#------------------------------------------------------------------------------
#$Date: 2015-09-26 05:18:10 +0300 (Sat, 26 Sep 2015) $
#$Revision: 158348 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/10/2241094.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_2241094
loop_
_publ_author_name
'Derbel, Amira'
'Mhiri, Tahar'
'Graia, Mohsen'
_publ_section_title
;
 Etude structurale et vibrationnelle d'un nouveau composé complexe de
 cobalt: [Co(imidazole)₄Cl]Cl
;
_journal_coeditor_code           SU5189
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              1185
_journal_page_last               1189
_journal_paper_doi               10.1107/S2056989015015807
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Co Cl (C3 H4 N2)4]Cl'
_chemical_formula_moiety         'C12 H16 Cl Co N8 +, Cl -'
_chemical_formula_sum            'C12 H16 Cl2 Co N8'
_chemical_formula_weight         402.16
_chemical_name_systematic
;
Chloridotetrakis(1H-imidazole-κN³)cobalt(II) chloride
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 89.998(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.8665(3)
_cell_length_b                   13.3043(6)
_cell_length_c                   13.9154(5)
_cell_measurement_temperature    293(2)
_cell_volume                     1641.50(11)
_computing_cell_refinement
;
SAINT (Bruker, 1998)
;
_computing_data_collection
;
SMART (Bruker, 1998)
;
_computing_data_reduction
;
SAINT (Bruker, 1998)
;
_computing_molecular_graphics
;
DIAMOND  (Brandenburg & Putz, 1999) et PLATON (Spek, 2009)
;
_computing_publication_material
;
WinGX (Farrugia, 2012) et PLATON (Spek, 2009)
;
_computing_structure_refinement
;
SHELXL2013 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART CCD area-detector'
_diffrn_measurement_method       'φ and ω'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0227
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2915
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.048
_diffrn_reflns_theta_min         2.118
_exptl_absorpt_coefficient_mu    1.382
_exptl_absorpt_correction_T_max  0.882
_exptl_absorpt_correction_T_min  0.840
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 1998)
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.627
_exptl_crystal_description       prism
_exptl_crystal_F_000             820
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.399
_refine_diff_density_min         -0.292
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2915
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0305
_refine_ls_R_factor_gt           0.0272
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0400P)²+0.4321P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0705
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                2705
_reflns_number_total             2915
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            su5189sup1.cif
_cod_data_source_block           I
_cod_database_code               2241094
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelxl_version_number           .2013
loop_
_space_group_symop_operation_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_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_occupancy
