0.7402 0.1976 0.0344 0.084 Uiso 1 1 calc R
C12 C 0.6419(5) 0.1572(5) 0.1050(5) 0.0799(17) Uani 1 1 d .
H12 H 0.6506 0.0767 0.1035 0.096 Uiso 1 1 calc R
C13 C 0.5752(5) 0.2042(6) 0.1484(4) 0.0788(17) Uani 1 1 d .
H13 H 0.5376 0.1560 0.1759 0.095 Uiso 1 1 calc R
C14 C 0.5650(4) 0.3225(5) 0.1505(4) 0.0665(14) Uani 1 1 d .
H14 H 0.5206 0.3562 0.1797 0.080 Uiso 1 1 calc R
C15 C 0.6219(4) 0.3916(4) 0.1083(3) 0.0507(12) Uani 1 1 d .
C16 C 0.6152(4) 0.5218(4) 0.1055(3) 0.0490(11) Uani 1 1 d .
C17 C 0.5547(4) 0.5865(5) 0.1459(4) 0.0643(14) Uani 1 1 d .
H17 H 0.5151 0.5489 0.1780 0.077 Uiso 1 1 calc R
C18 C 0.5523(5) 0.7064(5) 0.1392(4) 0.0741(16) Uani 1 1 d .
H18 H 0.5121 0.7506 0.1669 0.089 Uiso 1 1 calc R
C19 C 0.6115(5) 0.7592(5) 0.0902(4) 0.0763(16) Uani 1 1 d .
H19 H 0.6118 0.8400 0.0843 0.092 Uiso 1 1 calc R
C20 C 0.6701(5) 0.6909(5) 0.0502(4) 0.0710(15) Uani 1 1 d .
H20 H 0.7088 0.7266 0.0163 0.085 Uiso 1 1 calc R
C21 C 0.7035(5) 0.5337(5) -0.1232(5) 0.0659(15) Uani 1 1 d .
Cl1 Cl 0.73708(15) 0.52430(14) 0.40320(11) 0.0783(5) Uani 1 1 d .
N1 N 0.9005(3) 0.4895(4) 0.1351(3) 0.0577(11) Uani 1 1 d .
N2 N 0.8690(3) 0.3692(4) -0.0233(3) 0.0587(11) Uani 1 1 d .
N3 N 0.6860(3) 0.3457(3) 0.0651(3) 0.0536(10) Uani 1 1 d .
N4 N 0.6728(3) 0.5746(4) 0.0587(3) 0.0577(10) Uani 1 1 d .
N5 N 0.6626(4) 0.5588(5) -0.2054(5) 0.0852(15) Uani 1 1 d .
O1 O 0.6932(9) 0.4390(6) 0.3498(5) 0.261(6) Uani 1 1 d .
O2 O 0.7548(6) 0.6213(7) 0.3561(5) 0.207(4) Uani 1 1 d .
O3 O 0.8255(9) 0.4846(7) 0.4774(6) 0.227(5) Uani 1 1 d .
O4 O 0.6867(16) 0.5624(12) 0.4520(14) 0.389(11) Uani 1 1 d .
