#------------------------------------------------------------------------------
#$Date: 2011-09-10 06:16:28 +0300 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/2007427.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_2007427
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+, Co Cl4 2-'
_chemical_formula_iupac          '(C17 H24 N2 O) [Co Cl4]'
_chemical_formula_moiety         'C17 H24 N2 O 2+, Co Cl4 2-'
_chemical_formula_sum            'C17 H24 Cl4 Co N2 O'
_chemical_formula_weight         473.13
_chemical_name_common            'Doxylamine tetrachlorocobaltate(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                 107.313(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.5279(12)
_cell_length_b                   18.229(3)
_cell_length_c                   12.7795(13)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    170.0(10)
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      10.0
_cell_volume                     2119.0(5)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1988)
;
_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      170.0(10)
_diffrn_measurement_device       AFC-6S
_diffrn_measurement_method       '\w/2\q scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.1919
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5172
_diffrn_reflns_theta_max         27.5
_diffrn_reflns_theta_min         2.00
_diffrn_standards_decay_%        0.43
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.322
_exptl_absorpt_correction_T_max  0.81
_exptl_absorpt_correction_T_min  0.63
_exptl_absorpt_correction_type   'empirical (North et al., 1968) '
_exptl_absorpt_process_details   '\y scan (3 reflections)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.483
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             972
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.685
_refine_diff_density_min         -0.574
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.953
_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         4892
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.953
_refine_ls_R_factor_all          0.2150
_refine_ls_R_factor_gt           0.0484
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.066P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_ref         0.1673
_reflns_number_gt                1836
_reflns_number_total             4892
_reflns_threshold_expression     >2sigma(I)
_[local]_cod_data_source_file    fg1429.cif
_[local]_cod_data_source_block   2
_[local]_cod_cif_authors_sg_H-M  'P 21/n     '
_cod_original_cell_volume        2119.1(5)
_cod_database_code               2007427
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
Co1 0.83880(9) 0.38624(5) 0.72772(6) 0.0316(2) Uani d . 1 Co
Cl1 0.64766(19) 0.45348(10) 0.74963(14) 0.0482(5) Uani d . 1 Cl
Cl2 0.9194(2) 0.29487(9) 0.85458(12) 0.0463(5) Uani d . 1 Cl
Cl3 0.75288(18) 0.33718(10) 0.55459(12) 0.0416(4) Uani d . 1 Cl
Cl4 1.03089(18) 0.46165(10) 0.74139(13) 0.0439(4) Uani d . 1 Cl
O1 0.5206(4) 0.2320(2) 0.6630(3) 0.0319(10) Uani d . 1 O
N1 0.4119(6) 0.3460(3) 0.5560(4) 0.0368(13) Uani d . 1 N
