#------------------------------------------------------------------------------
#$Date: 2019-03-05 09:52:05 +0100 (mar 05 de mar de 2019) $
#$Revision: 213973 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/05/7050569.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_7050569
loop_
_publ_author_name
'Patra, Goutam Kumar'
'Goldberg, Israel'
_publ_section_title
;
 The synthesis and characterization of a series of bis-bidentate Schiff
 base ligands and their coordination complexes with silver(i),
 copper(i) and zinc(ii) d10 metal ionsElectronic supplementary
 information (ESI) available: Views of the crystal structures of
 ligands of 1, 2 and 3. See http://www.rsc.org/suppdata/nj/b3/b301632c/
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1124
_journal_paper_doi               10.1039/b301632c
_journal_volume                  27
_journal_year                    2003
_chemical_formula_moiety         'C26 H18 N4 . 2(C H Cl3)'
_chemical_formula_sum            'C28 H20 Cl6 N4'
_chemical_formula_weight         625.18
_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                70.9570(9)
_cell_angle_beta                 77.6140(9)
_cell_angle_gamma                84.1600(15)
_cell_formula_units_Z            1
_cell_length_a                   6.23400(10)
_cell_length_b                   9.3440(2)
_cell_length_c                   12.6120(3)
_cell_measurement_reflns_used    2712
_cell_measurement_temperature    110(2)
_cell_measurement_theta_max      28.17
_cell_measurement_theta_min      3.30
_cell_volume                     677.89(2)
_computing_cell_refinement       Denzo
_computing_data_collection       'Collect, Nonius B.V.'
_computing_data_reduction        Denzo
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR-92
_diffrn_ambient_temperature      110(2)
_diffrn_detector_area_resol_mean '56 microns'
_diffrn_measured_fraction_theta_full 0.948
_diffrn_measured_fraction_theta_max 0.948
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '1 deg. Phi & 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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0410
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3162
_diffrn_reflns_theta_full        28.17
_diffrn_reflns_theta_max         28.17
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.661
_exptl_absorpt_correction_T_max  0.9368
_exptl_absorpt_correction_T_min  0.7552
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rods
_exptl_crystal_F_000             318
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.333
_refine_diff_density_rms         0.055
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     172
_refine_ls_number_reflns         3162
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.0397
_refine_ls_R_factor_gt           0.0313
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0196P)²+0.3897P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0739
_refine_ls_wR_factor_ref         0.0784
_reflns_number_gt                2712
_reflns_number_total             3162
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b301632c.txt
_cod_data_source_block           Ligand-3
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7050569
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Cl1 Cl 0.48844(7) -0.35172(5) 0.29672(4) 0.03013(12) Uani 1 1 d . . .
Cl2 Cl 0.85229(6) -0.34823(5) 0.40607(4) 0.02757(11) Uani 1 1 d . . .
Cl3 Cl 0.41822(7) -0.23591(5) 0.48915(4) 0.03290(12) Uani 1 1 d . . .
N1 N 0.70500(18) 0.09804(13) 0.22539(10) 0.0144(2) Uani 1 1 d . . .
C2 C 0.8573(2) 0.17248(16) 0.24992(12) 0.0138(3) Uani 1 1 d . . .
C3 C 0.9814(2) 0.08953(17) 0.33323(12) 0.0171(3) Uani 1 1 d . . .
H3 H 0.9569 -0.0151 0.3712 0.020 Uiso 1 1 calc R . .
C5 C 1.1747(2) 0.31479(17) 0.30442(13) 0.0195(3) Uani 1 1 d . . .
H5 H 1.2814 0.3623 0.3240 0.023 Uiso 1 1 calc R . .
C4 C 1.1373(2) 0.15939(17) 0.35958(13) 0.0190(3) Uani 1 1 d . . .
H4 H 1.2204 0.1025 0.4154 0.023 Uiso 1 1 calc R . .
C6 C 1.0577(2) 0.39782(17) 0.22256(13) 0.0183(3) Uani 1 1 d . . .
H6 H 1.0847 0.5024 0.1855 0.022 Uiso 1 1 calc R . .
C7 C 0.8971(2) 0.32882(16) 0.19282(12) 0.0148(3) Uani 1 1 d . . .
C8 C 0.7760(2) 0.40717(16) 0.10628(13) 0.0173(3) Uani 1 1 d . . .
H8 H 0.7960 0.5120 0.0670 0.021 Uiso 1 1 calc R . .
C9 C 0.6306(2) 0.33029(16) 0.08022(13) 0.0166(3) Uani 1 1 d . . .
H9 H 0.5525 0.3799 0.0205 0.020 Uiso 1 1 calc R . .
C10 C 0.5975(2) 0.17540(15) 0.14337(12) 0.0139(3) Uani 1 1 d . . .
C11 C 0.4370(2) 0.09025(16) 0.11981(12) 0.0154(3) Uani 1 1 d . . .
H11 H 0.4228 -0.0148 0.1600 0.018 Uiso 1 1 calc R . .
N12 N 0.31665(18) 0.15512(13) 0.04622(10) 0.0151(2) Uani 1 1 d . . .
C13 C 0.1596(2) 0.07097(16) 0.02697(12) 0.0134(3) Uani 1 1 d . . .
C14 C 0.0947(2) -0.07487(16) 0.09507(12) 0.0162(3) Uani 1 1 d . . .
H14 H 0.1579 -0.1263 0.1601 0.019 Uiso 1 1 calc R . .
C15 C -0.0620(2) -0.14404(16) 0.06730(12) 0.0156(3) Uani 1 1 d . . .
H15 H -0.1040 -0.2435 0.1135 0.019 Uiso 1 1 calc R . .
