#------------------------------------------------------------------------------
#$Date: 2016-03-25 16:59:06 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179998 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/92/7029223.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_7029223
loop_
_publ_author_name
'Byrne, Joseph P.'
'Kitchen, Jonathan A.'
'Kotova, Oxana'
'Leigh, Vivienne'
'Bell, Alan P.'
'Boland, John J.'
'Albrecht, Martin'
'Gunnlaugsson, Thorfinnur'
_publ_section_title
;
 Synthesis, structural, photophysical and electrochemical studies of
 various d-metal complexes of btp [2,6-bis(1,2,3-triazol-4-yl)pyridine]
 ligands that give rise to the formation of metallo-supramolecular gels.
;
_journal_issue                   1
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              196
_journal_page_last               209
_journal_paper_doi               10.1039/c3dt52309h
_journal_volume                  43
_journal_year                    2014
_chemical_formula_sum            'C27 H23 N7 O4'
_chemical_formula_weight         509.52
_chemical_name_systematic
; 
 ? 
;
_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                92.45(3)
_cell_angle_beta                 101.17(3)
_cell_angle_gamma                100.30(3)
_cell_formula_units_Z            2
_cell_length_a                   6.3501(13)
_cell_length_b                   12.965(3)
_cell_length_c                   14.859(3)
_cell_measurement_reflns_used    3850
_cell_measurement_temperature    108(2)
_cell_measurement_theta_max      31.2592
_cell_measurement_theta_min      2.2114
_cell_volume                     1177.0(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      108(2)
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  'Rigaku saturn 724'
_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  0.0380
_diffrn_reflns_av_sigmaI/netI    0.0356
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13407
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.21
_exptl_absorpt_coefficient_mu    0.101
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Crystalclear
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.438
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.196
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.214
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     345
_refine_ls_number_reflns         3981
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.214
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0639
_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)+(0.0356P)²+0.8968P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1262
_refine_ls_wR_factor_ref         0.1304
_reflns_number_gt                3614
_reflns_number_total             3981
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3dt52309h.txt
_cod_data_source_block           jpb028
_cod_original_cell_volume        1176.9(4)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7029223
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-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
O1 O 0.7000(3) 0.62807(15) 1.06699(12) 0.0346(5) Uani 1 1 d .
O2 O 1.0660(3) 0.64617(15) 1.10776(13) 0.0390(5) Uani 1 1 d .
O3 O 0.7985(3) -0.10423(15) 1.13879(13) 0.0374(5) Uani 1 1 d .
O4 O 0.4314(3) -0.14009(15) 1.09124(12) 0.0360(5) Uani 1 1 d .
N1 N 1.0288(3) 0.52542(15) 0.62993(14) 0.0232(5) Uani 1 1 d .
N2 N 1.2031(3) 0.57120(16) 0.59625(14) 0.0261(5) Uani 1 1 d .
N3 N 1.3066(3) 0.49597(16) 0.57667(14) 0.0264(5) Uani 1 1 d .
N4 N 1.1562(3) 0.21518(15) 0.60828(13) 0.0222(5) Uani 1 1 d .
N5 N 1.1452(3) -0.06882(16) 0.61009(15) 0.0270(5) Uani 1 1 d .
N6 N 0.9941(4) -0.13983(16) 0.63479(15) 0.0273(5) Uani 1 1 d .
N7 N 0.8462(3) -0.08805(15) 0.66099(14) 0.0242(5) Uani 1 1 d .
C1 C 0.6911(5) 0.6384(2) 1.16354(18) 0.0397(7) Uani 1 1 d .
H1A H 0.7435 0.5796 1.1942 0.048 Uiso 1 1 calc R
H1B H 0.5399 0.6377 1.1696 0.048 Uiso 1 1 calc R
H1C H 0.7838 0.7049 1.1922 0.048 Uiso 1 1 calc R
C2 C 0.9014(5) 0.63248(19) 1.04880(19) 0.0311(6) Uani 1 1 d .
C3 C 0.8926(4) 0.61821(19) 0.94783(18) 0.0279(6) Uani 1 1 d .
C4 C 0.6956(4) 0.5968(2) 0.88456(18) 0.0298(6) Uani 1 1 d .
H4 H 0.5617 0.5897 0.9053 0.036 Uiso 1 1 calc R
C5 C 0.6934(4) 0.5858(2) 0.79072(18) 0.0298(6) Uani 1 1 d .
H5 H 0.5575 0.5704 0.7480 0.036 Uiso 1 1 calc R
C6 C 0.8867(4) 0.59688(18) 0.75887(17) 0.0242(5) Uani 1 1 d .
