#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/31/7013197.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_7013197
loop_
_publ_author_name
'Juan C. Mareque Rivas'
'Emiliano Salvagni'
'Rafael Torres Martín de Rosales'
'Simon Parsons'
_publ_section_title
;
 Internal hydrogen bonding in tetrahedral and trigonal bipyramidal
 zinc(II) complexes of pyridine-based ligands
;
_journal_issue                   17
_journal_name_full               'Dalton Trans.'
_journal_page_first              3339
_journal_page_last               3349
_journal_paper_doi               10.1039/b305476b
_journal_year                    2003
_chemical_formula_moiety         '[ZnCl2(L3)]MeCN'
_chemical_formula_sum            'C18 H29 Cl2 N5 O Zn'
_chemical_formula_weight         467.73
_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/difmap (H7N)'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.773(2)
_cell_angle_beta                 100.503(2)
_cell_angle_gamma                92.944(2)
_cell_formula_units_Z            2
_cell_length_a                   7.9950(13)
_cell_length_b                   10.2286(16)
_cell_length_c                   14.220(2)
_cell_measurement_reflns_used    6880
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29
_cell_measurement_theta_min      2.5
_cell_volume                     1114.6(3)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.889
_diffrn_measured_fraction_theta_max 0.889
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       'Omega and Phi'
_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  0.0229
_diffrn_reflns_av_sigmaI/netI    0.0336
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9678
_diffrn_reflns_theta_full        28.69
_diffrn_reflns_theta_max         28.69
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.721
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.394
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.81
_exptl_crystal_size_mid          0.76
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.745
_refine_diff_density_min         -0.334
_refine_diff_density_rms         0.070
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    'riding/refall (H7N)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         5113
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0363
_refine_ls_R_factor_gt           0.0322
_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)+(0.0498P)²+0.2635P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0848
_refine_ls_wR_factor_ref         0.0874
_reflns_number_gt                4582
_reflns_number_total             5113
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305476b.txt
_cod_data_source_block           r2769
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_exptl_absorpt_correction_type' value 'Multiscan' changed to
'multi-scan' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_Hall     ' -P 1'
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7013197
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
Zn Zn 0.75131(2) 0.858960(19) 0.721130(13) 0.02574(8) Uani 1 1 d . . .
Cl1 Cl 0.81771(7) 0.65043(5) 0.68905(3) 0.04247(13) Uani 1 1 d . . .
N1 N 0.59876(18) 0.93514(13) 0.81980(10) 0.0241(3) Uani 1 1 d . . .
C1 C 0.5064(2) 1.02875(17) 0.76673(13) 0.0293(4) Uani 1 1 d . . .
H1A H 0.5849 1.1085 0.7704 0.035 Uiso 1 1 calc R . .
H1B H 0.4107 1.0593 0.7985 0.035 Uiso 1 1 calc R . .
Cl2 Cl 0.94873(6) 1.02721(6) 0.73624(3) 0.04315(13) Uani 1 1 d . . .
N2 N 0.53744(17) 0.87641(13) 0.61784(10) 0.0228(3) Uani 1 1 d . . .
C2 C 0.4376(2) 0.96276(16) 0.66097(12) 0.0250(3) Uani 1 1 d . . .
C3 C 0.2871(2) 0.99422(17) 0.60987(13) 0.0291(3) Uani 1 1 d . . .
H3A H 0.2179 1.0545 0.6416 0.035 Uiso 1 1 calc R . .
C4 C 0.2394(2) 0.93578(18) 0.51119(13) 0.0296(4) Uani 1 1 d . . .
H4A H 0.1369 0.9570 0.4742 0.036 Uiso 1 1 calc R . .
C5 C 0.3394(2) 0.84690(17) 0.46606(13) 0.0267(3) Uani 1 1 d . . .
H5A H 0.3070 0.8061 0.3983 0.032 Uiso 1 1 calc R . .
C6 C 0.4891(2) 0.81848(15) 0.52231(12) 0.0225(3) Uani 1 1 d . . .
N7 N 0.59893(18) 0.72839(14) 0.48596(10) 0.0243(3) Uani 1 1 d . . .
H7N H 0.666(3) 0.702(2) 0.5277(17) 0.031(5) Uiso 1 1 d . . .
O8 O 0.50774(17) 0.70932(13) 0.32270(9) 0.0316(3) Uani 1 1 d . . .
C8 C 0.6034(2) 0.67729(15) 0.38888(11) 0.0227(3) Uani 1 1 d . . .
C9 C 0.7387(2) 0.57969(16) 0.37207(12) 0.0239(3) Uani 1 1 d . . .
C1OA C 0.7313(3) 0.5377(2) 0.26231(13) 0.0351(4) Uani 1 1 d . . .
H1OA H 0.7568 0.6168 0.2366 0.053 Uiso 1 1 calc R . .
H1OB H 0.6167 0.4959 0.2298 0.053 Uiso 1 1 calc R . .
H1OC H 0.8156 0.4733 0.2498 0.053 Uiso 1 1 calc R . .