C16 C 0.6069(2) -0.25400(17) 0.36797(13) 0.0205(3) Uani 1 1 d . . .
H16 H 0.6430 -0.1502 0.3144 0.025 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'
Cl Cl 0.1484 0.1585 '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'
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
_geom_angle_publ_flag
C10 N1 C2 117.85(12) . . ?
N1 C2 C3 118.52(12) . . ?
N1 C2 C7 122.24(12) . . ?
C3 C2 C7 119.23(12) . . ?
C4 C3 C2 120.41(13) . . ?
C4 C3 H3 119.8 . . ?
C2 C3 H3 119.8 . . ?
C6 C5 C4 120.34(13) . . ?
C6 C5 H5 119.8 . . ?
C4 C5 H5 119.8 . . ?
C3 C4 C5 120.49(13) . . ?
C3 C4 H4 119.8 . . ?
C5 C4 H4 119.8 . . ?
C5 C6 C7 120.53(14) . . ?
C5 C6 H6 119.7 . . ?
C7 C6 H6 119.7 . . ?
C6 C7 C8 123.24(13) . . ?
C6 C7 C2 119.00(13) . . ?
C8 C7 C2 117.75(12) . . ?
C9 C8 C7 119.29(13) . . ?
C9 C8 H8 120.4 . . ?
C7 C8 H8 120.4 . . ?
C8 C9 C10 119.16(13) . . ?
C8 C9 H9 120.4 . . ?
C10 C9 H9 120.4 . . ?
N1 C10 C9 123.66(13) . . ?
N1 C10 C11 115.75(12) . . ?
C9 C10 C11 120.59(12) . . ?
N12 C11 C10 121.15(13) . . ?
N12 C11 H11 119.4 . . ?
C10 C11 H11 119.4 . . ?
C11 N12 C13 119.99(12) . . ?
C15 C13 C14 118.72(12) 2 . ?
C15 C13 N12 115.72(12) 2 . ?
C14 C13 N12 125.55(13) . . ?
C15 C14 C13 119.79(13) . . ?
C15 C14 H14 120.1 . . ?
C13 C14 H14 120.1 . . ?
C14 C15 C13 121.49(13) . 2 ?
C14 C15 H15 119.3 . . ?
C13 C15 H15 119.3 2 . ?
Cl3 C16 Cl2 111.01(8) . . ?
Cl3 C16 Cl1 110.28(8) . . ?
Cl2 C16 Cl1 110.38(8) . . ?
Cl3 C16 H16 108.4 . . ?
Cl2 C16 H16 108.4 . . ?
Cl1 C16 H16 108.4 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Cl1 C16 1.7731(16) . ?
Cl2 C16 1.7640(15) . ?
Cl3 C16 1.7620(16) . ?
N1 C10 1.3240(18) . ?
N1 C2 1.3717(17) . ?
C2 C3 1.4137(19) . ?
C2 C7 1.4230(19) . ?
C3 C4 1.375(2) . ?
C3 H3 0.9500 . ?
C5 C6 1.373(2) . ?
C5 C4 1.410(2) . ?
C5 H5 0.9500 . ?
C4 H4 0.9500 . ?
C6 C7 1.4176(19) . ?
C6 H6 0.9500 . ?
C7 C8 1.420(2) . ?
C8 C9 1.364(2) . ?
C8 H8 0.9500 . ?
C9 C10 1.4177(19) . ?
C9 H9 0.9500 . ?
C10 C11 1.4714(18) . ?
C11 N12 1.2773(18) . ?
C11 H11 0.9500 . ?
N12 C13 1.4208(17) . ?
C13 C15 1.3948(19) 2 ?
C13 C14 1.399(2) . ?
C14 C15 1.3848(19) . ?
C14 H14 0.9500 . ?
C15 C13 1.3948(19) 2 ?
C15 H15 0.9500 . ?
C16 H16 1.0000 . ?
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
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C10 N1 C2 C3 -176.84(13) . . . . ?
C10 N1 C2 C7 1.9(2) . . . . ?
N1 C2 C3 C4 179.35(13) . . . . ?
C7 C2 C3 C4 0.6(2) . . . . ?
C2 C3 C4 C5 0.4(2) . . . . ?
C6 C5 C4 C3 -0.9(2) . . . . ?
C4 C5 C6 C7 0.4(2) . . . . ?
C5 C6 C7 C8 -177.81(14) . . . . ?
C5 C6 C7 C2 0.6(2) . . . . ?
N1 C2 C7 C6 -179.78(13) . . . . ?
C3 C2 C7 C6 -1.1(2) . . . . ?
N1 C2 C7 C8 -1.3(2) . . . . ?
C3 C2 C7 C8 177.42(13) . . . . ?
C6 C7 C8 C9 177.46(14) . . . . ?
C2 C7 C8 C9 -1.0(2) . . . . ?
C7 C8 C9 C10 2.5(2) . . . . ?
C2 N1 C10 C9 -0.2(2) . . . . ?
C2 N1 C10 C11 179.61(12) . . . . ?
C8 C9 C10 N1 -2.0(2) . . . . ?
C8 C9 C10 C11 178.17(13) . . . . ?
N1 C10 C11 N12 176.71(13) . . . . ?
C9 C10 C11 N12 -3.4(2) . . . . ?
C10 C11 N12 C13 -178.60(12) . . . . ?
C11 N12 C13 C15 -169.84(13) . . . 2 ?
C11 N12 C13 C14 11.4(2) . . . . ?
C15 C13 C14 C15 0.7(2) 2 . . . ?
N12 C13 C14 C15 179.45(13) . . . . ?
C13 C14 C15 C13 -0.7(2) . . . 2 ?