N2 0.6692(5) 0.1400(3) 0.5626(4) 0.0298(12) Uani d . 1 N
C1 0.3703(8) 0.4041(4) 0.4876(5) 0.0451(18) Uani d . 1 C
C2 0.2313(8) 0.4305(4) 0.4650(6) 0.051(2) Uani d . 1 C
C3 0.1349(9) 0.3980(4) 0.5140(6) 0.057(2) Uani d . 1 C
C4 0.1795(9) 0.3386(4) 0.5825(6) 0.0530(19) Uani d . 1 C
C5 0.3211(7) 0.3131(3) 0.6042(5) 0.0335(15) Uani d . 1 C
C6 0.3866(7) 0.2523(4) 0.6880(5) 0.0327(15) Uani d . 1 C
C7 0.2853(7) 0.1866(4) 0.6733(5) 0.0364(16) Uani d . 1 C
C8 0.2410(8) 0.1573(4) 0.7578(6) 0.0498(19) Uani d . 1 C
C9 0.1632(8) 0.0912(4) 0.7435(6) 0.055(2) Uani d . 1 C
C10 0.1290(8) 0.0552(4) 0.6459(7) 0.056(2) Uani d . 1 C
C11 0.1657(7) 0.0852(4) 0.5594(6) 0.0430(17) Uani d . 1 C
C12 0.2447(7) 0.1506(4) 0.5726(5) 0.0385(16) Uani d . 1 C
C13 0.4241(9) 0.2882(4) 0.8016(5) 0.055(2) Uani d . 1 C
C14 0.6105(7) 0.1782(3) 0.7321(5) 0.0355(15) Uani d . 1 C
C15 0.7284(7) 0.1600(3) 0.6810(5) 0.0345(15) Uani d . 1 C
C16 0.5853(7) 0.0701(3) 0.5465(5) 0.0411(17) Uani d . 1 C
C17 0.7868(8) 0.1369(4) 0.5097(6) 0.054(2) Uani d . 1 C
H1 0.5092 0.3278 0.5705 0.049(4) Uiso calc R 1 H
H2 0.6030 0.1777 0.5275 0.049(4) Uiso calc R 1 H
H1A 0.4381 0.4263 0.4558 0.049(4) Uiso calc R 1 H
H2A 0.2003 0.4706 0.4162 0.049(4) Uiso calc R 1 H
H3 0.0381 0.4168 0.5003 0.049(4) Uiso calc R 1 H
H4 0.1129 0.3155 0.6145 0.049(4) Uiso calc R 1 H
H8 0.2635 0.1822 0.8261 0.049(4) Uiso calc R 1 H
H9 0.1339 0.0713 0.8025 0.049(4) Uiso calc R 1 H
H10 0.0797 0.0092 0.6378 0.049(4) Uiso calc R 1 H
H11 0.1373 0.0613 0.4902 0.049(4) Uiso calc R 1 H
H12 0.2710 0.1707 0.5125 0.049(4) Uiso calc R 1 H
H13A 0.4877 0.3287 0.8044 0.049(4) Uiso calc R 1 H
H13B 0.4715 0.2534 0.8559 0.049(4) Uiso calc R 1 H
H13C 0.3363 0.3047 0.8148 0.049(4) Uiso calc R 1 H
H14A 0.5545 0.1358 0.7363 0.049(4) Uiso calc R 1 H
H14B 0.6521 0.1971 0.8040 0.049(4) Uiso calc R 1 H
H15A 0.7920 0.2010 0.6880 0.049(4) Uiso calc R 1 H
H15B 0.7849 0.1202 0.7197 0.049(4) Uiso calc R 1 H
H16A 0.5102 0.0732 0.5813 0.049(4) Uiso calc R 1 H
H16B 0.6499 0.0309 0.5776 0.049(4) Uiso calc R 1 H
H16C 0.5423 0.0616 0.4703 0.049(4) Uiso calc R 1 H
H17A 0.8390 0.1821 0.5209 0.049(4) Uiso calc R 1 H
H17B 0.7448 0.1287 0.4333 0.049(4) Uiso calc R 1 H
H17C 0.8523 0.0980 0.5406 0.049(4) 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
Co1 0.0324(5) 0.0332(5) 0.0260(4) -0.0031(4) 0.0037(3) -0.0036(4)
Cl1 0.0399(10) 0.0469(11) 0.0562(11) -0.0001(9) 0.0121(8) -0.0175(9)
Cl2 0.0607(11) 0.0372(10) 0.0282(8) -0.0100(9) -0.0066(7) 0.0002(7)
Cl3 0.0450(10) 0.0522(10) 0.0247(7) -0.0071(8) 0.0059(7) -0.0059(7)
Cl4 0.0382(9) 0.0506(11) 0.0411(9) -0.0128(8) 0.0090(7) -0.0026(8)
O1 0.038(3) 0.027(2) 0.031(2) 0.0029(19) 0.0104(19) 0.0068(18)
N1 0.036(3) 0.032(3) 0.036(3) 0.000(3) 0.002(2) -0.003(2)
N2 0.024(3) 0.029(3) 0.032(3) 0.000(2) 0.003(2) 0.003(2)
C1 0.064(5) 0.037(4) 0.027(3) -0.007(4) 0.003(3) 0.005(3)
C2 0.061(5) 0.031(4) 0.047(4) 0.012(4) -0.005(4) 0.004(3)
C3 0.060(5) 0.055(5) 0.056(5) 0.020(4) 0.018(4) -0.002(4)
C4 0.067(5) 0.045(5) 0.050(4) 0.010(4) 0.022(4) 0.001(4)
C5 0.044(4) 0.025(3) 0.031(3) 0.002(3) 0.011(3) -0.010(3)
C6 0.035(4) 0.042(4) 0.023(3) 0.005(3) 0.012(3) -0.001(3)
