#------------------------------------------------------------------------------
#$Date: 2016-03-26 22:29:45 +0200 (Sat, 26 Mar 2016) $
#$Revision: 180508 $
#$URL: svn://www.crystallography.net/cod/cif/7/21/77/7217714.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_7217714
loop_
_publ_author_name
'Liu, Tong-Peng'
'Huo, Li-Hua'
'Deng, Zhao-Peng'
'Zhao, Hui'
'Gao, Shan'
_publ_section_title
;
 Supramolecular architectures and luminescent properties of salts
 containing flexible bis(pyridyl) cations with aliphatic diamine spacer:
 Effects of inorganic anions, alkalinity and conformation of the
 bis(pyridyl) cations
;
_journal_name_full               'RSC Advances'
_journal_paper_doi               10.1039/C4RA05029K
_journal_year                    2014
_chemical_formula_moiety         'C14 H22 N4, 4(N O3)'
_chemical_formula_sum            'C14 H22 N8 O12'
_chemical_formula_weight         494.40
_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                90.07(3)
_cell_angle_beta                 100.10(3)
_cell_angle_gamma                111.18(3)
_cell_formula_units_Z            1
_cell_length_a                   6.6103(13)
_cell_length_b                   8.2099(16)
_cell_length_c                   10.764(2)
_cell_measurement_reflns_used    3891
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      3.20
_cell_volume                     534.9(2)
_computing_cell_refinement
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_collection
;
CrysAlis Pro (Agilent, 2013)
;
_computing_data_reduction
;
CrysAlis Pro (Agilent, 2013)
;
_computing_molecular_graphics    '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_publication_material  '(K. Brandenburg, Diamond 3.1, 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      295(2)
_diffrn_detector_area_resol_mean 16.1954
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Xcalibur, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_sigmaI/netI    0.0438
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            4226
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.18
_exptl_absorpt_coefficient_mu    0.135
_exptl_absorpt_correction_T_max  0.9787
_exptl_absorpt_correction_T_min  0.9709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlis Pro (Agilent, 2013)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.535
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             258
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.182
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1873
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0539
_refine_ls_R_factor_gt           0.0416
_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)+(0.0726P)²+0.1122P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1151
_refine_ls_wR_factor_ref         0.1374
_reflns_number_gt                1497
_reflns_number_total             1873
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4ra05029k2.cif
_cod_data_source_block           complex13
_cod_original_cell_volume        534.94(18)
_cod_database_code               7217714
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 0.7601(5) 0.4965(3) 1.29494(17) 0.1007(8) Uani 1 1 d .
O2 O 0.7480(4) 0.5489(2) 1.48361(15) 0.0783(6) Uani 1 1 d .
O3 O 0.6382(4) 0.2830(2) 1.4093(2) 0.1098(8) Uani 1 1 d .
O4 O 0.9889(3) 1.11510(17) 1.19826(14) 0.0566(4) Uani 1 1 d .
O5 O 1.0319(3) 0.86766(18) 1.19816(14) 0.0585(4) Uani 1 1 d .
O6 O 1.2243(3) 1.0771(2) 1.09708(16) 0.0671(5) Uani 1 1 d .
N1 N 0.2094(3) 0.4446(2) 1.13303(17) 0.0474(5) Uani 1 1 d D
H1N H 0.129(4) 0.3429(19) 1.153(2) 0.071 Uiso 1 1 d D
N2 N 0.7596(3) 0.86142(19) 1.37775(14) 0.0371(4) Uani 1 1 d D
H2N1 H 0.832(3) 0.875(2) 1.3166(15) 0.056 Uiso 1 1 d D
H2N2 H 0.745(4) 0.7597(17) 1.4052(18) 0.056 Uiso 1 1 d D
N3 N 0.7156(3) 0.4401(2) 1.39470(18) 0.0574(5) Uani 1 1 d .
N4 N 1.0857(3) 1.0205(2) 1.16330(15) 0.0454(4) Uani 1 1 d .
C1 C 0.3003(3) 0.5618(2) 1.23131(18) 0.0424(5) Uani 1 1 d .
H1 H 0.2780 0.5290 1.3120 0.051 Uiso 1 1 calc R
C2 C 0.4272(3) 0.7314(2) 1.21424(16) 0.0365(4) Uani 1 1 d .
C3 C 0.4535(3) 0.7755(2) 1.09247(17) 0.0402(5) Uani 1 1 d .
H3 H 0.5392 0.8894 1.0784 0.048 Uiso 1 1 calc R
C4 C 0.3535(3) 0.6518(3) 0.99169(17) 0.0449(5) Uani 1 1 d .
H4 H 0.3682 0.6819 0.9096 0.054 Uiso 1 1 calc R
C5 C 0.2329(3) 0.4845(3) 1.01458(19) 0.0462(5) Uani 1 1 d .