C7 C 1.0844(4) 0.6184(2) 0.82259(18) 0.0280(6) Uani 1 1 d .
H7 H 1.2182 0.6264 0.8017 0.034 Uiso 1 1 calc R
C8 C 1.0881(4) 0.6285(2) 0.91679(19) 0.0303(6) Uani 1 1 d .
H8 H 1.2237 0.6422 0.9597 0.036 Uiso 1 1 calc R
C9 C 0.8800(4) 0.58946(19) 0.65653(17) 0.0260(6) Uani 1 1 d .
H9A H 0.7289 0.5590 0.6238 0.031 Uiso 1 1 calc R
H9B H 0.9183 0.6612 0.6368 0.031 Uiso 1 1 calc R
C10 C 1.0210(4) 0.42055(18) 0.63233(17) 0.0236(5) Uani 1 1 d .
H10 H 0.9158 0.3707 0.6531 0.028 Uiso 1 1 calc R
C11 C 1.1976(4) 0.40181(18) 0.59831(16) 0.0218(5) Uani 1 1 d .
C12 C 1.2763(4) 0.30306(18) 0.58450(16) 0.0212(5) Uani 1 1 d .
C13 C 1.4653(4) 0.30351(19) 0.54922(16) 0.0244(6) Uani 1 1 d .
H13 H 1.5429 0.3668 0.5322 0.029 Uiso 1 1 calc R
C14 C 1.5367(4) 0.2091(2) 0.53971(17) 0.0256(6) Uani 1 1 d .
H14 H 1.6663 0.2069 0.5173 0.031 Uiso 1 1 calc R
C15 C 1.4154(4) 0.11812(19) 0.56352(16) 0.0243(5) Uani 1 1 d .
H15 H 1.4608 0.0526 0.5576 0.029 Uiso 1 1 calc R
C16 C 1.2266(4) 0.12414(18) 0.59616(16) 0.0222(5) Uani 1 1 d .
C17 C 1.0918(4) 0.02821(18) 0.62055(16) 0.0216(5) Uani 1 1 d .
C18 C 0.9017(4) 0.01684(19) 0.65297(16) 0.0247(6) Uani 1 1 d .
H18 H 0.8256 0.0704 0.6667 0.030 Uiso 1 1 calc R
C19 C 0.6522(4) -0.14733(19) 0.68789(17) 0.0252(6) Uani 1 1 d .
H19A H 0.6376 -0.2226 0.6682 0.030 Uiso 1 1 calc R
H19B H 0.5214 -0.1232 0.6546 0.030 Uiso 1 1 calc R
C20 C 0.6557(4) -0.13690(18) 0.78989(17) 0.0246(6) Uani 1 1 d .
C21 C 0.4567(4) -0.1480(2) 0.81765(18) 0.0302(6) Uani 1 1 d .
H21 H 0.3244 -0.1593 0.7728 0.036 Uiso 1 1 calc R
C22 C 0.4501(4) -0.1427(2) 0.91056(18) 0.0311(6) Uani 1 1 d .
H22 H 0.3133 -0.1497 0.9288 0.037 Uiso 1 1 calc R
C23 C 0.6419(4) -0.12737(19) 0.97701(17) 0.0269(6) Uani 1 1 d .
C24 C 0.8410(4) -0.11672(19) 0.94943(18) 0.0282(6) Uani 1 1 d .
H24 H 0.9731 -0.1067 0.9944 0.034 Uiso 1 1 calc R
C25 C 0.8481(4) -0.12061(19) 0.85636(17) 0.0278(6) Uani 1 1 d .
H25 H 0.9851 -0.1121 0.8381 0.033 Uiso 1 1 calc R
C26 C 0.6384(4) -0.1219(2) 1.07710(18) 0.0298(6) Uani 1 1 d .
C27 C 0.4066(5) -0.1363(2) 1.18594(18) 0.0388(7) Uani 1 1 d .
