#------------------------------------------------------------------------------
#$Date: 2015-08-08 05:06:54 +0300 (Sat, 08 Aug 2015) $
#$Revision: 153166 $
#$URL: svn://www.crystallography.net/cod/cif/7/03/55/7035506.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_7035506
loop_
_publ_author_name
'Yamada, Atsutoshi'
'Mabe, Takuya'
'Yamane, Ryohei'
'Noda, Kyoko'
'Wasada, Yuko'
'Inamo, Masahiko'
'Ishihara, Koji'
'Suzuki, Takayoshi'
'Takagi, Hideo D.'
_publ_section_title
;
 Flipping of the coordinated triazine moiety in Cu(i)-L2 and the small
 electronic factor, \kel, for direct outer-sphere cross reactions:
 syntheses, crystal structures and redox behaviour of copper(ii)/(i)-L2
 complexes (L = 3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine).
;
_journal_issue                   31
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13979
_journal_page_last               13990
_journal_paper_doi               10.1039/c5dt01808k
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety         'C40 H32 Cu N8 O2 2+, 2(B F4 1-)'
_chemical_formula_sum            'C40 H32 B2 Cu F8 N8 O2'
_chemical_formula_weight         893.90
_chemical_name_systematic
'Bis(3-(2-pyridyl)-5,6-diphenyl-1,2,4-triazine)diaquocopper(II) Tetrafluoroborate'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-05-14 deposited with the CCDC.
2015-06-19 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 93.50(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.870(4)
_cell_length_b                   11.255(3)
_cell_length_c                   29.713(13)
_cell_measurement_reflns_used    4080
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.2
_cell_volume                     3962(2)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 1.11'
_computing_molecular_graphics    ORTEP
_computing_publication_material  SHELXL-97
_computing_structure_refinement  SHELXL-97
_computing_structure_solution    SIR92
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            19083
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.17
_exptl_absorpt_coefficient_mu    0.637
_exptl_absorpt_correction_T_max  0.880
_exptl_absorpt_correction_T_min  0.700
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1820
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.845
_refine_diff_density_min         -0.609
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment
'H atoms of coordinated water were fixed; the others were constr'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     286
_refine_ls_number_reflns         4560
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0807
_refine_ls_R_factor_gt           0.0583
_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)+(0.1213P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1722
_refine_ls_wR_factor_ref         0.1822
_reflns_number_gt                3208
_reflns_number_total             4560
_reflns_threshold_expression     'I> 2σ(I)'
_cod_data_source_file            c5dt01808k3.cif
_cod_data_source_block           Cupdt
_cod_depositor_comments
'Adding full bibliography for 7035505--7035506.cif.'
_cod_database_code               7035506
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
Cu Cu 0.2500 0.2500 0.5000 0.0440(2) Uani 1 2 d S
F1 F -0.0422(3) 0.0061(4) 0.57460(15) 0.1361(15) Uani 1 1 d .
F2 F 0.1096(3) 0.0257(4) 0.6215(2) 0.167(2) Uani 1 1 d .
F3 F 0.0209(4) -0.1510(3) 0.61278(17) 0.1425(16) Uani 1 1 d .
F4A F 0.1072(7) -0.0797(8) 0.5650(3) 0.128(3) Uani 0.50 1 d P
F4B F -0.0467(5) -0.0043(4) 0.64292(19) 0.0812(16) Uani 0.50 1 d P
O1 O 0.0629(2) 0.1707(2) 0.50668(9) 0.0621(7) Uani 1 1 d .
N1 N 0.3316(2) 0.1223(2) 0.58482(8) 0.0344(5) Uani 1 1 d .
N2 N 0.2837(2) 0.2193(2) 0.56694(8) 0.0351(5) Uani 1 1 d .
N4 N 0.26457(19) 0.3033(2) 0.63861(8) 0.0317(5) Uani 1 1 d .
N32 N 0.1972(3) 0.4070(2) 0.52626(9) 0.0475(7) Uani 1 1 d .
C3 C 0.2546(2) 0.3065(2) 0.59358(9) 0.0295(6) Uani 1 1 d .
C5 C 0.3060(2) 0.2052(3) 0.65725(9) 0.0313(6) Uani 1 1 d .
C6 C 0.3430(2) 0.1110(2) 0.62919(9) 0.0285(5) Uani 1 1 d .
C31 C 0.2061(2) 0.4132(2) 0.57146(9) 0.0318(6) Uani 1 1 d .
C33 C 0.1558(5) 0.5016(4) 0.50417(13) 0.0794(16) Uani 1 1 d .
