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data_global
#=======================================================================
# 1. SUBMISSION DETAILS
_publ_contact_author_name 'Professor W. Clegg'
_publ_contact_author_address
;
School of Natural Sciences (Chemistry)
University of Newcastle
Newcastle upon Tyne NE1 7RU
England
;
_publ_contact_author_phone '0191 222 6649'
_publ_contact_author_fax '0191 222 6929'
_publ_contact_author_email w.clegg@ncl.ac.uk
_publ_requested_journal 'Acta Crystallographica E'
_publ_requested_category EM
_publ_requested_coeditor_name ?
_publ_contact_letter
;
#8 February 2007
Please consider this CIF submission for publication in Acta
Crystallographica E as a new-style paper.
All required files have been provided.
The manuscript has passed the checkcif tests and generates an acceptable
printcif output.
Yours sincerely
Bill Clegg
;
#=======================================================================
# 2. PROCESSING SUMMARY (IUCr Office Use Only)
_journal_date_recd_electronic 2007-02-08
_journal_date_to_coeditor ?
_journal_date_from_coeditor 2007-02-15
_journal_date_accepted 2007-02-15
_journal_date_printers_first 2007-02-15
_journal_date_printers_final ?
_journal_date_proofs_out 2007-02-19
_journal_date_proofs_in ?
_journal_coeditor_name ?
_journal_coeditor_code WN2117
_journal_paper_category QM
_journal_coeditor_notes
; ?
;
_journal_techeditor_code E070780
_iucr_compatibility_tag ACTA95
_journal_techeditor_notes
; ?
;
_journal_coden_ASTM ACSEBH
_journal_name_full 'Acta Crystallographica, Section E'
_journal_year 2007
_journal_volume 63
_journal_issue 03
_journal_page_first m856
_journal_page_last m856
_journal_suppl_publ_number ?
_journal_suppl_publ_pages ?
#============================================================================
# 3. TITLE AND AUTHOR LIST
_publ_section_title
;
<i>trans</i>-Bis(aniline-\k<i>N</i>)dichlorobis(ethanol-\k<i>O</i>)cobalt(II)
;
loop_
_publ_author_name
_publ_author_address
'Clegg, William'
;
School of Natural Sciences (Chemistry)
Newcastle University
Newcastle upon Tyne NE1 7RU
England
;
'Martin, Nicola C.'
;
School of Natural Sciences (Chemistry)
Newcastle University
Newcastle upon Tyne NE1 7RU
England
;
#=========================================================================
# 4. TEXT
_publ_section_abstract
;
The title compound, [CoCl~2~(C~6~H~7~N)~2~(C~2~H~6~O)~2~], was obtained
unintentionally as the product of an attempted synthesis of a
polycarboxylate-bridged network complex of cobalt(II) using aniline as a base
to deprotonate the organic acid. The molecule is centrosymmetric, so pairs of
equivalent ligands lie <i>trans</i> to each other in a slightly distorted
octahedral coordination geometry. Molecules are linked by O---H...Cl and
N---H...Cl hydrogen bonds involving all the potential donors, generating
sheets parallel to (001). The phenyl rings protrude on both sides of these
sheets and have normal hydrophobic contacts with each other, involving no
intercalation or stacking interactions.
;
_publ_section_comment
;
The molecule of the title complex, (I) (Fig. 1), is centrosymmetric, so pairs
of equivalent ligands lie <i>trans</i> to each other in a slightly distorted
octahedral coordination geometry, <i>cis</i> angles deviating from 90\% by
less than 4\%.
Molecules are linked by O---H...Cl and N---H...Cl hydrogen bonds involving all
potential donors, generating sheets parallel to (001), as shown in Fig. 2. The
phenyl rings protrude on both sides of these sheets and have normal
hydrophobic contacts with each other, involving no intercalation or stacking
interactions.
The corresponding four-coordinate complex without ethanol has tetrahedral
geometry (Burrow <i>et al.</i>, 1997), with layers of molecules linked
by
N---H...Cl hydrogen bonds.