H27A H 0.4579 -0.1960 1.2154 0.047 Uiso 1 1 calc R
H27B H 0.2521 -0.1399 1.1879 0.047 Uiso 1 1 calc R
H27C H 0.4930 -0.0704 1.2187 0.047 Uiso 1 1 calc R
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
C2 O1 C1 115.6(2)
C26 O4 C27 116.6(2)
N2 N1 C10 110.7(2)
N2 N1 C9 119.82(19)
C10 N1 C9 129.5(2)
N3 N2 N1 107.24(19)
N2 N3 C11 108.7(2)
C16 N4 C12 116.7(2)
N6 N5 C17 108.5(2)
N5 N6 N7 107.23(19)
N6 N7 C18 110.9(2)
N6 N7 C19 119.71(19)
C18 N7 C19 129.3(2)
O1 C1 H1A 109.5
O1 C1 H1B 109.5
H1A C1 H1B 109.5
O1 C1 H1C 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
O2 C2 O1 123.4(3)
O2 C2 C3 125.1(3)
O1 C2 C3 111.5(2)
C4 C3 C8 119.5(2)
C4 C3 C2 121.7(2)
C8 C3 C2 118.8(2)
C3 C4 C5 120.2(3)
C3 C4 H4 119.9
C5 C4 H4 119.9
C6 C5 C4 120.9(2)
C6 C5 H5 119.6
C4 C5 H5 119.6
C5 C6 C7 118.8(2)
C5 C6 C9 119.8(2)
C7 C6 C9 121.4(2)
C6 C7 C8 120.7(2)
C6 C7 H7 119.6
C8 C7 H7 119.6
C3 C8 C7 119.9(2)
C3 C8 H8 120.0
C7 C8 H8 120.0
N1 C9 C6 113.2(2)
N1 C9 H9A 108.9
C6 C9 H9A 108.9
N1 C9 H9B 108.9
C6 C9 H9B 108.9
H9A C9 H9B 107.8
N1 C10 C11 105.2(2)
N1 C10 H10 127.4
C11 C10 H10 127.4
C10 C11 N3 108.2(2)
C10 C11 C12 130.7(2)
N3 C11 C12 121.1(2)
N4 C12 C13 123.6(2)
N4 C12 C11 116.0(2)
C13 C12 C11 120.4(2)
C14 C13 C12 118.4(2)
C14 C13 H13 120.8
C12 C13 H13 120.8
C15 C14 C13 118.8(2)
C15 C14 H14 120.6
C13 C14 H14 120.6
C14 C15 C16 119.1(2)
C14 C15 H15 120.4
C16 C15 H15 120.4
N4 C16 C15 123.4(2)
N4 C16 C17 116.3(2)
C15 C16 C17 120.3(2)
N5 C17 C18 108.8(2)
N5 C17 C16 121.6(2)
C18 C17 C16 129.6(2)
N7 C18 C17 104.6(2)
N7 C18 H18 127.7
C17 C18 H18 127.7
N7 C19 C20 114.4(2)
N7 C19 H19A 108.7
C20 C19 H19A 108.7
N7 C19 H19B 108.7
C20 C19 H19B 108.7
H19A C19 H19B 107.6
C21 C20 C25 119.1(2)
C21 C20 C19 118.0(2)
C25 C20 C19 122.8(2)
C22 C21 C20 120.4(2)
C22 C21 H21 119.8
C20 C21 H21 119.8
C21 C22 C23 120.5(3)
C21 C22 H22 119.7
C23 C22 H22 119.7
C24 C23 C22 119.2(2)
C24 C23 C26 119.4(2)
C22 C23 C26 121.4(2)
C23 C24 C25 120.4(2)
C23 C24 H24 119.8
C25 C24 H24 119.8
C20 C25 C24 120.4(2)
C20 C25 H25 119.8
C24 C25 H25 119.8
O3 C26 O4 123.5(2)
O3 C26 C23 125.1(3)
O4 C26 C23 111.4(2)
O4 C27 H27A 109.5
O4 C27 H27B 109.5
H27A C27 H27B 109.5
O4 C27 H27C 109.5
H27A C27 H27C 109.5
H27B C27 H27C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
O1 C2 1.349(3)
O1 C1 1.448(3)
O2 C2 1.207(3)
O3 C26 1.210(3)
O4 C26 1.352(3)
O4 C27 1.446(3)
N1 N2 1.354(3)
N1 C10 1.354(3)
N1 C9 1.462(3)
N2 N3 1.322(3)
N3 C11 1.375(3)
N4 C16 1.352(3)
N4 C12 1.354(3)
N5 N6 1.324(3)
N5 C17 1.370(3)
N6 N7 1.352(3)
N7 C18 1.359(3)
N7 C19 1.465(3)