H33 H 0.1495 0.4996 0.4721 0.064 Uiso 1 1 calc R
C34 C 0.1214(5) 0.6029(4) 0.52590(13) 0.0763(15) Uani 1 1 d .
H34 H 0.0920 0.6687 0.5090 0.064 Uiso 1 1 calc R
C35 C 0.1299(3) 0.6073(3) 0.57173(11) 0.0472(8) Uani 1 1 d .
H35 H 0.1067 0.6760 0.5873 0.064 Uiso 1 1 calc R
C36 C 0.1729(3) 0.5100(3) 0.59510(10) 0.0377(6) Uani 1 1 d .
H36 H 0.1794 0.5102 0.6271 0.064 Uiso 1 1 calc R
C51 C 0.3064(2) 0.2013(3) 0.70696(10) 0.0360(6) Uani 1 1 d .
C52 C 0.3516(3) 0.2960(3) 0.73117(11) 0.0510(8) Uani 1 1 d .
H52 H 0.3855 0.3597 0.7160 0.064 Uiso 1 1 calc R
C53 C 0.3477(4) 0.2987(4) 0.77782(13) 0.0653(11) Uani 1 1 d .
H53 H 0.3811 0.3629 0.7945 0.064 Uiso 1 1 calc R
C54 C 0.2959(4) 0.2093(4) 0.79966(12) 0.0652(12) Uani 1 1 d .
H54 H 0.2916 0.2124 0.8315 0.064 Uiso 1 1 calc R
C55 C 0.2500(4) 0.1148(5) 0.77575(13) 0.0681(12) Uani 1 1 d .
H55 H 0.2135 0.0529 0.7910 0.064 Uiso 1 1 calc R
C56 C 0.2568(3) 0.1095(3) 0.72918(12) 0.0512(8) Uani 1 1 d .
H56 H 0.2272 0.0429 0.7128 0.064 Uiso 1 1 calc R
C61 C 0.3967(2) -0.0008(3) 0.64518(9) 0.0335(6) Uani 1 1 d .
C62 C 0.3719(3) -0.1041(3) 0.62109(11) 0.0409(7) Uani 1 1 d .
H62 H 0.3179 -0.1022 0.5961 0.064 Uiso 1 1 calc R
C63 C 0.4252(3) -0.2102(3) 0.63317(13) 0.0480(8) Uani 1 1 d .
H63 H 0.4078 -0.2807 0.6166 0.064 Uiso 1 1 calc R
C64 C 0.5040(3) -0.2124(3) 0.66948(13) 0.0503(9) Uani 1 1 d .
H64 H 0.5408 -0.2847 0.6779 0.064 Uiso 1 1 calc R
C65 C 0.5291(3) -0.1105(3) 0.69341(12) 0.0486(8) Uani 1 1 d .
H65 H 0.5834 -0.1129 0.7183 0.064 Uiso 1 1 calc R
C66 C 0.4761(2) -0.0044(3) 0.68163(10) 0.0406(7) Uani 1 1 d .
H66 H 0.4939 0.0658 0.6984 0.064 Uiso 1 1 calc R
B19 B 0.0296(4) -0.0370(4) 0.6056(2) 0.0682(14) Uani 1 1 d .
H01 H 0.0641 0.1227 0.5247 0.064 Uiso 1 1 d .
H02 H 0.0405 0.1348 0.4839 0.064 Uiso 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'
B B 0.0013 0.0007 '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'
F F 0.0171 0.0103 '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'
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 Cu N2 180.0 . 7_556
N2 Cu N32 79.64(10) . .
N2 Cu N32 100.36(10) 7_556 .
N2 Cu N32 100.36(10) . 7_556
N2 Cu N32 79.64(10) 7_556 7_556
N32 Cu N32 180.00(13) . 7_556
N2 Cu O1 89.05(10) . .
N2 Cu O1 90.95(10) 7_556 .
N32 Cu O1 89.03(11) . .
N32 Cu O1 90.97(11) 7_556 .
N2 Cu O1 90.95(10) . 7_556
N2 Cu O1 89.05(10) 7_556 7_556
N32 Cu O1 90.97(11) . 7_556
N32 Cu O1 89.03(11) 7_556 7_556
O1 Cu O1 180.0 . 7_556
Cu O1 H01 110.1(2) . .
Cu O1 H02 111.6(2) . .
H01 O1 H02 102.8(3) . .
C6 N1 N2 119.5(2) . .
C3 N2 N1 119.5(2) . .
C3 N2 Cu 114.66(19) . .
