#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/32/2233260.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_2233260
loop_
_publ_author_name
'Wang, Wen-Zhen'
'Ismayilov, Rayyat Huseyn'
'Lee, Gene-Hsiang'
'Wen, Yuh-Sheng'
'Peng, Shie-Ming'
_publ_section_title
;
 Bis(morpholin-4-ium) tetrachloridocobalt(II)
;
_journal_coeditor_code           PK2366
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m51
_journal_paper_doi               10.1107/S1600536811053128
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '(C4 H10 N O)2 [Co Cl4]'
_chemical_formula_moiety         '2(C4 H10 N O +), Cl4 Co 2-'
_chemical_formula_sum            'C8 H20 Cl4 Co N2 O2'
_chemical_formula_weight         376.99
_chemical_name_systematic
;
Bis(morpholin-4-ium) tetrachloridocobalt(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.064(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.7545(5)
_cell_length_b                   15.0283(8)
_cell_length_c                   10.4785(5)
_cell_measurement_reflns_used    2047
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.03
_cell_measurement_theta_min      2.37
_cell_volume                     1532.22(13)
_computing_cell_refinement       'SAINT (Bruker, 2007)'
_computing_data_collection       'SMART (Bruker, 2007)'
_computing_data_reduction        'SAINT (Bruker, 2007)'
_computing_molecular_graphics    'XP in SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_measurement_device_type  'Bruker SMART APEX CCD area-detector'
_diffrn_measurement_method       'φ and ω 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  0.0472
_diffrn_reflns_av_sigmaI/netI    0.0520
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            10714
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.07
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.809
_exptl_absorpt_correction_T_max  0.899
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2001)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.634
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.319
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.886
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2661
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.886
_refine_ls_R_factor_all          0.0531
_refine_ls_R_factor_gt           0.0302
_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)+(0.0120P)²+2.9504P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0523
_refine_ls_wR_factor_ref         0.0586
_reflns_number_gt                2001
_reflns_number_total             2661
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            pk2366.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2233260
_cod_database_fobs_code          2233260
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Co Co 0.68020(4) 0.58131(3) 0.71185(4) 0.01425(11) Uani d . 1 1
Cl Cl1 0.49824(8) 0.64671(5) 0.79526(7) 0.01891(18) Uani d . 1 1
Cl Cl2 0.70544(8) 0.43579(5) 0.76441(7) 0.02066(19) Uani d . 1 1
Cl Cl3 0.87551(8) 0.65335(5) 0.78680(7) 0.01802(18) Uani d . 1 1
Cl Cl4 0.65461(8) 0.60624(5) 0.49825(7) 0.01990(19) Uani d . 1 1
O O1 0.0543(2) 0.71540(14) 0.4880(2) 0.0254(6) Uani d . 1 1
N N1 0.3114(2) 0.62863(16) 0.5349(2) 0.0180(6) Uani d . 1 1
H H1A 0.3245 0.5998 0.4592 0.022 Uiso calc R 1 1
H H1B 0.3855 0.6164 0.5914 0.022 Uiso calc R 1 1
C C1 0.1733(3) 0.7481(2) 0.4313(3) 0.0251(8) Uani d . 1 1
H H1C 0.1655 0.8134 0.4207 0.030 Uiso calc R 1 1
H H1D 0.1780 0.7213 0.3454 0.030 Uiso calc R 1 1
