#------------------------------------------------------------------------------
#$Date: 2016-03-25 13:16:52 +0200 (Fri, 25 Mar 2016) $
#$Revision: 179835 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/31/7013199.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_7013199
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(L5)]'
_chemical_formula_sum            'C15 H23 Cl2 N3 O2 Zn'
_chemical_formula_weight         413.63
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.9906(7)
_cell_length_b                   16.3898(10)
_cell_length_c                   20.4387(12)
_cell_measurement_reflns_used    5226
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28
_cell_measurement_theta_min      2.5
_cell_volume                     3681.7(4)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.946
_diffrn_measurement_device_type  'Bruker SMART APEX'
_diffrn_measurement_method       Omega
_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  0.0499
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            22085
_diffrn_reflns_theta_full        28.89
_diffrn_reflns_theta_max         28.89
_diffrn_reflns_theta_min         1.99
_exptl_absorpt_coefficient_mu    1.635
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   Sadabs
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.492
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.585
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.218
_refine_ls_hydrogen_treatment    'riding/refall (H7N)'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     212
_refine_ls_number_reflns         4586
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.218
_refine_ls_R_factor_all          0.0691
_refine_ls_R_factor_gt           0.0581
_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)+(0.0421P)²+3.2380P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1141
_refine_ls_wR_factor_ref         0.1183
_reflns_number_gt                3980
_reflns_number_total             4586
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b305476b.txt
_cod_data_source_block           r3687
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Orthorhombic' changed to 'orthorhombic'
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_H-M      Pbca
_cod_database_code               7013199
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, 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 0.77896(3) 0.10512(2) 0.579283(17) 0.02090(12) Uani 1 1 d . . .
N1 N 0.8307(2) 0.01142(16) 0.64287(12) 0.0217(5) Uani 1 1 d . . .
C1 C 0.7283(3) -0.0469(2) 0.63651(15) 0.0253(7) Uani 1 1 d . . .
H1A H 0.6587 -0.0272 0.6629 0.030 Uiso 1 1 calc R . .
H1B H 0.7535 -0.1006 0.6541 0.030 Uiso 1 1 calc R . .
C1OC C 0.6620(3) 0.2511(2) 0.39614(18) 0.0312(8) Uani 1 1 d . . .
H1OA H 0.6904 0.3025 0.3771 0.047 Uiso 1 1 calc R . .
H1OB H 0.7128 0.2370 0.4339 0.047 Uiso 1 1 calc R . .
H1OC H 0.5772 0.2570 0.4102 0.047 Uiso 1 1 calc R . .
C1OA C 0.8030(3) 0.1742(2) 0.3220(2) 0.0388(9) Uani 1 1 d . . .
H1OD H 0.8319 0.2263 0.3044 0.058 Uiso 1 1 calc R . .
H1OE H 0.8074 0.1322 0.2880 0.058 Uiso 1 1 calc R . .
H1OF H 0.8541 0.1581 0.3592 0.058 Uiso 1 1 calc R . .
Cl1 Cl 0.91542(8) 0.15225(5) 0.50765(4) 0.02629(18) Uani 1 1 d . . .
Cl2 Cl 0.66159(9) 0.19389(6) 0.62884(4) 0.0373(2) Uani 1 1 d . . .
N2 N 0.6960(2) 0.01062(15) 0.52894(12) 0.0192(5) Uani 1 1 d . . .
C2 C 0.6887(3) -0.05681(19) 0.56630(15) 0.0222(6) Uani 1 1 d . . .
C3 C 0.6419(3) -0.12892(19) 0.54291(17) 0.0245(7) Uani 1 1 d . . .
H3A H 0.6405 -0.1765 0.5694 0.029 Uiso 1 1 calc R . .
C4 C 0.5970(3) -0.13017(19) 0.47981(17) 0.0263(7) Uani 1 1 d . . .
H4A H 0.5610 -0.1786 0.4632 0.032 Uiso 1 1 calc R . .
C5 C 0.6037(3) -0.06176(19) 0.44056(16) 0.0247(7) Uani 1 1 d . . .
H5A H 0.5734 -0.0624 0.3970 0.030 Uiso 1 1 calc R . .
C6 C 0.6563(3) 0.00781(18) 0.46681(14) 0.0196(6) Uani 1 1 d . . .