C10B C 0.6990(3) 0.45591(18) 0.41242(14) 0.0336(4) Uani 1 1 d . . .
H10D H 0.5849 0.4135 0.3794 0.050 Uiso 1 1 calc R . .
H10E H 0.7026 0.4832 0.4830 0.050 Uiso 1 1 calc R . .
H10F H 0.7840 0.3920 0.4006 0.050 Uiso 1 1 calc R . .
C10C C 0.9167(2) 0.64816(19) 0.42239(15) 0.0355(4) Uani 1 1 d . . .
H10A H 0.9398 0.7268 0.3957 0.053 Uiso 1 1 calc R . .
H10B H 1.0027 0.5851 0.4106 0.053 Uiso 1 1 calc R . .
H10C H 0.9213 0.6764 0.4930 0.053 Uiso 1 1 calc R . .
C11 C 0.6981(2) 1.01264(17) 0.91589(12) 0.0281(3) Uani 1 1 d . . .
H11A H 0.6209 1.0650 0.9527 0.034 Uiso 1 1 calc R . .
H11B H 0.7862 1.0763 0.9048 0.034 Uiso 1 1 calc R . .
C12 C 0.7828(2) 0.91829(18) 0.97505(12) 0.0296(4) Uani 1 1 d . . .
H12A H 0.8620 0.8673 0.9388 0.035 Uiso 1 1 calc R . .
H12B H 0.8502 0.9706 1.0382 0.035 Uiso 1 1 calc R . .
N13 N 0.65457(19) 0.82547(14) 0.99344(10) 0.0271(3) Uani 1 1 d . . .
C13 C 0.7327(3) 0.7370(2) 1.05393(14) 0.0387(4) Uani 1 1 d . . .
H13A H 0.7965 0.7910 1.1164 0.058 Uiso 1 1 calc R . .
H13B H 0.8107 0.6836 1.0198 0.058 Uiso 1 1 calc R . .
H13C H 0.6433 0.6771 1.0662 0.058 Uiso 1 1 calc R . .
C14 C 0.5590(2) 0.74581(17) 0.89998(12) 0.0286(3) Uani 1 1 d . . .
H14A H 0.4722 0.6820 0.9121 0.034 Uiso 1 1 calc R . .
H14B H 0.6378 0.6934 0.8644 0.034 Uiso 1 1 calc R . .
C15 C 0.4721(2) 0.83620(17) 0.83813(12) 0.0269(3) Uani 1 1 d . . .
H15A H 0.4093 0.7811 0.7748 0.032 Uiso 1 1 calc R . .
H15B H 0.3883 0.8844 0.8721 0.032 Uiso 1 1 calc R . .
N1S N 0.7970(4) 0.3655(3) 1.0085(2) 0.0810(8) Uani 1 1 d . . .
C1S C 0.8183(3) 0.3808(2) 0.9344(2) 0.0491(5) Uani 1 1 d . . .
C2S C 0.8503(3) 0.3998(3) 0.84126(18) 0.0540(6) Uani 1 1 d . . .
H2SA H 0.9322 0.4786 0.8518 0.092(11) Uiso 1 1 calc R . .
H2SB H 0.7430 0.4136 0.8001 0.092(11) Uiso 1 1 calc R . .
H2SC H 0.8973 0.3203 0.8086 0.081(10) 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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn 0.2839 1.4301 '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
N2 Zn N1 82.90(6) . . ?
N2 Zn Cl1 108.21(4) . . ?
N1 Zn Cl1 125.43(4) . . ?
N2 Zn Cl2 109.86(4) . . ?
N1 Zn Cl2 104.00(4) . . ?
Cl1 Zn Cl2 119.91(3) . . ?
C1 N1 C15 108.98(14) . . ?
C1 N1 C11 109.00(13) . . ?
C15 N1 C11 108.75(12) . . ?
C1 N1 Zn 100.16(10) . . ?
C15 N1 Zn 115.90(10) . . ?
C11 N1 Zn 113.53(10) . . ?
N1 C1 C2 111.24(13) . . ?
N1 C1 H1A 109.4 . . ?
C2 C1 H1A 109.4 . . ?
N1 C1 H1B 109.4 . . ?
C2 C1 H1B 109.4 . . ?
H1A C1 H1B 108.0 . . ?
C6 N2 C2 119.43(14) . . ?
C6 N2 Zn 131.34(11) . . ?
C2 N2 Zn 109.23(10) . . ?
N2 C2 C3 122.04(15) . . ?
N2 C2 C1 115.80(14) . . ?
C3 C2 C1 122.06(15) . . ?
C2 C3 C4 118.25(16) . . ?
C2 C3 H3A 120.9 . . ?
C4 C3 H3A 120.9 . . ?
C5 C4 C3 120.47(16) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C4 C5 C6 118.29(16) . . ?
C4 C5 H5A 120.9 . . ?
C6 C5 H5A 120.9 . . ?
N2 C6 C5 121.52(15) . . ?
N2 C6 N7 114.67(14) . . ?
C5 C6 N7 123.81(15) . . ?
C8 N7 C6 127.14(14) . . ?
C8 N7 H7N 117.3(15) . . ?
