#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2007426.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2007426
loop_
_publ_author_name
'Parvez, M.'
'Sabir, A. P.'
_publ_section_title
;
 Doxylaminium Tetrachlorozincate(II) and Doxylaminium
 Tetrachlorocobaltate(II)
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              933
_journal_page_last               935
_journal_volume                  54
_journal_year                    1998
_chemical_formula_analytical     'C17 H24 N2 O 2+, Zn Cl4 2-'
_chemical_formula_iupac          '(C17 H24 N2 O) [Zn Cl4]'
_chemical_formula_moiety         'C17 H24 N2 O 2+, Zn Cl4 2-'
_chemical_formula_sum            'C17 H24 Cl4 N2 O Zn'
_chemical_formula_weight         479.58
_chemical_name_common            'Doxylamine tetrachlorozincate(II)'
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00
_cell_angle_beta                 107.536(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5604(15)
_cell_length_b                   18.2218(17)
_cell_length_c                   12.782(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293.0(10)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      20.0
_cell_volume                     2123.2(7)
_computing_cell_refinement       'CAD-4 Software'
_computing_data_collection       'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1994)'
_computing_molecular_graphics
'TEXSAN (Molecular Structure Corporation, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SAPI91 (Fan, 1991)'
_diffrn_ambient_temperature      293.0(10)
_diffrn_measurement_device       'Enraf-Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0557
_diffrn_reflns_av_sigmaI/netI    0.0402
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            4079
_diffrn_reflns_theta_max         68.00
_diffrn_reflns_theta_min         5.0
_diffrn_standards_decay_%        1.12
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.301
_exptl_absorpt_correction_T_max  0.32
_exptl_absorpt_correction_T_min  0.29
_exptl_absorpt_correction_type   'empirical (North et al., 1968)'
_exptl_absorpt_process_details   '\y scan (3 reflections)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.500
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.626
_refine_diff_density_min         -0.487
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment
'H atoms geometrically idealized with C-H and N-H 0.95 \%A'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     227
_refine_ls_number_reflns         3852
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+( 0.054P)^2^+1.605P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                2927
_reflns_number_total             3852
_reflns_threshold_expression     I>2\s(I)
_[local]_cod_data_source_file    fg1429.cif
_[local]_cod_data_source_block   1
_[local]_cod_cif_authors_sg_H-M  'P 21/n     '
_cod_original_cell_volume        2123.3(7)
_cod_database_code               2007426
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y+1/2, z-1/2'
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Zn1 0.83893(5) 0.38719(3) 0.72756(4) 0.03871(15) Uani d . 1 Zn
Cl1 0.64886(11) 0.45356(6) 0.75069(9) 0.0595(3) Uani d . 1 Cl
Cl2 0.91646(12) 0.29540(5) 0.85367(8) 0.0558(3) Uani d . 1 Cl
Cl3 0.75256(11) 0.33754(6) 0.55514(7) 0.0509(3) Uani d . 1 Cl
Cl4 1.02927(11) 0.46236(6) 0.73998(8) 0.0525(3) Uani d . 1 Cl