H5 H 0.1674 0.3986 0.9482 0.055 Uiso 1 1 calc R
C6 C 0.5356(3) 0.8623(3) 1.32544(18) 0.0445(5) Uani 1 1 d .
H6A H 0.5482 0.9782 1.2996 0.053 Uiso 1 1 calc R
H6B H 0.4456 0.8340 1.3903 0.053 Uiso 1 1 calc R
C7 C 0.8838(3) 0.9982(2) 1.48095(17) 0.0421(5) Uani 1 1 d .
H7A H 0.8104 0.9744 1.5531 0.051 Uiso 1 1 calc R
H7B H 0.8878 1.1114 1.4530 0.051 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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 N1 C5 122.68(16) . .
C1 N1 H1N 113.5(18) . .
C5 N1 H1N 123.7(18) . .
C7 N2 C6 113.09(14) . .
C7 N2 H2N1 110.1(15) . .
C6 N2 H2N1 108.3(15) . .
C7 N2 H2N2 109.5(14) . .
C6 N2 H2N2 108.5(15) . .
H2N1 N2 H2N2 107.1(13) . .
O1 N3 O3 122.6(2) . .
O1 N3 O2 117.28(19) . .
O3 N3 O2 120.1(2) . .
O6 N4 O5 121.99(17) . .
O6 N4 O4 120.52(16) . .
O5 N4 O4 117.48(16) . .
N1 C1 C2 120.21(17) . .
N1 C1 H1 119.9 . .
C2 C1 H1 119.9 . .
C1 C2 C3 118.07(17) . .
C1 C2 C6 120.27(17) . .
C3 C2 C6 121.66(16) . .
C4 C3 C2 120.48(17) . .
C4 C3 H3 119.8 . .
C2 C3 H3 119.8 . .
C5 C4 C3 118.89(18) . .
C5 C4 H4 120.6 . .
C3 C4 H4 120.6 . .
N1 C5 C4 119.65(18) . .
N1 C5 H5 120.2 . .
C4 C5 H5 120.2 . .
N2 C6 C2 110.22(14) . .
N2 C6 H6A 109.6 . .
C2 C6 H6A 109.6 . .
N2 C6 H6B 109.6 . .
C2 C6 H6B 109.6 . .
H6A C6 H6B 108.1 . .
N2 C7 C7 109.93(18) . 2_778
N2 C7 H7A 109.7 . .
C7 C7 H7A 109.7 2_778 .
N2 C7 H7B 109.7 . .
C7 C7 H7B 109.7 2_778 .
H7A C7 H7B 108.2 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
O1 N3 1.211(3) .
O2 N3 1.244(2) .
O3 N3 1.225(3) .
O4 N4 1.264(2) .
O5 N4 1.252(2) .
O6 N4 1.219(2) .
N1 C1 1.328(3) .
N1 C5 1.338(3) .
N1 H1N 0.86(3) .
N2 C7 1.476(2) .
N2 C6 1.492(2) .
N2 H2N1 0.86(3) .
N2 H2N2 0.86(3) .
C1 C2 1.374(3) .
C1 H1 0.9300 .
C2 C3 1.384(2) .
C2 C6 1.497(3) .
C3 C4 1.381(3) .
C3 H3 0.9300 .
C4 C5 1.364(3) .
C4 H4 0.9300 .
C5 H5 0.9300 .
C6 H6A 0.9700 .
C6 H6B 0.9700 .
C7 C7 1.508(4) 2_778
C7 H7A 0.9700 .
C7 H7B 0.9700 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N1 H1N O4 0.86(3) 1.873(11) 2.730(2) 172(3) 1_445
N2 H2N1 O5 0.86(3) 2.003(11) 2.852(2) 166.2(18) .
N2 H2N1 O4 0.86(3) 2.361(14) 3.020(2) 133.2(16) .
N2 H2N2 O2 0.86(3) 1.931(10) 2.790(2) 172(2) .
N2 H2N2 O1 0.86(3) 2.505(17) 3.126(3) 129.4(15) .
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_4
C5 N1 C1 C2 -1.0(3) .
N1 C1 C2 C3 1.0(3) .
N1 C1 C2 C6 -178.07(16) .
C1 C2 C3 C4 0.3(3) .
C6 C2 C3 C4 179.31(16) .
C2 C3 C4 C5 -1.6(3) .
C1 N1 C5 C4 -0.4(3) .
C3 C4 C5 N1 1.6(3) .
C7 N2 C6 C2 175.06(15) .
C1 C2 C6 N2 89.7(2) .
C3 C2 C6 N2 -89.3(2) .
C6 N2 C7 C7 -173.88(19) 2_778