C7 0.033(4) 0.049(4) 0.030(3) 0.005(3) 0.013(3) 0.001(3)
C8 0.054(4) 0.066(5) 0.036(4) -0.003(4) 0.023(3) 0.001(4)
C9 0.052(5) 0.061(5) 0.057(5) -0.007(4) 0.025(4) 0.018(4)
C10 0.034(4) 0.052(5) 0.078(6) -0.007(4) 0.010(4) 0.012(4)
C11 0.029(4) 0.042(4) 0.056(4) -0.004(3) 0.010(3) -0.004(3)
C12 0.033(4) 0.051(4) 0.031(3) -0.001(3) 0.009(3) -0.001(3)
C13 0.079(6) 0.053(5) 0.034(4) -0.008(4) 0.018(4) -0.010(3)
C14 0.037(4) 0.038(4) 0.027(3) 0.002(3) 0.003(3) 0.004(3)
C15 0.032(3) 0.032(4) 0.030(3) 0.000(3) -0.005(3) -0.001(3)
C16 0.048(4) 0.035(4) 0.034(3) -0.010(3) 0.003(3) -0.003(3)
C17 0.051(5) 0.061(5) 0.055(5) -0.004(4) 0.026(4) -0.002(4)
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'
Co Co 0.3494 0.9721 '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 Co1 Cl1 108.81(7) n
Cl4 Co1 Cl2 107.16(7) n
Cl1 Co1 Cl2 114.55(8) n
Cl4 Co1 Cl3 111.11(7) n
Cl1 Co1 Cl3 104.98(7) n
Cl2 Co1 Cl3 110.27(7) n
C14 O1 C6 116.4(4) y
C5 N1 C1 122.7(6) y
C16 N2 C15 112.0(5) y
C17 N2 C15 111.4(5) y
C17 N2 C16 110.8(5) y
C2 C1 N1 119.6(7) n
C1 C2 C3 119.2(7) n
C4 C3 C2 120.1(7) n
C5 C4 C3 119.5(7) n
N1 C5 C4 118.9(6) n
N1 C5 C6 117.2(6) n
C4 C5 C6 123.7(6) n
O1 C6 C7 109.9(5) n
O1 C6 C13 110.1(5) n
C7 C6 C13 114.5(5) n
O1 C6 C5 103.4(5) n
C7 C6 C5 111.8(5) n
C13 C6 C5 106.5(5) n
C8 C7 C12 118.4(6) n
C8 C7 C6 122.8(6) n
C12 C7 C6 118.6(5) n
C7 C8 C9 120.4(7) n
C10 C9 C8 120.6(7) n
C9 C10 C11 119.9(7) n
C10 C11 C12 120.2(7) n
C7 C12 C11 120.4(6) n
O1 C14 C15 105.9(5) n
N2 C15 C14 113.0(5) n
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 Cl1 2.2806(19) y
Co1 Cl2 2.2916(18) y
Co1 Cl3 2.2994(16) y
Co1 Cl4 2.2538(18) y
O1 C14 1.423(7) y
O1 C6 1.453(7) y
N1 C1 1.356(8) y
N1 C5 1.343(8) y
N2 C15 1.494(7) y
N2 C16 1.486(7) y
N2 C17 1.472(8) y
C1 C2 1.357(9) n
C2 C3 1.389(10) n
C3 C4 1.377(10) n
C4 C5 1.376(9) n
C5 C6 1.538(8) n
C6 C7 1.515(9) n
C6 C13 1.534(8) n
C7 C8 1.378(8) n
C7 C12 1.393(8) n
C8 C9 1.397(10) n
C9 C10 1.362(10) n
C10 C11 1.369(9) n
C11 C12 1.393(9) n
C14 C15 1.495(8) 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 2.40 3.259(7) 151 y
N2 H2 Cl2 1_555 1_555 4_555 0.95 2.43 3.221(6) 141 y
N1 H1 O1 1_555 1_555 1_555 0.95 2.09 2.533(8) 107 y
N2 H2 O1 1_555 1_555 1_555 0.95 2.33 2.747(8) 106 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 -0.8(9) n
N1 C1 C2 C3 1.1(10) n
C1 C2 C3 C4 -1.7(11) n
C2 C3 C4 C5 1.8(11) n
C1 N1 C5 C4 0.8(9) n
C1 N1 C5 C6 -174.5(5) n
C3 C4 C5 N1 -1.3(10) n
C3 C4 C5 C6 173.7(6) n
C14 O1 C6 C7 -63.5(6) n
C14 O1 C6 C13 63.5(7) n
C14 O1 C6 C5 177.0(5) n
N1 C5 C6 O1 -18.5(7) n
C4 C5 C6 O1 166.4(6) n
N1 C5 C6 C7 -136.6(5) n
C4 C5 C6 C7 48.3(8) n
N1 C5 C6 C13 97.6(6) n
C4 C5 C6 C13 -77.5(8) n
O1 C6 C7 C8 119.0(7) n
C13 C6 C7 C8 -5.5(9) n
C5 C6 C7 C8 -126.8(7) n
O1 C6 C7 C12 -55.7(7) n
C13 C6 C7 C12 179.8(6) n
C5 C6 C7 C12 58.5(7) n
C12 C7 C8 C9 3.0(10) n
C6 C7 C8 C9 -171.7(6) n
C7 C8 C9 C10 -0.5(11) n
C8 C9 C10 C11 -2.6(11) n
C9 C10 C11 C12 3.3(10) n
C8 C7 C12 C11 -2.3(10) n
C6 C7 C12 C11 172.6(6) n
C10 C11 C12 C7 -0.9(10) n
C6 O1 C14 C15 172.7(5) n
C17 N2 C15 C14 168.6(5) n
C16 N2 C15 C14 -66.6(6) n
O1 C14 C15 N2 -52.1(6) n