N1 N2 Cu 125.81(18) . .
C5 N4 C3 116.9(2) . .
C33 N32 C31 117.1(3) . .
C33 N32 Cu 128.1(2) . .
C31 N32 Cu 114.81(19) . .
N2 C3 N4 124.7(3) . .
N2 C3 C31 116.7(2) . .
N4 C3 C31 118.6(2) . .
N4 C5 C6 119.6(2) . .
N4 C5 C51 115.1(2) . .
C6 C5 C51 125.2(3) . .
N1 C6 C5 119.5(2) . .
N1 C6 C61 114.7(2) . .
C5 C6 C61 125.8(2) . .
N32 C31 C36 123.2(3) . .
N32 C31 C3 114.2(2) . .
C36 C31 C3 122.6(3) . .
N32 C33 C34 122.7(3) . .
N32 C33 H33 118.6 . .
C34 C33 H33 118.6 . .
C35 C34 C33 119.4(3) . .
C35 C34 H34 120.3 . .
C33 C34 H34 120.3 . .
C34 C35 C36 118.5(3) . .
C34 C35 H35 120.7 . .
C36 C35 H35 120.7 . .
C31 C36 C35 119.0(3) . .
C31 C36 H36 120.5 . .
C35 C36 H36 120.5 . .
C52 C51 C56 119.6(3) . .
C52 C51 C5 118.5(3) . .
C56 C51 C5 121.7(3) . .
C51 C52 C53 120.1(4) . .
C51 C52 H52 119.9 . .
C53 C52 H52 119.9 . .
C54 C53 C52 120.1(4) . .
C54 C53 H53 119.9 . .
C52 C53 H53 119.9 . .
C53 C54 C55 120.1(3) . .
C53 C54 H54 120.0 . .
C55 C54 H54 120.0 . .
C54 C55 C56 120.2(4) . .
C54 C55 H55 119.9 . .
C56 C55 H55 119.9 . .
C51 C56 C55 119.8(4) . .
C51 C56 H56 120.1 . .
C55 C56 H56 120.1 . .
C62 C61 C66 119.3(3) . .
C62 C61 C6 118.3(3) . .
C66 C61 C6 122.3(3) . .
C61 C62 C63 120.5(3) . .
C61 C62 H62 119.7 . .
C63 C62 H62 119.7 . .
C64 C63 C62 119.5(3) . .
C64 C63 H63 120.2 . .
C62 C63 H63 120.2 . .
C65 C64 C63 120.3(3) . .
C65 C64 H64 119.9 . .
C63 C64 H64 119.9 . .
C64 C65 C66 120.6(3) . .
C64 C65 H65 119.7 . .
C66 C65 H65 119.7 . .
C65 C66 C61 119.8(3) . .
C65 C66 H66 120.1 . .
C61 C66 H66 120.1 . .
F2 B19 F3 123.9(5) . .
F2 B19 F1 120.2(5) . .
F3 B19 F1 115.1(5) . .
F2 B19 F4B 93.5(5) . .
F3 B19 F4B 93.5(4) . .
F1 B19 F4B 91.8(5) . .
F2 B19 F4A 89.8(5) . .
F3 B19 F4A 83.5(5) . .
F1 B19 F4A 87.8(5) . .
F4B B19 F4A 176.5(5) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Cu N2 2.034(3) .
Cu N2 2.034(3) 7_556
Cu N32 2.045(2) .
Cu N32 2.045(2) 7_556
Cu O1 2.413(3) .
Cu O1 2.413(3) 7_556
F1 B19 1.310(6) .
F2 B19 1.252(5) .
F3 B19 1.306(5) .
F4A B19 1.633(10) .
F4B B19 1.520(8) .
O1 H01 0.760(3) .
O1 H02 0.819(3) .
N1 C6 1.323(4) .
N1 N2 1.327(3) .
N2 C3 1.320(4) .
N4 C5 1.317(4) .
N4 C3 1.336(4) .
N32 C33 1.330(4) .
N32 C31 1.342(4) .
C3 C31 1.469(4) .
C5 C6 1.434(4) .
C5 C51 1.477(4) .
C6 C61 1.477(4) .
C31 C36 1.368(4) .
C33 C34 1.384(5) .
C33 H33 0.9500 .
C34 C35 1.360(5) .
C34 H34 0.9500 .
C35 C36 1.378(4) .
C35 H35 0.9500 .
C36 H36 0.9500 .
C51 C52 1.377(5) .
C51 C56 1.377(5) .
C52 C53 1.390(5) .
C52 H52 0.9500 .