;
_publ_section_related_literature
;
The corresponding four-coordinate complex without ethanol has tetrahedral
geometry (Burrow et al., 1997), with layers of molecules linked by N---H...Cl
hydrogen bonds.
;
_publ_section_exptl_prep
;
The title compound was obtained unintentionally as the product of an attempted
synthesis of a polymeric network complex of cobalt with pyromellitic acid,
using vapour diffusion of aniline into an ethanol solution of cobalt(II)
chloride and pyromellitic acid at room temperature.
;
_publ_section_exptl_refinement
;
H atoms bonded to N and O atoms were located in a difference map and refined
with distance restraints of O---H = 0.84(2) and N---H = 0.87(2) \%A, and with
<i>U</i>~iso~(H) = 1.2<i>U</i>~eq~(N,O). Other H atoms were positioned
geometrically and refined using a riding model (including free rotation about
the ethanol C---C bond),
with C---H = 0.95--0.99 \%A and
with <i>U</i>~iso~(H) = 1.2
(1.5 for methyl groups) times <i>U</i>~eq~(C).
;
_publ_section_references
;
Bruker (2001). <i>SMART</i> and <i>SAINT</i>. Bruker AXS Inc., Madison,
Wisconsin, USA.
Burrow, R. A., Horner, M., Lang, L. S., Neves, A. & Vencato, I. (1997).
<i>Z. Kristallogr. New Cryst. Struct.</i> <b>212</b>, 41--41.
Sheldrick, G. M. (2001). <i>SHELXTL</i>. Version 5.0. Bruker AXS Inc.,
Madison, Wisconsin, USA.
Sheldrick, G. M. (2004). <i>SADABS</i>. University of G\"ottingen,
Germany.
;
_publ_section_figure_captions
;
Fig. 1. The molecular structure of (I), with atom labels and 50% probability
displacement ellipsoids for non-H atoms.
Fig. 2. The packing of (I), viewed down the <i>c</i> axis, showing one layer of
molecules connected by O---H...Cl and N---H...Cl hydrogen bonds (dashed
lines). H atoms not involved in hydrogen bonding have been omitted.
;
_publ_section_table_legends
;
Table 1. Selected geometric parameters (\%A, \%).
Table 2. Hydrogen bonding geometry (\%A, \%).
;
_publ_section_acknowledgements
;
The authors thank the EPSRC for financial support.
;
#==============================================================================
data_I
#==============================================================================
# 5. GENERAL AND CHEMICAL DATA
_audit_creation_method SHELXL97
_chemical_name_systematic
;
trans-Bis(aniline-\kN)dichlorobis(ethanol-\kO)cobalt(II)
;
_chemical_name_common ?
_chemical_melting_point ?
_chemical_compound_source ?
_chemical_formula_iupac '[Co Cl2 (C6 H7 N)2 (C2 H6 O)2]'
_chemical_formula_moiety 'C16 H26 Cl2 Co N2 O2'
_chemical_formula_sum 'C16 H26 Cl2 Co N2 O2'
_chemical_formula_weight 408.22
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'
#==============================================================================
# 6. CRYSTAL DATA
_symmetry_cell_setting triclinic
_symmetry_space_group_name_H-M 'P -1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a 5.8166(16)
_cell_length_b 6.8339(19)
_cell_length_c 12.263(3)
_cell_angle_alpha 87.642(5)
_cell_angle_beta 81.726(5)
_cell_angle_gamma 73.017(5)
_cell_volume 461.3(2)
_cell_formula_units_Z 1
_cell_measurement_temperature 160(2)
_cell_measurement_reflns_used 2052
_cell_measurement_theta_min 3.12
_cell_measurement_theta_max 28.64
_exptl_crystal_description block
_exptl_crystal_colour pink
_exptl_crystal_size_max 0.30
_exptl_crystal_size_mid 0.20
_exptl_crystal_size_min 0.04
_exptl_crystal_density_meas ?