C6 N7 H7N 115.5(15) . . ?
O8 C8 N7 121.96(15) . . ?
O8 C8 C9 123.11(15) . . ?
N7 C8 C9 114.92(14) . . ?
C1OA C9 C8 108.18(14) . . ?
C1OA C9 C10C 109.30(15) . . ?
C8 C9 C10C 110.09(13) . . ?
C1OA C9 C10B 109.54(14) . . ?
C8 C9 C10B 109.05(14) . . ?
C10C C9 C10B 110.63(15) . . ?
C9 C1OA H1OA 109.5 . . ?
C9 C1OA H1OB 109.5 . . ?
H1OA C1OA H1OB 109.5 . . ?
C9 C1OA H1OC 109.5 . . ?
H1OA C1OA H1OC 109.5 . . ?
H1OB C1OA H1OC 109.5 . . ?
C9 C10B H10D 109.5 . . ?
C9 C10B H10E 109.5 . . ?
H10D C10B H10E 109.5 . . ?
C9 C10B H10F 109.5 . . ?
H10D C10B H10F 109.5 . . ?
H10E C10B H10F 109.5 . . ?
C9 C10C H10A 109.5 . . ?
C9 C10C H10B 109.5 . . ?
H10A C10C H10B 109.5 . . ?
C9 C10C H10C 109.5 . . ?
H10A C10C H10C 109.5 . . ?
H10B C10C H10C 109.5 . . ?
N1 C11 C12 110.14(14) . . ?
N1 C11 H11A 109.6 . . ?
C12 C11 H11A 109.6 . . ?
N1 C11 H11B 109.6 . . ?
C12 C11 H11B 109.6 . . ?
H11A C11 H11B 108.1 . . ?
N13 C12 C11 110.27(14) . . ?
N13 C12 H12A 109.6 . . ?
C11 C12 H12A 109.6 . . ?
N13 C12 H12B 109.6 . . ?
C11 C12 H12B 109.6 . . ?
H12A C12 H12B 108.1 . . ?
C12 N13 C13 111.31(15) . . ?
C12 N13 C14 109.30(13) . . ?
C13 N13 C14 109.84(14) . . ?
N13 C13 H13A 109.5 . . ?
N13 C13 H13B 109.5 . . ?
H13A C13 H13B 109.5 . . ?
N13 C13 H13C 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
N13 C14 C15 110.31(14) . . ?
N13 C14 H14A 109.6 . . ?
C15 C14 H14A 109.6 . . ?
N13 C14 H14B 109.6 . . ?
C15 C14 H14B 109.6 . . ?
H14A C14 H14B 108.1 . . ?
N1 C15 C14 111.08(14) . . ?
N1 C15 H15A 109.4 . . ?
C14 C15 H15A 109.4 . . ?
N1 C15 H15B 109.4 . . ?
C14 C15 H15B 109.4 . . ?
H15A C15 H15B 108.0 . . ?
N1S C1S C2S 178.4(3) . . ?
C1S C2S H2SA 109.5 . . ?
C1S C2S H2SB 109.5 . . ?
H2SA C2S H2SB 109.5 . . ?
C1S C2S H2SC 109.5 . . ?
H2SA C2S H2SC 109.5 . . ?
H2SB C2S H2SC 109.5 . . ?
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
Zn N2 2.0823(14) . ?
Zn N1 2.0830(14) . ?
Zn Cl1 2.2016(6) . ?
Zn Cl2 2.2238(6) . ?
N1 C1 1.482(2) . ?
N1 C15 1.489(2) . ?
N1 C11 1.491(2) . ?
C1 C2 1.505(2) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
N2 C6 1.342(2) . ?
N2 C2 1.350(2) . ?
C2 C3 1.377(2) . ?
C3 C4 1.383(3) . ?
C3 H3A 0.9500 . ?
C4 C5 1.379(2) . ?
C4 H4A 0.9500 . ?
C5 C6 1.392(2) . ?
C5 H5A 0.9500 . ?
C6 N7 1.393(2) . ?
N7 C8 1.381(2) . ?
N7 H7N 0.83(2) . ?
O8 C8 1.211(2) . ?
C8 C9 1.527(2) . ?
C9 C1OA 1.521(2) . ?
C9 C10C 1.533(2) . ?
C9 C10B 1.535(2) . ?
C1OA H1OA 0.9800 . ?
C1OA H1OB 0.9800 . ?
C1OA H1OC 0.9800 . ?
C10B H10D 0.9800 . ?
C10B H10E 0.9800 . ?
C10B H10F 0.9800 . ?
C10C H10A 0.9800 . ?
C10C H10B 0.9800 . ?
C10C H10C 0.9800 . ?
C11 C12 1.513(2) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 N13 1.456(2) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
N13 C13 1.459(2) . ?
N13 C14 1.462(2) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C14 C15 1.512(2) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
N1S C1S 1.138(4) . ?
C1S C2S 1.443(4) . ?
C2S H2SA 0.9800 . ?
C2S H2SB 0.9800 . ?
C2S H2SC 0.9800 . ?