O1 0.5188(3) 0.23172(13) 0.66225(19) 0.0399(6) Uani d . 1 O
N1 0.4124(3) 0.34568(16) 0.5574(2) 0.0440(7) Uani d . 1 N
N2 0.6675(3) 0.14009(15) 0.5620(2) 0.0371(7) Uani d . 1 N
C1 0.3723(5) 0.4030(2) 0.4891(3) 0.0560(11) Uani d . 1 C
C2 0.2331(6) 0.4303(2) 0.4682(4) 0.0668(13) Uani d . 1 C
C3 0.1376(6) 0.3976(3) 0.5146(4) 0.0703(14) Uani d . 1 C
C4 0.1817(5) 0.3387(2) 0.5836(4) 0.0626(12) Uani d . 1 C
C5 0.3234(4) 0.3129(2) 0.6056(3) 0.0434(9) Uani d . 1 C
C6 0.3882(4) 0.2528(2) 0.6883(3) 0.0412(8) Uani d . 1 C
C7 0.2855(4) 0.1869(2) 0.6739(3) 0.0412(8) Uani d . 1 C
C8 0.2426(5) 0.1574(2) 0.7587(4) 0.0595(11) Uani d . 1 C
C9 0.1631(5) 0.0927(3) 0.7440(5) 0.0722(14) Uani d . 1 C
C10 0.1270(5) 0.0572(3) 0.6461(5) 0.0668(13) Uani d . 1 C
C11 0.1651(4) 0.0862(2) 0.5595(4) 0.0563(11) Uani d . 1 C
C12 0.2437(4) 0.1514(2) 0.5732(3) 0.0444(9) Uani d . 1 C
C13 0.4280(5) 0.2881(2) 0.8021(3) 0.0621(12) Uani d . 1 C
C14 0.6081(4) 0.1769(2) 0.7305(3) 0.0449(9) Uani d . 1 C
C15 0.7275(4) 0.1602(2) 0.6799(3) 0.0446(9) Uani d . 1 C
C16 0.5852(5) 0.0701(2) 0.5447(3) 0.0521(10) Uani d . 1 C
C17 0.7827(5) 0.1369(3) 0.5079(4) 0.0687(13) Uani d . 1 C
H1 0.5095 0.3275 0.5722 0.073(3) Uiso calc R 1 H
H2 0.6009 0.1776 0.5269 0.073(3) Uiso calc R 1 H
H1A 0.4391 0.4242 0.4558 0.073(3) Uiso calc R 1 H
H2A 0.2032 0.4717 0.4218 0.073(3) Uiso calc R 1 H
H3 0.0403 0.4158 0.4990 0.073(3) Uiso calc R 1 H
H4 0.1154 0.3160 0.6159 0.073(3) Uiso calc R 1 H
H8 0.2677 0.1816 0.8277 0.073(3) Uiso calc R 1 H
H9 0.1337 0.0730 0.8029 0.073(3) Uiso calc R 1 H
H10 0.0750 0.0121 0.6375 0.073(3) Uiso calc R 1 H
H11 0.1379 0.0619 0.4906 0.073(3) Uiso calc R 1 H
H12 0.2692 0.1719 0.5130 0.073(3) Uiso calc R 1 H
H13A 0.4692 0.2520 0.8564 0.073(3) Uiso calc R 1 H
H13B 0.3421 0.3078 0.8141 0.073(3) Uiso calc R 1 H
H13C 0.4972 0.3262 0.8066 0.073(3) Uiso calc R 1 H
H14A 0.5521 0.1342 0.7324 0.073(3) Uiso calc R 1 H
H14B 0.6486 0.1947 0.8032 0.073(3) Uiso calc R 1 H
H15A 0.7891 0.2019 0.6867 0.073(3) Uiso calc R 1 H
H15B 0.7856 0.1209 0.7187 0.073(3) Uiso calc R 1 H
H16A 0.5108 0.0724 0.5799 0.073(3) Uiso calc R 1 H
H16B 0.6504 0.0309 0.5748 0.073(3) Uiso calc R 1 H
H16C 0.5415 0.0622 0.4684 0.073(3) Uiso calc R 1 H
H17A 0.8354 0.1818 0.5191 0.073(3) Uiso calc R 1 H
H17B 0.7393 0.1290 0.4315 0.073(3) Uiso calc R 1 H
H17C 0.8479 0.0977 0.5381 0.073(3) Uiso calc R 1 H
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_12
_atom_site_aniso_U_13
_atom_site_aniso_U_23
Zn1 0.0406(3) 0.0378(3) 0.0351(3) -0.0035(2) 0.00724(19) -0.0040(2)
Cl1 0.0483(6) 0.0562(6) 0.0748(7) -0.0016(5) 0.0197(5) -0.0225(5)
Cl2 0.0731(7) 0.0429(5) 0.0372(5) -0.0123(5) -0.0050(4) -0.0007(4)
Cl3 0.0562(6) 0.0605(6) 0.0328(4) -0.0097(5) 0.0086(4) -0.0072(4)
Cl4 0.0469(5) 0.0548(6) 0.0540(6) -0.0140(4) 0.0125(4) -0.0020(5)
O1 0.0406(13) 0.0399(13) 0.0376(13) 0.0032(11) 0.0094(11) 0.0080(11)
N1 0.0446(17) 0.0392(17) 0.0431(18) -0.0011(14) 0.0056(14) 0.0010(14)
N2 0.0376(16) 0.0320(14) 0.0375(16) 0.0022(12) 0.0047(13) 0.0034(12)
C1 0.069(3) 0.043(2) 0.047(2) -0.004(2) 0.005(2) 0.0042(19)
C2 0.086(4) 0.043(2) 0.059(3) 0.020(2) 0.004(3) 0.005(2)
C3 0.073(3) 0.063(3) 0.072(3) 0.030(3) 0.017(3) -0.005(3)
C4 0.059(3) 0.059(3) 0.075(3) 0.016(2) 0.028(2) -0.005(2)
C5 0.053(2) 0.038(2) 0.042(2) 0.0031(17) 0.0177(18) -0.0061(16)
C6 0.052(2) 0.042(2) 0.0335(18) 0.0004(17) 0.0180(17) -0.0031(16)