_exptl_crystal_density_diffrn 1.469
_exptl_crystal_density_method 'not measured'
_exptl_crystal_F_000 213
_exptl_absorpt_coefficient_mu 1.229
_exptl_absorpt_correction_type multi-scan
_exptl_absorpt_correction_T_min 0.710
_exptl_absorpt_correction_T_max 0.950
_exptl_absorpt_process_details '(SADABS; Sheldrick, 2004)'
#==============================================================================
# 7. EXPERIMENTAL DATA
_exptl_special_details
;
;
_diffrn_ambient_temperature 160(2)
_diffrn_radiation_wavelength 0.71073
_diffrn_radiation_type MoK\a
_diffrn_radiation_source 'sealed tube'
_diffrn_radiation_monochromator graphite
_diffrn_measurement_device_type 'Bruker SMART 1K CCD area-detector'
_diffrn_measurement_method 'thin-slice \w'
_diffrn_detector_area_resol_mean 8.192
_diffrn_standards_number 0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time ?
_diffrn_standards_decay_% ?
_diffrn_reflns_number 2296
_diffrn_reflns_av_R_equivalents 0.0271
_diffrn_reflns_av_sigmaI/netI 0.0480
_diffrn_reflns_limit_h_min -6
_diffrn_reflns_limit_h_max 6
_diffrn_reflns_limit_k_min -8
_diffrn_reflns_limit_k_max 7
_diffrn_reflns_limit_l_min -14
_diffrn_reflns_limit_l_max 14
_diffrn_reflns_theta_min 1.68
_diffrn_reflns_theta_max 25.00
_reflns_number_total 1583
_reflns_number_gt 1278
_reflns_threshold_expression I>2\s(I)
_computing_data_collection 'SMART (Bruker, 2001)'
_computing_cell_refinement 'SAINT (Bruker, 2001)'
_computing_data_reduction 'SAINT'
_computing_structure_solution 'SHELXTL (Sheldrick, 2001)'
_computing_structure_refinement SHELXTL
_computing_molecular_graphics SHELXTL
_computing_publication_material 'SHELXTL and local programs'
#==============================================================================
# 8. REFINEMENT DATA
_refine_special_details
;
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type full
_refine_ls_weighting_scheme calc
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^)+(0.0677P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary direct
_atom_sites_solution_secondary difmap
_atom_sites_solution_hydrogens mixed
_refine_ls_hydrogen_treatment mixed
_refine_ls_extinction_method none
_refine_ls_extinction_coef ?
_refine_ls_number_reflns 1583
_refine_ls_number_parameters 116
_refine_ls_number_restraints 3
_refine_ls_R_factor_all 0.0509
_refine_ls_R_factor_gt 0.0401
_refine_ls_wR_factor_ref 0.1050
_refine_ls_wR_factor_gt 0.1004
_refine_ls_goodness_of_fit_ref 1.028
_refine_ls_restrained_S_all 1.027
_refine_ls_shift/su_max 0.000
_refine_ls_shift/su_mean 0.000
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_theta_full 25.00
_diffrn_measured_fraction_theta_full 0.983
_refine_diff_density_max 0.819
_refine_diff_density_min -0.948
#==============================================================================
# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.5000 0.5000 0.5000 0.0127(2) Uani 1 2 d S . .
Cl Cl 0.26740(13) 0.26735(11) 0.45695(6) 0.0178(2) Uani 1 1 d . . .
O O 0.2256(4) 0.5979(3) 0.63639(18) 0.0165(5) Uani 1 1 d D . .
H1O H 0.095(4) 0.608(5) 0.613(3) 0.020 Uiso 1 1 d D . .
C1 C 0.2075(6) 0.7554(5) 0.7133(3) 0.0215(8) Uani 1 1 d . . .
H1A H 0.1462 0.8907 0.6787 0.026 Uiso 1 1 calc R . .
H1B H 0.3710 0.7442 0.7319 0.026 Uiso 1 1 calc R . .
C2 C 0.0399(7) 0.7412(6) 0.8177(3) 0.0291(9) Uani 1 1 d . . .
H2A H -0.1218 0.7512 0.7995 0.044 Uiso 1 1 calc R . .
H2B H 0.0287 0.8532 0.8674 0.044 Uiso 1 1 calc R . .
H2C H 0.1041 0.6099 0.8539 0.044 Uiso 1 1 calc R . .