Co Co1 0.81347(4) 0.21324(2) 0.37752(3) 0.01963(9) Uani d 1
Cl Cl1 1.05621(8) 0.10160(5) 0.37941(7) 0.03569(16) Uani d 1
Cl Cl2 1.44553(8) 0.40796(6) 0.37507(7) 0.03951(17) Uani d 1
N N1 0.9146(3) 0.34849(16) 0.3746(2) 0.0300(5) Uani d 1
C C1 1.0619(3) 0.3624(2) 0.3717(3) 0.0328(6) Uani d 1
H H1 1.1328 0.3109 0.3701 0.039 Uiso calc 1
N N2 1.0955(3) 0.45971(18) 0.3714(2) 0.0401(6) Uani d 1
H H2N 1.1848 0.4849 0.3702 0.048 Uiso calc 1
C C2 0.9645(3) 0.5127(2) 0.3734(3) 0.0435(7) Uani d 1
H H2 0.9539 0.5822 0.3737 0.052 Uiso calc 1
C C3 0.8525(3) 0.4432(2) 0.3748(3) 0.0385(7) Uani d 1
H H3 0.7498 0.4575 0.3757 0.046 Uiso calc 1
N N3 0.8045(4) 0.22115(18) 0.52089(16) 0.0319(6) Uani d 1
C C4 0.8591(4) 0.1555(3) 0.5825(2) 0.0344(9) Uani d 1
H H4 0.9140 0.0985 0.5658 0.041 Uiso calc 1
N N4 0.8246(4) 0.1822(2) 0.67242(18) 0.0415(7) Uani d 1
H H4N 0.8488 0.1499 0.7237 0.050 Uiso calc 1
C C5 0.7453(5) 0.2690(3) 0.6690(2) 0.0443(10) Uani d 1
H H5 0.7074 0.3049 0.7210 0.053 Uiso calc 1
C C6 0.7323(5) 0.2928(3) 0.5757(2) 0.0385(9) Uani d 1
H H6 0.6823 0.3489 0.5518 0.046 Uiso calc 1
N N5 0.8038(3) 0.21234(18) 0.23384(16) 0.0289(5) Uani d 1
C C7 0.8709(4) 0.1515(3) 0.1730(2) 0.0357(9) Uani d 1
H H7 0.9358 0.0996 0.1903 0.043 Uiso calc 1
N N6 0.8326(4) 0.1746(2) 0.08285(18) 0.0391(7) Uani d 1
H H6N 0.8641 0.1450 0.0317 0.047 Uiso calc 1
C C8 0.7344(5) 0.2537(3) 0.0865(2) 0.0417(9) Uani d 1
H H8 0.6885 0.2855 0.0346 0.050 Uiso calc 1
C C9 0.7177(5) 0.2762(2) 0.1793(2) 0.0363(9) Uani d 1
H H9 0.6569 0.3273 0.2033 0.044 Uiso calc 1
N N7 0.6433(3) 0.11427(17) 0.3800(2) 0.0308(5) Uani d 1
C C10 0.4975(3) 0.1353(2) 0.3745(3) 0.0391(7) Uani d 1
H H10 0.4577 0.1999 0.3716 0.047 Uiso calc 1
N N8 0.4150(3) 0.05047(19) 0.3737(3) 0.0429(6) Uani d 1
H H8N 0.3184 0.0467 0.3702 0.051 Uiso calc 1
C C11 0.5122(3) -0.0281(2) 0.3794(3) 0.0444(8) Uani d 1
H H11 0.4874 -0.0960 0.3805 0.053 Uiso calc 1
C C12 0.6517(3) 0.0117(2) 0.3829(3) 0.0396(7) Uani d 1
H H12 0.7406 -0.0252 0.3868 0.048 Uiso calc 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
_geom_angle_publ_flag
N3 Co1 N5 174.57(9) y
N3 Co1 N7 89.27(12) y
N5 Co1 N7 88.92(11) y
N3 Co1 N1 89.46(11) y
N5 Co1 N1 90.26(11) y
N7 Co1 N1 157.60(9) y
N3 Co1 Cl1 93.01(9) y
N5 Co1 Cl1 92.40(8) y
N7 Co1 Cl1 104.28(7) y
N1 Co1 Cl1 98.13(7) y
C1 N1 C3 105.5(2) ?
C1 N1 Co1 124.59(18) ?
C3 N1 Co1 129.90(19) ?
N1 C1 N2 111.0(3) ?
N1 C1 H1 124.5 ?
N2 C1 H1 124.5 ?
C1 N2 C2 108.3(2) ?
C1 N2 H2N 125.8 ?
C2 N2 H2N 125.8 ?
C3 C2 N2 105.8(2) ?
C3 C2 H2 127.1 ?
N2 C2 H2 127.1 ?
C2 C3 N1 109.3(3) ?
C2 C3 H3 125.3 ?
N1 C3 H3 125.3 ?
C4 N3 C6 105.6(3) ?
C4 N3 Co1 126.9(2) ?
C6 N3 Co1 127.4(2) ?
N3 C4 N4 110.4(3) ?
N3 C4 H4 124.8 ?
N4 C4 H4 124.8 ?
C4 N4 C5 108.3(3) ?
C4 N4 H4N 125.9 ?
C5 N4 H4N 125.9 ?
C6 C5 N4 106.3(3) ?
C6 C5 H5 126.9 ?
N4 C5 H5 126.9 ?
C5 C6 N3 109.4(3) ?
C5 C6 H6 125.3 ?
N3 C6 H6 125.3 ?
C7 N5 C9 106.1(3) ?
C7 N5 Co1 128.9(2) ?
C9 N5 Co1 125.0(2) ?
N5 C7 N6 110.4(3) ?
N5 C7 H7 124.8 ?
N6 C7 H7 124.8 ?
C7 N6 C8 107.8(3) ?
C7 N6 H6N 126.1 ?
C8 N6 H6N 126.1 ?
C9 C8 N6 106.2(3) ?
C9 C8 H8 126.9 ?
N6 C8 H8 126.9 ?