C C2 0.3035(3) 0.7266(2) 0.5115(3) 0.0196(7) Uani d . 1 1
H H2C 0.3842 0.7463 0.4667 0.024 Uiso calc R 1 1
H H2D 0.3043 0.7586 0.5942 0.024 Uiso calc R 1 1
C C3 0.1836(3) 0.5950(2) 0.5878(3) 0.0177(7) Uani d . 1 1
H H3A 0.1749 0.6202 0.6742 0.021 Uiso calc R 1 1
H H3B 0.1876 0.5293 0.5954 0.021 Uiso calc R 1 1
C C4 0.0621(3) 0.6215(2) 0.5008(3) 0.0224(8) Uani d . 1 1
H H4A 0.0697 0.5943 0.4155 0.027 Uiso calc R 1 1
H H4B -0.0230 0.5990 0.5356 0.027 Uiso calc R 1 1
O O2 0.7598(2) 0.98715(13) 0.6677(2) 0.0219(5) Uani d . 1 1
N N2 0.8070(3) 0.81133(16) 0.5829(2) 0.0182(6) Uani d . 1 1
H H2A 0.8219 0.7525 0.6039 0.022 Uiso calc R 1 1
H H2B 0.8078 0.8167 0.4955 0.022 Uiso calc R 1 1
C C5 0.8865(3) 0.9630(2) 0.6206(3) 0.0259(8) Uani d . 1 1
H H5A 0.9605 1.0003 0.6622 0.031 Uiso calc R 1 1
H H5B 0.8830 0.9745 0.5274 0.031 Uiso calc R 1 1
C C6 0.9189(3) 0.8666(2) 0.6456(3) 0.0257(8) Uani d . 1 1
H H6A 1.0076 0.8511 0.6108 0.031 Uiso calc R 1 1
H H6B 0.9267 0.8550 0.7388 0.031 Uiso calc R 1 1
C C7 0.6702(3) 0.8394(2) 0.6240(3) 0.0196(7) Uani d . 1 1
H H7A 0.6639 0.8255 0.7157 0.024 Uiso calc R 1 1
H H7B 0.5964 0.8066 0.5742 0.024 Uiso calc R 1 1
C C8 0.6522(3) 0.9378(2) 0.6026(3) 0.0232(8) Uani d . 1 1
H H8A 0.6505 0.9505 0.5099 0.028 Uiso calc R 1 1
H H8B 0.5630 0.9567 0.6332 0.028 Uiso calc R 1 1
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
Cl1 Co Cl2 113.65(3)
Cl1 Co Cl4 106.01(3)
Cl2 Co Cl4 113.73(3)
Cl1 Co Cl3 108.68(3)
Cl2 Co Cl3 107.50(3)
Cl4 Co Cl3 107.00(3)
C1 O1 C4 109.9(2)
C3 N1 C2 111.2(2)
C3 N1 H1A 109.4
C2 N1 H1A 109.4
C3 N1 H1B 109.4
C2 N1 H1B 109.4
H1A N1 H1B 108.0
O1 C1 C2 111.9(2)
O1 C1 H1C 109.2
C2 C1 H1C 109.2
O1 C1 H1D 109.2
C2 C1 H1D 109.2
H1C C1 H1D 107.9
N1 C2 C1 109.5(2)
N1 C2 H2C 109.8
C1 C2 H2C 109.8
N1 C2 H2D 109.8
C1 C2 H2D 109.8
H2C C2 H2D 108.2
N1 C3 C4 109.3(2)
N1 C3 H3A 109.8
C4 C3 H3A 109.8
N1 C3 H3B 109.8
C4 C3 H3B 109.8
H3A C3 H3B 108.3
O1 C4 C3 111.0(3)
O1 C4 H4A 109.4
C3 C4 H4A 109.4
O1 C4 H4B 109.4
C3 C4 H4B 109.4
H4A C4 H4B 108.0
C8 O2 C5 109.5(2)
C6 N2 C7 111.0(2)
C6 N2 H2A 109.4
C7 N2 H2A 109.4
C6 N2 H2B 109.4
C7 N2 H2B 109.4
H2A N2 H2B 108.0
O2 C5 C6 111.5(3)
O2 C5 H5A 109.3
C6 C5 H5A 109.3
O2 C5 H5B 109.3
C6 C5 H5B 109.3
H5A C5 H5B 108.0
N2 C6 C5 108.8(3)
N2 C6 H6A 109.9
C5 C6 H6A 109.9
N2 C6 H6B 109.9
C5 C6 H6B 109.9
H6A C6 H6B 108.3
N2 C7 C8 109.4(2)
N2 C7 H7A 109.8
C8 C7 H7A 109.8
N2 C7 H7B 109.8
C8 C7 H7B 109.8
H7A C7 H7B 108.2
O2 C8 C7 111.6(3)
O2 C8 H8A 109.3
C7 C8 H8A 109.3
O2 C8 H8B 109.3
C7 C8 H8B 109.3
H8A C8 H8B 108.0
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co Cl1 2.2583(8)
Co Cl2 2.2644(8)
Co Cl4 2.2656(8)
Co Cl3 2.2818(8)
O1 C1 1.428(4)
O1 C4 1.419(4)
N1 C3 1.488(4)
N1 C2 1.494(4)
N1 H1A 0.9200
N1 H1B 0.9200
C1 C2 1.507(4)
C1 H1C 0.9900
C1 H1D 0.9900
C2 H2C 0.9900
C2 H2D 0.9900
C3 C4 1.498(4)
C3 H3A 0.9900
C3 H3B 0.9900
C4 H4A 0.9900
C4 H4B 0.9900
O2 C8 1.420(4)
O2 C5 1.410(4)
N2 C6 1.486(4)
N2 C7 1.492(4)
N2 H2A 0.9200
N2 H2B 0.9200
C5 C6 1.503(4)
C5 H5A 0.9900
C5 H5B 0.9900
C6 H6A 0.9900
C6 H6B 0.9900
C7 C8 1.503(4)
C7 H7A 0.9900
C7 H7B 0.9900
C8 H8A 0.9900
C8 H8B 0.9900
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A Cl2 3_666 0.92 2.40 3.275(3) 158.5
N1 H1B Cl1 . 0.92 2.38 3.184(2) 146.4
N2 H2A Cl3 . 0.92 2.45 3.232(3) 142.3
N2 H2B Cl3 4_575 0.92 2.37 3.264(3) 163.1
C2 H2C Cl1 4_575 0.99 2.71 3.603(3) 150.5
C3 H3B Cl4 3_666 0.99 2.77 3.556(3) 136.3
C5 H5A Cl3 2_756 0.99 2.83 3.767(3) 158.0