N N 0.2846(5) 0.7522(4) 0.4102(2) 0.0158(6) Uani 1 1 d D . .
H1C H 0.293(7) 0.860(3) 0.444(3) 0.019 Uiso 1 1 d D . .
H1D H 0.139(3) 0.743(5) 0.432(3) 0.019 Uiso 1 1 d D . .
C3 C 0.3387(6) 0.7559(4) 0.2928(3) 0.0153(7) Uani 1 1 d . . .
C4 C 0.5275(6) 0.8296(5) 0.2440(3) 0.0225(8) Uani 1 1 d . . .
H4 H 0.6184 0.8803 0.2885 0.027 Uiso 1 1 calc R . .
C5 C 0.5829(7) 0.8292(5) 0.1308(3) 0.0267(8) Uani 1 1 d . . .
H5 H 0.7112 0.8811 0.0979 0.032 Uiso 1 1 calc R . .
C6 C 0.4557(7) 0.7549(5) 0.0649(3) 0.0292(9) Uani 1 1 d . . .
H6 H 0.4958 0.7547 -0.0130 0.035 Uiso 1 1 calc R . .
C7 C 0.2666(7) 0.6797(5) 0.1139(3) 0.0274(8) Uani 1 1 d . . .
H7 H 0.1777 0.6273 0.0692 0.033 Uiso 1 1 calc R . .
C8 C 0.2086(6) 0.6813(5) 0.2273(3) 0.0209(8) Uani 1 1 d . . .
H8 H 0.0789 0.6311 0.2603 0.025 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Co 0.0061(3) 0.0094(3) 0.0209(4) -0.0010(2) -0.0035(2) 0.0015(2)
Cl 0.0090(4) 0.0140(4) 0.0297(5) -0.0037(3) -0.0050(3) -0.0008(3)
O 0.0090(12) 0.0161(11) 0.0240(13) -0.0030(9) -0.0058(10) -0.0006(9)
C1 0.0161(18) 0.0168(17) 0.031(2) -0.0049(14) -0.0039(15) -0.0030(14)
C2 0.029(2) 0.0248(19) 0.031(2) -0.0067(16) 0.0007(17) -0.0056(16)
N 0.0097(14) 0.0112(13) 0.0248(16) -0.0015(11) -0.0049(12) 0.0009(11)
C3 0.0124(17) 0.0069(14) 0.0227(17) 0.0009(12) -0.0032(13) 0.0036(12)
C4 0.0173(19) 0.0158(16) 0.035(2) 0.0042(14) -0.0069(15) -0.0046(14)
C5 0.0185(19) 0.0197(18) 0.036(2) 0.0078(15) 0.0019(16) 0.0002(15)
C6 0.030(2) 0.0197(18) 0.028(2) 0.0035(15) -0.0001(16) 0.0065(16)
C7 0.030(2) 0.0189(17) 0.032(2) -0.0043(15) -0.0120(16) -0.0016(15)
C8 0.0184(18) 0.0155(17) 0.0280(19) -0.0004(14) -0.0042(14) -0.0030(14)
#==============================================================================
# 10. GEOMETRY
_geom_special_details
;
?
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co Cl 2.4836(9) . y
Co Cl 2.4835(9) 2_666 ?
Co O 2.120(2) . y
Co O 2.120(2) 2_666 ?
Co N 2.175(3) . y
Co N 2.175(3) 2_666 ?
O H1O 0.833(10) . ?
O C1 1.431(4) . ?
C1 H1A 0.990 . ?
C1 H1B 0.990 . ?
C1 C2 1.512(5) . ?
C2 H2A 0.980 . ?
C2 H2B 0.980 . ?
C2 H2C 0.980 . ?
N H1C 0.873(10) . ?
N H1D 0.869(10) . ?
N C3 1.431(4) . ?
C3 C4 1.388(5) . ?
C3 C8 1.382(5) . ?
C4 H4 0.950 . ?
C4 C5 1.378(5) . ?
C5 H5 0.950 . ?
C5 C6 1.372(6) . ?
C6 H6 0.950 . ?
C6 C7 1.396(6) . ?
C7 H7 0.950 . ?
