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#$Date: 2016-03-26 20:59:30 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180459 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/28/7212804.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_7212804
loop_
_publ_author_name
'Hu, Sheng'
'Zhang, Ze-Ming'
'Meng, Zhao-Sha'
'Lin, Zhuo-Jia'
'Tong, Ming-Liang'
_publ_section_title
;
 Anion-dependent construction of
 copper(i/ii)-1,2,4,5-tetra(4-pyridyl)benzene frameworks
;
_journal_issue                   12
_journal_name_full               CrystEngComm
_journal_page_first              4378
_journal_paper_doi               10.1039/c0ce00141d
_journal_volume                  12
_journal_year                    2010
_chemical_formula_sum            'C28 H21 Br2 Cu2 N5'
_chemical_formula_weight         714.40
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 118.973(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1150(19)
_cell_length_b                   22.273(3)
_cell_length_c                   10.6802(15)
_cell_measurement_temperature    293(2)
_cell_volume                     2729.3(7)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.945
_diffrn_measured_fraction_theta_max 0.945
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0496
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       3
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4976
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         1.83
_exptl_absorpt_coefficient_mu    4.513
_exptl_absorpt_correction_T_max  0.3352
_exptl_absorpt_correction_T_min  0.2530
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_density_diffrn    1.739
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1408
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.31
_refine_diff_density_max         1.306
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     169
_refine_ls_number_reflns         2537
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.137
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0547
_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)+(0.0578P)²+5.5660P] where P=(Fo²+2Fc²)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1242
_refine_ls_wR_factor_ref         0.1309
_reflns_number_gt                2040
_reflns_number_total             2537
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c0ce00141d.txt
_cod_data_source_block           complex3
_cod_original_cell_volume        2729.4(7)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7212804
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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 0.91871(6) 0.33624(3) 0.79580(8) 0.0389(2) Uani 1 1 d .
Br1 Br 0.87224(6) 0.37504(3) 0.55449(7) 0.0441(2) Uani 1 1 d .
N1 N 0.9294(4) 0.24655(19) 0.8397(5) 0.0297(10) Uani 1 1 d .
N2 N 1.3137(4) -0.1197(2) 0.8544(6) 0.0372(12) Uani 1 1 d .
C1 C 1.0340(5) 0.2233(3) 0.9284(6) 0.0337(13) Uani 1 1 d .
H1A H 1.0979 0.2489 0.9651 0.040 Uiso 1 1 calc R
C2 C 1.0535(5) 0.1641(2) 0.9691(6) 0.0316(13) Uani 1 1 d .
H2A H 1.1284 0.1502 1.0301 0.038 Uiso 1 1 calc R
C3 C 0.9589(5) 0.1256(2) 0.9170(6) 0.0279(12) Uani 1 1 d .
C4 C 0.8514(5) 0.1480(2) 0.8215(6) 0.0299(12) Uani 1 1 d .
H4A H 0.7864 0.1231 0.7808 0.036 Uiso 1 1 calc R
C5 C 0.8417(5) 0.2080(2) 0.7870(6) 0.0324(13) Uani 1 1 d .
H5A H 0.7683 0.2225 0.7220 0.039 Uiso 1 1 calc R
C6 C 0.9786(5) 0.0609(2) 0.9635(6) 0.0279(12) Uani 1 1 d .
C7 C 1.0585(5) 0.0282(2) 0.9414(5) 0.0275(12) Uani 1 1 d .
H7A H 1.0989 0.0479 0.9022 0.033 Uiso 1 1 calc R
C8 C 1.0815(5) -0.0319(2) 0.9743(6) 0.0273(12) Uani 1 1 d .
C9 C 1.1629(5) -0.0627(2) 0.9357(6) 0.0284(12) Uani 1 1 d .
C10 C 1.2583(5) -0.0338(3) 0.9440(7) 0.0439(16) Uani 1 1 d .
H10A H 1.2752 0.0055 0.9778 0.053 Uiso 1 1 calc R
C11 C 1.3295(6) -0.0635(3) 0.9016(8) 0.0473(17) Uani 1 1 d .
H11A H 1.3927 -0.0426 0.9066 0.057 Uiso 1 1 calc R
C12 C 1.2208(5) -0.1476(3) 0.8476(6) 0.0363(14) Uani 1 1 d .
H12A H 1.2069 -0.1871 0.8149 0.044 Uiso 1 1 calc R
C13 C 1.1445(5) -0.1219(2) 0.8858(6) 0.0327(13) Uani 1 1 d .