N7 N 0.6756(3) 0.08005(17) 0.43168(13) 0.0224(6) Uani 1 1 d . . .
H7N H 0.723(3) 0.108(2) 0.4471(19) 0.024(10) Uiso 1 1 d . . .
O8 O 0.5556(2) 0.05817(14) 0.34339(11) 0.0285(5) Uani 1 1 d . . .
C8 C 0.6269(3) 0.10118(19) 0.37249(15) 0.0213(6) Uani 1 1 d . . .
C9 C 0.6708(3) 0.18339(19) 0.34493(16) 0.0249(7) Uani 1 1 d . . .
C10B C 0.5895(4) 0.2052(2) 0.28678(17) 0.0397(9) Uani 1 1 d . . .
H10A H 0.6156 0.2575 0.2683 0.059 Uiso 1 1 calc R . .
H10B H 0.5049 0.2094 0.3014 0.059 Uiso 1 1 calc R . .
H10C H 0.5961 0.1626 0.2533 0.059 Uiso 1 1 calc R . .
C11 C 0.8421(3) 0.0365(2) 0.71275(15) 0.0274(7) Uani 1 1 d . . .
H11A H 0.8507 -0.0125 0.7407 0.033 Uiso 1 1 calc R . .
H11B H 0.7681 0.0662 0.7265 0.033 Uiso 1 1 calc R . .
C12 C 0.9521(3) 0.0906(2) 0.72062(18) 0.0353(8) Uani 1 1 d . . .
H12A H 0.9416 0.1402 0.6935 0.042 Uiso 1 1 calc R . .
H12B H 0.9586 0.1079 0.7669 0.042 Uiso 1 1 calc R . .
O13 O 1.0609(2) 0.05045(17) 0.70196(13) 0.0399(6) Uani 1 1 d . . .
C14 C 1.0529(3) 0.0275(2) 0.63498(19) 0.0354(9) Uani 1 1 d . . .
H14A H 1.1290 -0.0005 0.6219 0.043 Uiso 1 1 calc R . .
H14B H 1.0446 0.0772 0.6077 0.043 Uiso 1 1 calc R . .
C15 C 0.9460(3) -0.0283(2) 0.62240(18) 0.0282(7) Uani 1 1 d . . .
H15A H 0.9420 -0.0418 0.5752 0.034 Uiso 1 1 calc R . .
H15B H 0.9570 -0.0798 0.6470 0.034 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 83.06(10) . . ?
N2 Zn Cl2 117.82(7) . . ?
N1 Zn Cl2 111.12(8) . . ?
N2 Zn Cl1 103.22(7) . . ?
N1 Zn Cl1 118.62(8) . . ?
Cl2 Zn Cl1 117.93(4) . . ?
C1 N1 C15 109.9(3) . . ?
C1 N1 C11 109.0(2) . . ?
C15 N1 C11 108.6(3) . . ?
C1 N1 Zn 102.28(19) . . ?
C15 N1 Zn 112.27(19) . . ?
C11 N1 Zn 114.6(2) . . ?
N1 C1 C2 111.9(2) . . ?
N1 C1 H1A 109.2 . . ?
C2 C1 H1A 109.2 . . ?
N1 C1 H1B 109.2 . . ?
C2 C1 H1B 109.2 . . ?
H1A C1 H1B 107.9 . . ?
C9 C1OC H1OA 109.5 . . ?
C9 C1OC H1OB 109.5 . . ?
H1OA C1OC H1OB 109.5 . . ?
C9 C1OC H1OC 109.5 . . ?
H1OA C1OC H1OC 109.5 . . ?
H1OB C1OC H1OC 109.5 . . ?
C9 C1OA H1OD 109.5 . . ?
C9 C1OA H1OE 109.5 . . ?
H1OD C1OA H1OE 109.5 . . ?
C9 C1OA H1OF 109.5 . . ?
H1OD C1OA H1OF 109.5 . . ?
H1OE C1OA H1OF 109.5 . . ?
C6 N2 C2 119.3(3) . . ?
C6 N2 Zn 129.7(2) . . ?
C2 N2 Zn 111.0(2) . . ?
N2 C2 C3 122.1(3) . . ?
N2 C2 C1 115.7(3) . . ?
C3 C2 C1 122.1(3) . . ?
