#------------------------------------------------------------------------------
#$Date: 2016-02-20 18:35:30 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176787 $
#$URL: svn://www.crystallography.net/cod/cif/2/21/75/2217539.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_2217539
loop_
_publ_author_name
'Guo, Hang-Ming'
'Li, Hua-Qiong'
'Zhao, Guo-Liang'
'Ng, Seik Weng'
_publ_section_title
;
 Bis(1-adamantylammonium) tetrachloridocobaltate(II)
;
_journal_coeditor_code           HJ2005
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m415
_journal_page_last               m415
_journal_paper_doi               10.1107/S160053680800189X
_journal_volume                  64
_journal_year                    2008
_chemical_formula_iupac          '(C10 H18 N)2 [Co Cl4]'
_chemical_formula_moiety         '2(C10 H18 N +), Cl4 Co1 2-'
_chemical_formula_sum            'C20 H36 Cl4 Co N2'
_chemical_formula_weight         505.24
_chemical_name_systematic
;
Bis(1-adamantylammonium) tetrachloridocobaltate(II)
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 104.0870(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   30.6005(6)
_cell_length_b                   7.30460(10)
_cell_length_c                   11.0009(2)
_cell_measurement_reflns_used    3080
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      22.3
_cell_measurement_theta_min      2.6
_cell_volume                     2385.02(7)
_computing_cell_refinement       'SAINT (Bruker, 2006)'
_computing_data_collection       'APEX2 (not SMART) (Bruker, 2006)'
_computing_data_reduction        'SAINT (Bruker, 2006)'
_computing_molecular_graphics    'X-SEED (Barbour, 2001)'
_computing_publication_material  'publCIF (Westrip, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      295(2)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII area-detector'
_diffrn_measurement_method       'φ and ω'
_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  0.0269
_diffrn_reflns_av_sigmaI/netI    0.0288
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11019
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.91
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.176
_exptl_absorpt_correction_T_max  0.862
_exptl_absorpt_correction_T_min  0.709
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            Blue
_exptl_crystal_density_diffrn    1.407
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1060
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.519
_refine_diff_density_min         -0.492
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     142
_refine_ls_number_reflns         2946
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_gt           0.0406
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0368P)²+2.5214P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0906
_refine_ls_wR_factor_ref         0.0998
_reflns_number_gt                2115
_reflns_number_total             2946
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            hj2005.cif
_cod_data_source_block           I
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               2217539
_cod_database_fobs_code          2217539