H13A H 1.0813 -0.1436 0.8785 0.039 Uiso 1 1 calc R
C14 C 1.0000 0.3687(7) 0.2500 0.121(6) Uani 1 2 d SU
C15 C 1.0000 0.3039(7) 0.2500 0.090(4) Uani 1 2 d S
N3 N 1.0000 0.2553(9) 0.2500 0.163(7) Uani 1 2 d SU
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'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
N2 Cu1 N1 112.66(18) 3_455 .
N2 Cu1 Br1 106.81(14) 3_455 .
N1 Cu1 Br1 122.08(13) . .
N2 Cu1 Br1 109.03(15) 3_455 2_756
N1 Cu1 Br1 104.65(14) . 2_756
Br1 Cu1 Br1 100.35(3) . 2_756
N2 Cu1 Cu1 150.94(13) 3_455 2_756
N1 Cu1 Cu1 95.93(12) . 2_756
Br1 Cu1 Cu1 58.35(3) . 2_756
Br1 Cu1 Cu1 56.03(3) 2_756 2_756
Cu1 Br1 Cu1 65.62(3) . 2_756
C5 N1 C1 115.6(5) . .
C5 N1 Cu1 126.1(4) . .
C1 N1 Cu1 118.4(4) . .
C11 N2 C12 115.4(5) . .
C11 N2 Cu1 124.9(4) . 3_545
C12 N2 Cu1 119.7(4) . 3_545
N1 C1 C2 124.5(5) . .
N1 C1 H1A 117.7 . .
C2 C1 H1A 117.7 . .
C1 C2 C3 118.3(5) . .
C1 C2 H2A 120.8 . .
C3 C2 H2A 120.8 . .
C4 C3 C2 118.1(5) . .
C4 C3 C6 122.9(5) . .
C2 C3 C6 118.9(5) . .
C3 C4 C5 118.7(5) . .
C3 C4 H4A 120.6 . .
C5 C4 H4A 120.6 . .
N1 C5 C4 124.6(5) . .
N1 C5 H5A 117.7 . .
C4 C5 H5A 117.7 . .
C7 C6 C8 118.7(5) . 5_757
C7 C6 C3 118.0(4) . .
C8 C6 C3 123.2(4) 5_757 .
C8 C7 C6 123.8(5) . .
C8 C7 H7A 118.1 . .
C6 C7 H7A 118.1 . .
C7 C8 C6 117.4(5) . 5_757
C7 C8 C9 118.5(4) . .
C6 C8 C9 124.0(5) 5_757 .
C10 C9 C13 116.9(5) . .
C10 C9 C8 121.3(5) . .
C13 C9 C8 121.8(5) . .
C9 C10 C11 119.4(5) . .
C9 C10 H10A 120.3 . .
C11 C10 H10A 120.3 . .
N2 C11 C10 124.7(5) . .
N2 C11 H11A 117.7 . .
C10 C11 H11A 117.7 . .
N2 C12 C13 124.3(5) . .
N2 C12 H12A 117.8 . .
C13 C12 H12A 117.8 . .
C12 C13 C9 119.4(5) . .
C12 C13 H13A 120.3 . .
C9 C13 H13A 120.3 . .
N3 C15 C14 180.000(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu1 N2 2.021(4) 3_455
Cu1 N1 2.041(4) .
Cu1 Br1 2.4977(10) .
Cu1 Br1 2.5638(10) 2_756
Cu1 Cu1 2.7430(13) 2_756
Br1 Cu1 2.5638(10) 2_756
N1 C5 1.323(7) .
N1 C1 1.337(7) .
N2 C11 1.327(7) .
N2 C12 1.339(7) .
N2 Cu1 2.021(4) 3_545
C1 C2 1.372(7) .
C1 H1A 0.9300 .
C2 C3 1.384(8) .
C2 H2A 0.9300 .
C3 C4 1.372(8) .
C3 C6 1.505(7) .
C4 C5 1.376(7) .
C4 H4A 0.9300 .
C5 H5A 0.9300 .
C6 C7 1.387(7) .
C6 C8 1.411(7) 5_757
C7 C8 1.379(7) .
C7 H7A 0.9300 .
C8 C6 1.411(7) 5_757
C8 C9 1.486(7) .
C9 C10 1.372(8) .
C9 C13 1.397(7) .
C10 C11 1.387(8) .
C10 H10A 0.9300 .
C11 H11A 0.9300 .
C12 C13 1.375(7) .
C12 H12A 0.9300 .
C13 H13A 0.9300 .
C14 C15 1.44(2) .
C15 N3 1.084(19) .