C2 C3 C4 118.1(3) . . ?
C2 C3 H3A 120.9 . . ?
C4 C3 H3A 120.9 . . ?
C3 C4 C5 120.8(3) . . ?
C3 C4 H4A 119.6 . . ?
C5 C4 H4A 119.6 . . ?
C4 C5 C6 117.7(3) . . ?
C4 C5 H5A 121.1 . . ?
C6 C5 H5A 121.1 . . ?
N2 C6 C5 122.0(3) . . ?
N2 C6 N7 114.0(3) . . ?
C5 C6 N7 124.1(3) . . ?
C8 N7 C6 127.4(3) . . ?
C8 N7 H7N 119(3) . . ?
C6 N7 H7N 114(3) . . ?
O8 C8 N7 122.7(3) . . ?
O8 C8 C9 122.3(3) . . ?
N7 C8 C9 115.0(3) . . ?
C1OC C9 C10B 109.0(3) . . ?
C1OC C9 C1OA 109.9(3) . . ?
C10B C9 C1OA 109.8(3) . . ?
C1OC C9 C8 111.4(3) . . ?
C10B C9 C8 107.8(3) . . ?
C1OA C9 C8 108.8(3) . . ?
C9 C10B H10A 109.5 . . ?
C9 C10B H10B 109.5 . . ?
H10A C10B H10B 109.5 . . ?
C9 C10B H10C 109.5 . . ?
H10A C10B H10C 109.5 . . ?
H10B C10B H10C 109.5 . . ?
N1 C11 C12 109.4(3) . . ?
N1 C11 H11A 109.8 . . ?
C12 C11 H11A 109.8 . . ?
N1 C11 H11B 109.8 . . ?
C12 C11 H11B 109.8 . . ?
H11A C11 H11B 108.2 . . ?
O13 C12 C11 112.0(3) . . ?
O13 C12 H12A 109.2 . . ?
C11 C12 H12A 109.2 . . ?
O13 C12 H12B 109.2 . . ?
C11 C12 H12B 109.2 . . ?
H12A C12 H12B 107.9 . . ?
C12 O13 C14 109.2(3) . . ?
O13 C14 C15 111.8(3) . . ?
O13 C14 H14A 109.3 . . ?
C15 C14 H14A 109.3 . . ?
O13 C14 H14B 109.3 . . ?
C15 C14 H14B 109.3 . . ?
H14A C14 H14B 107.9 . . ?
N1 C15 C14 110.5(3) . . ?
N1 C15 H15A 109.5 . . ?
C14 C15 H15A 109.5 . . ?
N1 C15 H15B 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 108.1 . . ?
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 2.071(3) . ?
Zn N1 2.091(3) . ?
Zn Cl2 2.1924(9) . ?
Zn Cl1 2.2338(9) . ?
N1 C1 1.481(4) . ?
N1 C15 1.485(4) . ?
N1 C11 1.491(4) . ?
C1 C2 1.508(4) . ?
C1 H1A 0.9900 . ?
C1 H1B 0.9900 . ?
C1OC C9 1.528(5) . ?
C1OC H1OA 0.9800 . ?
C1OC H1OB 0.9800 . ?
C1OC H1OC 0.9800 . ?
C1OA C9 1.534(5) . ?
C1OA H1OD 0.9800 . ?
C1OA H1OE 0.9800 . ?
C1OA H1OF 0.9800 . ?
N2 C6 1.344(4) . ?
N2 C2 1.346(4) . ?
C2 C3 1.375(4) . ?
C3 C4 1.381(5) . ?
C3 H3A 0.9500 . ?
C4 C5 1.381(5) . ?
C4 H4A 0.9500 . ?
C5 C6 1.386(4) . ?
C5 H5A 0.9500 . ?
C6 N7 1.401(4) . ?
N7 C8 1.368(4) . ?
N7 H7N 0.76(4) . ?
O8 C8 1.210(4) . ?
C8 C9 1.538(4) . ?
C9 C10B 1.529(5) . ?
C10B H10A 0.9800 . ?
C10B H10B 0.9800 . ?
C10B H10C 0.9800 . ?
C11 C12 1.508(5) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C12 O13 1.417(5) . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
O13 C14 1.422(5) . ?
C14 C15 1.511(5) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