C8 C9 N5 109.6(3) ?
C8 C9 H9 125.2 ?
N5 C9 H9 125.2 ?
C10 N7 C12 105.4(3) ?
C10 N7 Co1 126.5(2) ?
C12 N7 Co1 128.0(2) ?
N7 C10 N8 110.7(3) ?
N7 C10 H10 124.6 ?
N8 C10 H10 124.6 ?
C10 N8 C11 107.5(2) ?
C10 N8 H8N 126.2 ?
C11 N8 H8N 126.2 ?
C12 C11 N8 106.4(3) ?
C12 C11 H11 126.8 ?
N8 C11 H11 126.8 ?
C11 C12 N7 109.9(3) ?
C11 C12 H12 125.0 ?
N7 C12 H12 125.0 ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N3 1.999(2) y
Co1 N5 2.001(2) y
Co1 N7 2.003(2) y
Co1 N1 2.011(2) y
Co1 Cl1 2.6151(7) y
N1 C1 1.319(4) .
N1 C3 1.375(3) .
C1 N2 1.328(4) .
C1 H1 0.9300 ?
N2 C2 1.358(4) .
N2 H2N 0.8600 ?
C2 C3 1.357(4) .
C2 H2 0.9300 ?
C3 H3 0.9300 ?
N3 C4 1.316(4) .
N3 C6 1.379(4) .
C4 N4 1.336(4) .
C4 H4 0.9300 ?
N4 C5 1.352(5) .
N4 H4N 0.8600 ?
C5 C6 1.341(5) .
C5 H5 0.9300 ?
C6 H6 0.9300 ?
N5 C7 1.314(4) .
N5 C9 1.372(4) .
C7 N6 1.336(4) .
C7 H7 0.9300 ?
N6 C8 1.367(5) .
N6 H6N 0.8600 ?
C8 C9 1.334(4) .
C8 H8 0.9300 ?
C9 H9 0.9300 ?
N7 C10 1.324(4) .
N7 C12 1.368(4) .
C10 N8 1.345(4) .
C10 H10 0.9300 ?
N8 C11 1.357(4) .
N8 H8N 0.8600 ?
C11 C12 1.346(4) .
C11 H11 0.9300 ?
C12 H12 0.9300 ?
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 H2N Cl2 . 0.86 2.53 3.180(3) 133
N4 H4N Cl2 4_566 0.86 2.40 3.247(3) 168
N6 H6N Cl2 4_565 0.86 2.40 3.251(3) 169
N8 H8N Cl1 1_455 0.86 2.44 3.254(3) 158
C3 H3 Cl2 1_455 0.93 2.78 3.639(3) 154
C4 H4 Cl1 3_756 0.93 2.78 3.541(4) 140
C10 H10 Cl2 1_455 0.93 2.77 3.657(3) 160
C2 H2 Im3 2_655 0.93 2.815 3.526(3) 134
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
C3 N1 C1 N2 0.9(5)
Co1 N1 C1 N2 -179.3(2)
N1 C1 N2 C2 -0.5(5)
C1 N2 C2 C3 -0.1(5)
N2 C2 C3 N1 0.6(5)
C1 N1 C3 C2 -0.9(5)
Co1 N1 C3 C2 179.3(3)
C6 N3 C4 N4 0.1(4)
Co1 N3 C4 N4 -176.3(3)
N3 C4 N4 C5 -0.4(5)
C4 N4 C5 C6 0.5(5)
N4 C5 C6 N3 -0.4(5)
C4 N3 C6 C5 0.2(5)
Co1 N3 C6 C5 176.6(3)
C9 N5 C7 N6 0.7(4)
Co1 N5 C7 N6 178.6(2)
N5 C7 N6 C8 -0.7(5)
C7 N6 C8 C9 0.4(5)
N6 C8 C9 N5 0.0(5)
C7 N5 C9 C8 -0.4(5)
Co1 N5 C9 C8 -178.4(3)
C12 N7 C10 N8 -0.1(5)
Co1 N7 C10 N8 177.0(2)
N7 C10 N8 C11 0.3(5)
C10 N8 C11 C12 -0.4(5)
N8 C11 C12 N7 0.3(5)
C10 N7 C12 C11 -0.1(5)
Co1 N7 C12 C11 -177.2(3)

_cod_database_fobs_code 2241094