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'
H H 0.0000 0.0000 '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'
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C21 Cu1 N4 94.0(2)
C21 Cu1 N2 93.0(2)
N4 Cu1 N2 172.60(17)
C21 Cu1 N1 141.6(2)
N4 Cu1 N1 93.87(17)
N2 Cu1 N1 79.21(17)
C21 Cu1 N3 122.8(2)
N4 Cu1 N3 78.80(17)
N2 Cu1 N3 99.11(16)
N1 Cu1 N3 95.66(15)
N1 C1 C2 121.7(6)
N1 C1 H1 119.2
C2 C1 H1 119.2
C3 C2 C1 119.6(7)
C3 C2 H2 120.2
C1 C2 H2 120.2
C2 C3 C4 120.5(6)
C2 C3 H3 119.8
C4 C3 H3 119.8
C3 C4 C5 118.8(7)
C3 C4 H4 120.6
C5 C4 H4 120.6
N1 C5 C4 120.7(6)
N1 C5 C6 115.3(4)
C4 C5 C6 124.1(6)
N2 C6 C7 121.5(5)
N2 C6 C5 115.8(5)
C7 C6 C5 122.7(5)
C6 C7 C8 118.4(6)
C6 C7 H7 120.8
C8 C7 H7 120.8
C9 C8 C7 119.6(6)
C9 C8 H8 120.2
C7 C8 H8 120.2
C8 C9 C10 119.4(6)
C8 C9 H9 120.3
C10 C9 H9 120.3
N2 C10 C9 121.8(6)
N2 C10 H10 119.1
C9 C10 H10 119.1
N3 C11 C12 122.2(5)
N3 C11 H11 118.9
C12 C11 H11 118.9
C11 C12 C13 119.4(5)
C11 C12 H12 120.3
C13 C12 H12 120.3
C14 C13 C12 119.1(6)
C14 C13 H13 120.5
C12 C13 H13 120.5
C13 C14 C15 118.8(5)
C13 C14 H14 120.6
C15 C14 H14 120.6
N3 C15 C14 122.1(5)
N3 C15 C16 114.8(4)
C14 C15 C16 123.1(5)
N4 C16 C17 120.5(5)
N4 C16 C15 115.1(4)
C17 C16 C15 124.4(5)
C18 C17 C16 120.6(6)
C18 C17 H17 119.7
C16 C17 H17 119.7
C17 C18 C19 118.1(5)
C17 C18 H18 121.0
C19 C18 H18 121.0
C20 C19 C18 119.4(5)
C20 C19 H19 120.3
C18 C19 H19 120.3
N4 C20 C19 121.7(5)
N4 C20 H20 119.1
C19 C20 H20 119.1
N5 C21 Cu1 173.3(5)
O4 Cl1 O1 114.6(12)
O4 Cl1 O2 103.7(7)
O1 Cl1 O2 115.6(6)
O4 Cl1 O3 98.0(11)
O1 Cl1 O3 108.8(5)
O2 Cl1 O3 114.9(5)
C1 N1 C5 118.7(5)
C1 N1 Cu1 128.0(4)
C5 N1 Cu1 113.2(3)
C10 N2 C6 119.2(5)
C10 N2 Cu1 124.3(4)
C6 N2 Cu1 116.5(4)
C11 N3 C15 118.4(4)
C11 N3 Cu1 128.0(4)
C15 N3 Cu1 113.5(3)
C20 N4 C16 119.7(5)
C20 N4 Cu1 122.7(4)
C16 N4 Cu1 117.5(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Cu1 C21 1.959(7)
Cu1 N4 2.003(4)
Cu1 N2 2.011(4)
Cu1 N1 2.103(4)
Cu1 N3 2.132(4)
C1 N1 1.339(7)
C1 C2 1.376(8)
C1 H1 0.9300
C2 C3 1.346(10)
C2 H2 0.9300
C3 C4 1.356(10)
C3 H3 0.9300
C4 C5 1.399(7)
C4 H4 0.9300
C5 N1 1.355(7)
C5 C6 1.460(7)
C6 N2 1.344(6)
C6 C7 1.372(7)
C7 C8 1.383(9)
C7 H7 0.9300
C8 C9 1.346(9)
C8 H8 0.9300
C9 C10 1.376(8)
C9 H9 0.9300
C10 N2 1.319(7)
C10 H10 0.9300
C11 N3 1.331(6)
C11 C12 1.371(7)
C11 H11 0.9300
C12 C13 1.375(8)
C12 H12 0.9300
C13 C14 1.362(8)
C13 H13 0.9300
C14 C15 1.386(7)
C14 H14 0.9300
C15 N3 1.339(6)
C15 C16 1.494(7)
C16 N4 1.344(6)
C16 C17 1.376(7)
C17 C18 1.375(8)
C17 H17 0.9300
C18 C19 1.384(8)
C18 H18 0.9300
C19 C20 1.376(7)
C19 H19 0.9300
C20 N4 1.337(7)
C20 H20 0.9300
C21 N5 1.182(7)
Cl1 O4 1.225(10)
Cl1 O1 1.263(6)
Cl1 O2 1.375(7)
Cl1 O3 1.376(8)