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z'
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
N N1 0.18030(9) 0.5000 0.3577(3) 0.0615(9) Uani d S 1
H H1A 0.1921 0.4006 0.3315 0.092 Uiso calc PR 0.50
H H1B 0.1863 0.4999 0.4410 0.092 Uiso calc SR 1
H H1C 0.1921 0.5995 0.3316 0.092 Uiso calc PR 0.50
C C1 0.13007(10) 0.5000 0.3050(3) 0.0452(8) Uani d S 1
C C2 0.11951(12) 0.5000 0.1618(3) 0.0713(13) Uani d S 1
H H2A 0.1324 0.3923 0.1324 0.086 Uiso calc PR 0.50
H H2B 0.1324 0.6077 0.1324 0.086 Uiso calc PR 0.50
C C3 0.06830(12) 0.5000 0.1108(3) 0.0668(12) Uani d S 1
H H3 0.0611 0.5000 0.0190 0.080 Uiso calc SR 1
C C4 0.04858(9) 0.3300(5) 0.1559(2) 0.0737(9) Uani d . 1
H H4A 0.0613 0.2214 0.1271 0.088 Uiso calc R 1
H H4B 0.0162 0.3277 0.1221 0.088 Uiso calc R 1
C C5 0.05938(9) 0.3314(4) 0.2990(2) 0.0650(8) Uani d . 1
H H5 0.0465 0.2222 0.3286 0.078 Uiso calc R 1
C C6 0.11079(8) 0.3304(4) 0.3507(2) 0.0568(7) Uani d . 1
H H6A 0.1181 0.3289 0.4415 0.068 Uiso calc R 1
H H6B 0.1236 0.2219 0.3220 0.068 Uiso calc R 1
C C7 0.03975(12) 0.5000 0.3436(3) 0.0691(12) Uani d S 1
H H7A 0.0463 0.5000 0.4344 0.083 Uiso calc SR 1
H H7B 0.0073 0.5000 0.3116 0.083 Uiso calc SR 1
N N2 0.30310(10) 0.5000 0.1192(3) 0.0888(13) Uani d S 1
H H2C 0.2904 0.5989 0.1431 0.133 Uiso calc PR 0.50
H H2D 0.2905 0.4000 0.1419 0.133 Uiso calc PR 0.50
H H2E 0.2991 0.5011 0.0363 0.133 Uiso calc SR 1
C C8 0.35290(10) 0.5000 0.1809(3) 0.0483(8) Uani d S 1
C C9 0.35959(12) 0.5000 0.3224(3) 0.0530(9) Uani d S 1
H H9A 0.3457 0.6077 0.3484 0.064 Uiso calc PR 0.50
H H9B 0.3457 0.3923 0.3484 0.064 Uiso calc PR 0.50
C C10 0.40942(14) 0.5000 0.3820(3) 0.0678(11) Uani d S 1
H H10 0.4142 0.5000 0.4734 0.081 Uiso calc SR 1
C C11 0.43062(10) 0.3295(5) 0.3422(3) 0.0803(10) Uani d . 1
H H11A 0.4167 0.2212 0.3675 0.096 Uiso calc R 1
H H11B 0.4625 0.3266 0.3826 0.096 Uiso calc R 1
C C12 0.42392(9) 0.3305(4) 0.1996(2) 0.0650(7) Uani d . 1
H H12A 0.4377 0.2208 0.1738 0.078 Uiso calc R 1
C C13 0.37368(9) 0.3305(4) 0.1389(2) 0.0608(7) Uani d . 1
H H13A 0.3687 0.3304 0.0483 0.073 Uiso calc R 1
H H13B 0.3598 0.2216 0.1634 0.073 Uiso calc R 1
C C14 0.44527(13) 0.5000 0.1588(4) 0.0678(11) Uani d S 1
H H14A 0.4774 0.5000 0.1963 0.081 Uiso calc SR 1
H H14B 0.4408 0.5000 0.0684 0.081 Uiso calc SR 1
Co Co1 0.244385(15) 0.0000 0.28152(4) 0.04942(16) Uani d S 1
Cl Cl1 0.22131(2) 0.24581(10) 0.15542(7) 0.0678(2) Uani d . 1
Cl Cl2 0.21345(4) 0.0000 0.44545(11) 0.0907(4) Uani d S 1
Cl Cl3 0.32036(3) 0.0000 0.34080(8) 0.0561(2) Uani d S 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'
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_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
C1 N1 H1A . . 109.5
C1 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
C1 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
N1 C1 C6 . 6_565 108.50(17)
N1 C1 C6 . . 108.50(17)
C6 C1 C6 6_565 . 110.3(3)
N1 C1 C2 . . 109.7(2)
C6 C1 C2 6_565 . 109.94(17)
C6 C1 C2 . . 109.94(17)
C1 C2 C3 . . 108.5(3)
C1 C2 H2A . . 110.0
C3 C2 H2A . . 110.0
C1 C2 H2B . . 110.0
C3 C2 H2B . . 110.0
H2A C2 H2B . . 108.4
C4 C3 C4 6_565 . 110.0(3)
C4 C3 C2 6_565 . 109.49(19)
C4 C3 C2 . . 109.49(19)