C7 0.043(2) 0.046(2) 0.0385(19) 0.0054(17) 0.0183(16) 0.0022(16)
C8 0.062(3) 0.071(3) 0.050(2) -0.004(2) 0.025(2) 0.006(2)
C9 0.058(3) 0.082(4) 0.083(4) -0.008(3) 0.030(3) 0.028(3)
C10 0.045(2) 0.054(3) 0.096(4) -0.007(2) 0.014(3) 0.011(3)
C11 0.041(2) 0.058(3) 0.067(3) -0.002(2) 0.011(2) -0.004(2)
C12 0.040(2) 0.051(2) 0.044(2) -0.0012(17) 0.0152(16) -0.0010(17)
C13 0.082(3) 0.062(3) 0.044(2) -0.004(2) 0.022(2) -0.013(2)
C14 0.051(2) 0.041(2) 0.0364(19) -0.0006(17) 0.0030(16) 0.0044(16)
C15 0.039(2) 0.041(2) 0.045(2) -0.0014(16) -0.0016(16) 0.0003(17)
C16 0.059(3) 0.037(2) 0.052(2) -0.0082(19) 0.0031(19) -0.0005(18)
C17 0.059(3) 0.072(3) 0.084(3) -0.004(2) 0.035(3) -0.011(3)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zn Zn -1.5491 0.6778 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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_publ_flag
Cl4 Zn1 Cl1 109.19(4) n
Cl4 Zn1 Cl2 108.23(4) n
Cl1 Zn1 Cl2 113.54(5) n
Cl4 Zn1 Cl3 110.98(4) n
Cl1 Zn1 Cl3 105.32(4) n
Cl2 Zn1 Cl3 109.59(4) n
C14 O1 C6 116.5(3) y
C5 N1 C1 123.6(4) y
C16 N2 C15 112.9(3) y
C17 N2 C15 111.9(3) y
C17 N2 C16 109.7(3) y
N1 C1 C2 118.7(4) n
C3 C2 C1 119.7(4) n
C2 C3 C4 120.2(5) n
C3 C4 C5 119.4(5) n
N1 C5 C4 118.4(4) n
N1 C5 C6 117.5(3) n
C4 C5 C6 123.9(4) n
O1 C6 C5 103.4(3) n
O1 C6 C7 109.5(3) n
C5 C6 C7 111.7(3) n
O1 C6 C13 110.4(3) n
C5 C6 C13 106.9(3) n
C7 C6 C13 114.3(3) n
C8 C7 C12 118.4(4) n
C8 C7 C6 123.1(4) n
C12 C7 C6 118.3(3) n
C7 C8 C9 120.5(4) n
C10 C9 C8 120.5(4) n
C9 C10 C11 120.3(4) n
C10 C11 C12 119.6(4) n
C11 C12 C7 120.6(4) n
O1 C14 C15 105.7(3) n
N2 C15 C14 112.0(3) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Zn1 Cl1 2.2750(11) y
Zn1 Cl2 2.2858(11) y
Zn1 Cl3 2.2936(11) y
Zn1 Cl4 2.2447(11) y
O1 C6 1.437(4) y
O1 C14 1.427(4) y
N1 C1 1.341(5) y
N1 C5 1.333(5) y
N2 C15 1.488(4) y
N2 C16 1.479(4) y
N2 C17 1.467(5) y
C1 C2 1.369(6) n
C2 C3 1.365(7) n
C3 C4 1.372(6) n
C4 C5 1.381(6) n
C5 C6 1.518(5) n
C6 C7 1.526(5) n
C6 C13 1.530(5) n
C7 C8 1.379(5) n
C7 C12 1.388(5) n
C8 C9 1.384(6) n
C9 C10 1.357(7) n
C10 C11 1.371(6) n
C11 C12 1.388(5) n
C14 C15 1.503(5) n
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_D
_geom_hbond_site_symmetry_H
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_publ_flag
N1 H1 Cl3 1_555 1_555 1_555 0.95 2.41 3.265(5) 150 y
N2 H2 Cl2 1_555 1_555 4_555 0.95 2.43 3.222(4) 141 y
N1 H1 O1 1_555 1_555 1_555 0.95 2.08 2.513(6) 106 y
N2 H2 O1 1_555 1_555 1_555 0.95 2.32 2.748(7) 107 y
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_publ_flag
C5 N1 C1 C2 0.9(6) n
N1 C1 C2 C3 -1.8(7) n
C1 C2 C3 C4 1.4(7) n
C2 C3 C4 C5 0.0(7) n
C1 N1 C5 C4 0.5(6) n
C1 N1 C5 C6 -175.0(3) n
C3 C4 C5 N1 -0.9(6) n
C3 C4 C5 C6 174.3(4) n
C14 O1 C6 C5 177.6(3) n
C14 O1 C6 C7 -63.1(4) n
C14 O1 C6 C13 63.5(4) n
N1 C5 C6 O1 -19.3(4) n
C4 C5 C6 O1 165.4(4) n
N1 C5 C6 C7 -137.1(3) n
C4 C5 C6 C7 47.7(5) n
N1 C5 C6 C13 97.2(4) n
C4 C5 C6 C13 -78.0(5) n
O1 C6 C7 C8 118.8(4) n
C5 C6 C7 C8 -127.2(4) n
C13 C6 C7 C8 -5.6(6) n
O1 C6 C7 C12 -55.5(4) n
C5 C6 C7 C12 58.5(4) n
C13 C6 C7 C12 -179.9(3) n
C12 C7 C8 C9 1.7(6) n
C6 C7 C8 C9 -172.5(4) n
C7 C8 C9 C10 0.3(7) n
C8 C9 C10 C11 -1.9(7) n
C9 C10 C11 C12 1.3(7) n
C10 C11 C12 C7 0.8(6) n
C8 C7 C12 C11 -2.3(6) n
C6 C7 C12 C11 172.2(3) n
C6 O1 C14 C15 174.8(3) n
C17 N2 C15 C14 169.6(3) n
C16 N2 C15 C14 -66.1(4) n
O1 C14 C15 N2 -53.9(4) n