C7 C8 1.383(5) . ?
C8 H8 0.950 . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl Co Cl 180 . 2_666 ?
Cl Co O 86.06(6) . . y
Cl Co O 86.06(7) 2_666 2_666 ?
Cl Co O 93.94(7) 2_666 . ?
Cl Co O 93.94(6) . 2_666 ?
Cl Co N 92.33(8) . . y
Cl Co N 87.67(8) 2_666 . ?
Cl Co N 92.33(8) 2_666 2_666 ?
Cl Co N 87.67(8) . 2_666 ?
O Co O 180 . 2_666 ?
O Co N 86.22(10) . . y
O Co N 93.78(10) 2_666 . ?
O Co N 86.22(10) 2_666 2_666 ?
O Co N 93.78(10) . 2_666 ?
N Co N 180 . 2_666 ?
Co O H1O 106(3) . . ?
Co O C1 126.4(2) . . ?
H1O O C1 113(3) . . ?
O C1 H1A 109.3 . . ?
O C1 H1B 109.3 . . ?
O C1 C2 111.8(3) . . ?
H1A C1 H1B 107.9 . . ?
H1A C1 C2 109.3 . . ?
H1B C1 C2 109.3 . . ?
C1 C2 H2A 109.5 . . ?
C1 C2 H2B 109.5 . . ?
C1 C2 H2C 109.5 . . ?
H2A C2 H2B 109.5 . . ?
H2A C2 H2C 109.5 . . ?
H2B C2 H2C 109.5 . . ?
Co N H1C 103(2) . . ?
Co N H1D 101(2) . . ?
Co N C3 118.62(19) . . ?
H1C N H1D 106(3) . . ?
H1C N C3 115(2) . . ?
H1D N C3 112(2) . . ?
N C3 C4 119.9(3) . . ?
N C3 C8 120.5(3) . . ?
C4 C3 C8 119.6(3) . . ?
C3 C4 H4 120.1 . . ?
C3 C4 C5 119.9(3) . . ?
H4 C4 C5 120.1 . . ?
C4 C5 H5 119.5 . . ?
C4 C5 C6 121.1(4) . . ?
H5 C5 C6 119.5 . . ?
C5 C6 H6 120.4 . . ?
C5 C6 C7 119.1(4) . . ?
H6 C6 C7 120.4 . . ?
C6 C7 H7 119.9 . . ?
C6 C7 C8 120.1(3) . . ?
H7 C7 C8 119.9 . . ?
C3 C8 C7 120.2(3) . . ?
C3 C8 H8 119.9 . . ?
C7 C8 H8 119.9 . . ?
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_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Cl Co O C1 -177.0(2) . . . . ?
Cl Co O C1 3.0(2) 2_666 . . . ?
N Co O C1 -84.4(2) . . . . ?
N Co O C1 95.6(2) 2_666 . . . ?
Co O C1 C2 -162.3(2) . . . . ?
Cl Co N C3 -79.7(2) . . . . ?
Cl Co N C3 100.3(2) 2_666 . . . ?
O Co N C3 -165.6(2) . . . . ?
O Co N C3 14.4(2) 2_666 . . . ?
Co N C3 C4 -81.7(3) . . . . ?
Co N C3 C8 96.5(3) . . . . ?
N C3 C4 C5 178.7(3) . . . . ?
C8 C3 C4 C5 0.4(5) . . . . ?
C3 C4 C5 C6 -0.6(5) . . . . ?
C4 C5 C6 C7 0.3(5) . . . . ?
C5 C6 C7 C8 0.3(5) . . . . ?
N C3 C8 C7 -178.1(3) . . . . ?
C4 C3 C8 C7 0.2(5) . . . . ?
C6 C7 C8 C3 -0.5(5) . . . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
_geom_hbond_publ_flag
O H1O Cl 0.833(10) 2.306(14) 3.114(2) 163(3) 2_566 y
N H1C Cl 0.873(10) 2.756(18) 3.560(3) 154(3) 1_565 y
N H1D Cl 0.869(10) 2.574(13) 3.422(3) 165(3) 2_566 y
#===================== End of CIF submission =================================