C4 C3 H3 6_565 . 109.3
C4 C3 H3 . . 109.3
C2 C3 H3 . . 109.3
C3 C4 C5 . . 109.2(2)
C3 C4 H4A . . 109.8
C5 C4 H4A . . 109.8
C3 C4 H4B . . 109.8
C5 C4 H4B . . 109.8
H4A C4 H4B . . 108.3
C7 C5 C4 . . 109.8(3)
C7 C5 C6 . . 109.7(2)
C4 C5 C6 . . 109.0(2)
C7 C5 H5 . . 109.4
C4 C5 H5 . . 109.4
C6 C5 H5 . . 109.4
C1 C6 C5 . . 108.7(2)
C1 C6 H6A . . 109.9
C5 C6 H6A . . 109.9
C1 C6 H6B . . 109.9
C5 C6 H6B . . 109.9
H6A C6 H6B . . 108.3
C5 C7 C5 . 6_565 109.9(3)
C5 C7 H7A . . 109.7
C5 C7 H7A 6_565 . 109.7
C5 C7 H7B . . 109.7
C5 C7 H7B 6_565 . 109.7
H7A C7 H7B . . 108.2
C8 N2 H2C . . 109.5
C8 N2 H2D . . 109.5
H2C N2 H2D . . 109.5
C8 N2 H2E . . 109.5
H2C N2 H2E . . 109.5
H2D N2 H2E . . 109.5
N2 C8 C13 . . 108.41(19)
N2 C8 C13 . 6_565 108.41(19)
C13 C8 C13 . 6_565 109.6(3)
N2 C8 C9 . . 109.3(3)
C13 C8 C9 . . 110.53(19)
C13 C8 C9 6_565 . 110.53(19)
C10 C9 C8 . . 108.4(3)
C10 C9 H9A . . 110.0
C8 C9 H9A . . 110.0
C10 C9 H9B . . 110.0
C8 C9 H9B . . 110.0
H9A C9 H9B . . 108.4
C9 C10 C11 . . 109.4(2)
C9 C10 C11 . 6_565 109.4(2)
C11 C10 C11 . 6_565 110.3(4)
C9 C10 H10 . . 109.2
C11 C10 H10 . . 109.2
C11 C10 H10 6_565 . 109.2
C10 C11 C12 . . 109.4(2)
C10 C11 H11A . . 109.8
C12 C11 H11A . . 109.8
C10 C11 H11B . . 109.8
C12 C11 H11B . . 109.8
H11A C11 H11B . . 108.2
C14 C12 C13 . . 109.4(3)
C14 C12 C11 . . 110.3(3)
C13 C12 C11 . . 108.6(2)
C14 C12 H12A . . 109.5
C13 C12 H12A . . 109.5
C11 C12 H12A . . 109.5
C8 C13 C12 . . 108.7(2)
C8 C13 H13A . . 109.9
C12 C13 H13A . . 109.9
C8 C13 H13B . . 109.9
C12 C13 H13B . . 109.9
H13A C13 H13B . . 108.3
C12 C14 C12 6_565 . 109.3(3)
C12 C14 H14A 6_565 . 109.8
C12 C14 H14A . . 109.8
C12 C14 H14B 6_565 . 109.8
C12 C14 H14B . . 109.8
H14A C14 H14B . . 108.3
Cl2 Co1 Cl3 . . 112.11(4)
Cl2 Co1 Cl1 . . 111.30(3)
Cl3 Co1 Cl1 . . 108.75(3)
Cl2 Co1 Cl1 . 6 111.30(3)
Cl3 Co1 Cl1 . 6 108.74(3)
Cl1 Co1 Cl1 . 6 104.31(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
N1 C1 . 1.505(4)
N1 H1A . 0.8900
N1 H1B . 0.8900
N1 H1C . 0.8900
C1 C6 6_565 1.509(3)
C1 C6 . 1.509(3)
C1 C2 . 1.530(4)
C2 C3 . 1.530(5)
C2 H2A . 0.9700
C2 H2B . 0.9700
C3 C4 6_565 1.516(4)
C3 C4 . 1.516(4)
C3 H3 . 0.9800
C4 C5 . 1.528(4)
C4 H4A . 0.9700
C4 H4B . 0.9700
C5 C7 . 1.504(4)
C5 C6 . 1.537(3)
C5 H5 . 0.9800
C6 H6A . 0.9700
C6 H6B . 0.9700
C7 C5 6_565 1.504(4)
C7 H7A . 0.9700
C7 H7B . 0.9700
N2 C8 . 1.510(4)
N2 H2C . 0.8900
N2 H2D . 0.8900
N2 H2E . 0.8900
C8 C13 . 1.515(3)
C8 C13 6_565 1.515(3)
C8 C9 . 1.520(4)
C9 C10 . 1.506(5)
C9 H9A . 0.9700
C9 H9B . 0.9700
C10 C11 . 1.517(4)
C10 C11 6_565 1.517(4)
C10 H10 . 0.9800
C11 C12 . 1.531(4)
C11 H11A . 0.9700
C11 H11B . 0.9700
C12 C14 . 1.518(4)
C12 C13 . 1.520(4)
C12 H12A . 0.9800
C13 H13A . 0.9700
C13 H13B . 0.9700
C14 C12 6_565 1.518(4)
C14 H14A . 0.9700
C14 H14B . 0.9700
Co1 Cl2 . 2.2313(11)
Co1 Cl3 . 2.2567(9)
Co1 Cl1 . 2.2738(7)
Co1 Cl1 6 2.2738(7)
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
N2 H2E Cl1 4 0.89 2.72 3.437(3) 138.5
N2 H2E Cl1 4 0.89 2.72 3.437(3) 138.5
N2 H2D Cl1 . 0.89 2.43 3.218(3) 147.2
N2 H2C Cl1 6_565 0.89 2.43 3.218(3) 147.5
N1 H1C Cl1 6_565 0.89 2.58 3.366(2) 147.2
N1 H1B Cl3 7_556 0.89 2.46 3.322(3) 163.7
N1 H1A Cl1 . 0.89 2.58 3.366(2) 147.3