C53 C54 1.364(7) .
C53 H53 0.9500 .
C54 C55 1.373(7) .
C54 H54 0.9500 .
C55 C56 1.392(5) .
C55 H55 0.9500 .
C56 H56 0.9500 .
C61 C62 1.388(4) .
C61 C66 1.392(4) .
C62 C63 1.389(4) .
C62 H62 0.9500 .
C63 C64 1.384(6) .
C63 H63 0.9500 .
C64 C65 1.372(5) .
C64 H64 0.9500 .
C65 C66 1.386(5) .
C65 H65 0.9500 .
C66 H66 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
C6 N1 N2 C3 4.4(4) .
C6 N1 N2 Cu -176.3(2) .
N2 Cu N2 C3 135(6) 7_556
N32 Cu N2 C3 1.9(2) .
N32 Cu N2 C3 -178.1(2) 7_556
O1 Cu N2 C3 -87.3(2) .
O1 Cu N2 C3 92.7(2) 7_556
N2 Cu N2 N1 -44(6) 7_556
N32 Cu N2 N1 -177.5(3) .
N32 Cu N2 N1 2.5(3) 7_556
O1 Cu N2 N1 93.3(2) .
O1 Cu N2 N1 -86.7(2) 7_556
N2 Cu N32 C33 178.4(4) .
N2 Cu N32 C33 -1.6(4) 7_556
N32 Cu N32 C33 96.1(9) 7_556
O1 Cu N32 C33 -92.4(4) .
O1 Cu N32 C33 87.6(4) 7_556
N2 Cu N32 C31 -1.7(2) .
N2 Cu N32 C31 178.3(2) 7_556
N32 Cu N32 C31 -84.0(8) 7_556
O1 Cu N32 C31 87.5(2) .
O1 Cu N32 C31 -92.5(2) 7_556
N1 N2 C3 N4 -3.6(4) .
Cu N2 C3 N4 177.0(2) .
N1 N2 C3 C31 177.6(2) .
Cu N2 C3 C31 -1.8(3) .
C5 N4 C3 N2 -0.3(4) .
C5 N4 C3 C31 178.5(2) .
C3 N4 C5 C6 3.1(4) .
C3 N4 C5 C51 -175.0(2) .
N2 N1 C6 C5 -1.6(4) .
N2 N1 C6 C61 179.6(2) .
N4 C5 C6 N1 -2.2(4) .
C51 C5 C6 N1 175.7(3) .
N4 C5 C6 C61 176.4(3) .
C51 C5 C6 C61 -5.7(4) .
C33 N32 C31 C36 1.3(5) .
Cu N32 C31 C36 -178.6(2) .
C33 N32 C31 C3 -178.8(4) .
Cu N32 C31 C3 1.3(3) .
N2 C3 C31 N32 0.3(4) .
N4 C3 C31 N32 -178.5(3) .
N2 C3 C31 C36 -179.8(3) .
N4 C3 C31 C36 1.3(4) .
C31 N32 C33 C34 -0.7(8) .
Cu N32 C33 C34 179.1(4) .
N32 C33 C34 C35 0.1(9) .
C33 C34 C35 C36 0.0(7) .
N32 C31 C36 C35 -1.2(5) .
C3 C31 C36 C35 178.9(3) .
C34 C35 C36 C31 0.5(6) .
N4 C5 C51 C52 -50.3(4) .
C6 C5 C51 C52 131.7(3) .
N4 C5 C51 C56 125.6(3) .
C6 C5 C51 C56 -52.4(4) .
C56 C51 C52 C53 0.3(5) .
C5 C51 C52 C53 176.3(3) .
C51 C52 C53 C54 -2.1(6) .
C52 C53 C54 C55 1.7(6) .
C53 C54 C55 C56 0.4(6) .
C52 C51 C56 C55 1.7(5) .
C5 C51 C56 C55 -174.1(3) .
C54 C55 C56 C51 -2.1(6) .
N1 C6 C61 C62 -37.2(4) .
C5 C6 C61 C62 144.1(3) .
N1 C6 C61 C66 138.8(3) .
C5 C6 C61 C66 -39.9(4) .
C66 C61 C62 C63 0.1(5) .
C6 C61 C62 C63 176.2(3) .
C61 C62 C63 C64 -0.2(5) .
C62 C63 C64 C65 0.1(5) .
C63 C64 C65 C66 0.1(5) .
C64 C65 C66 C61 -0.1(5) .
C62 C61 C66 C65 0.0(4) .
C6 C61 C66 C65 -175.9(3) .