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C2 C3 1.493(4)
C3 C4 1.387(4)
C3 C8 1.392(4)
C4 C5 1.393(4)
C4 H4 0.9500
C5 C6 1.385(4)
C5 H5 0.9500
C6 C7 1.394(4)
C6 C9 1.511(3)
C7 C8 1.396(4)
C7 H7 0.9500
C8 H8 0.9500
C9 H9A 0.9900
C9 H9B 0.9900
C10 C11 1.370(3)
C10 H10 0.9500
C11 C12 1.476(3)
C12 C13 1.399(3)
C13 C14 1.391(3)
C13 H13 0.9500
C14 C15 1.387(3)
C14 H14 0.9500
C15 C16 1.391(3)
C15 H15 0.9500
C16 C17 1.480(3)
C17 C18 1.371(3)
C18 H18 0.9500
C19 C20 1.511(3)
C19 H19A 0.9900
C19 H19B 0.9900
C20 C21 1.389(4)
C20 C25 1.391(4)
C21 C22 1.388(4)
C21 H21 0.9500
C22 C23 1.389(4)
C22 H22 0.9500
C23 C24 1.389(4)
C23 C26 1.491(4)
C24 C25 1.392(4)
C24 H24 0.9500
C25 H25 0.9500
C27 H27A 0.9800
C27 H27B 0.9800
C27 H27C 0.9800
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
C10 N1 N2 N3 0.3(3)
C9 N1 N2 N3 -179.0(2)
N1 N2 N3 C11 -0.2(3)
C17 N5 N6 N7 -0.2(3)
N5 N6 N7 C18 0.2(3)
N5 N6 N7 C19 177.0(2)
C1 O1 C2 O2 -1.4(4)
C1 O1 C2 C3 178.5(2)
O2 C2 C3 C4 176.2(3)
O1 C2 C3 C4 -3.7(3)
O2 C2 C3 C8 -4.8(4)
O1 C2 C3 C8 175.3(2)
C8 C3 C4 C5 -0.1(4)
C2 C3 C4 C5 178.9(2)
C3 C4 C5 C6 -0.6(4)
C4 C5 C6 C7 0.6(4)
C4 C5 C6 C9 -177.2(2)
C5 C6 C7 C8 0.1(4)
C9 C6 C7 C8 177.9(2)
C4 C3 C8 C7 0.8(4)
C2 C3 C8 C7 -178.2(2)
C6 C7 C8 C3 -0.8(4)
N2 N1 C9 C6 -113.0(2)
C10 N1 C9 C6 67.8(3)
C5 C6 C9 N1 -135.7(2)
C7 C6 C9 N1 46.6(3)
N2 N1 C10 C11 -0.2(3)
C9 N1 C10 C11 179.0(2)
N1 C10 C11 N3 0.1(3)
N1 C10 C11 C12 179.6(2)
N2 N3 C11 C10 0.0(3)
N2 N3 C11 C12 -179.5(2)
C16 N4 C12 C13 -0.2(3)
C16 N4 C12 C11 -179.9(2)
C10 C11 C12 N4 0.5(4)
N3 C11 C12 N4 179.9(2)
C10 C11 C12 C13 -179.2(2)
N3 C11 C12 C13 0.3(3)
N4 C12 C13 C14 -1.4(4)
C11 C12 C13 C14 178.3(2)
C12 C13 C14 C15 1.4(4)
C13 C14 C15 C16 0.0(4)
C12 N4 C16 C15 1.8(3)
C12 N4 C16 C17 -178.8(2)
C14 C15 C16 N4 -1.7(4)
C14 C15 C16 C17 178.9(2)
N6 N5 C17 C18 0.1(3)
N6 N5 C17 C16 -178.4(2)
N4 C16 C17 N5 179.1(2)
C15 C16 C17 N5 -1.4(3)
N4 C16 C17 C18 1.0(4)
C15 C16 C17 C18 -179.6(2)
N6 N7 C18 C17 -0.1(3)
C19 N7 C18 C17 -176.5(2)
N5 C17 C18 N7 0.0(3)
C16 C17 C18 N7 178.3(2)
N6 N7 C19 C20 107.6(2)
C18 N7 C19 C20 -76.2(3)
N7 C19 C20 C21 152.0(2)
N7 C19 C20 C25 -30.4(3)
C25 C20 C21 C22 0.1(4)
C19 C20 C21 C22 177.8(2)
C20 C21 C22 C23 -0.7(4)
C21 C22 C23 C24 0.4(4)
C21 C22 C23 C26 -179.7(2)
C22 C23 C24 C25 0.5(4)
C26 C23 C24 C25 -179.4(2)
C21 C20 C25 C24 0.7(4)
C19 C20 C25 C24 -176.8(2)
C23 C24 C25 C20 -1.0(4)
C27 O4 C26 O3 0.7(4)
C27 O4 C26 C23 -179.7(2)
C24 C23 C26 O3 3.3(4)
C22 C23 C26 O3 -176.6(3)
C24 C23 C26 O4 -176.3(2)
C22 C23 C26 O4 3.8(3)
