#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006209.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_2006209
loop_
_publ_author_name
'Friesen, D. A.'
'Quail, J. W.'
'Waltz, W. L.'
'Nashiem, R. E.'
_publ_section_title
;
cis-and
trans-Diisothiocyanato(1,4,8,11-tetraazacyclotetradecane)chromium(III)
Perchlorate
;
_journal_issue 6
_journal_name_full 'Acta Crystallographica Section C'
_journal_page_first 687
_journal_page_last 691
_journal_volume 53
_journal_year 1997
_chemical_formula_moiety '[Cr(N C S)2 (C10 H24 N4)] , (Cl O4)'
_chemical_formula_sum 'C12 H24 Cl Cr N6 O4 S2'
_chemical_formula_weight 467.928
_chemical_name_common
'trans-diisothiocyanato(cyclam)chromium(III) perchlorate'
_chemical_name_systematic
;
trans-diisothiocyanato(1,4,8,11-tetraazacyclotetradecane)chromium(III)
perchlorate
;
_space_group_IT_number 2
_symmetry_cell_setting triclinic
_symmetry_space_group_name_Hall '-P 1'
_symmetry_space_group_name_H-M 'P -1'
_cell_angle_alpha 65.930(15)
_cell_angle_beta 69.870(12)
_cell_angle_gamma 83.86(2)
_cell_formula_units_Z 1
_cell_length_a 7.6925(14)
_cell_length_b 8.471(2)
_cell_length_c 8.9387(8)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 173(2)
_cell_measurement_theta_max 27.79
_cell_measurement_theta_min 11.53
_cell_volume 498.96(17)
_computing_cell_refinement 'SET4 and CELDIM CAD-4 Software'
_computing_data_collection 'CAD-4 Software (Enraf-Nonius, 1989)'
_computing_data_reduction
'DATRD2 in NRCVAX94 (Gabe, Le Page, Charland, Lee & White, 1989)'
_computing_molecular_graphics 'NRCVAX94, ORTEPII (Johnson, 1976)'
_computing_publication_material
'NRCVAX94, SHELXL93, WordPerfect macro PREPCIF97 (Ferguson, 1997)'
_computing_structure_refinement 'NRCVAX94, SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution 'DIRDIF (Beurskens et al., 1992)'
_diffrn_ambient_temperature 173(2)
_diffrn_measurement_device 'Enraf-Nonius CAD-4'
_diffrn_measurement_method '\q/2\q scan b/P/b'
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'fine-focus sealed tube'
_diffrn_radiation_type CuK\a
_diffrn_radiation_wavelength 1.54180
_diffrn_reflns_av_R_equivalents 0.019
_diffrn_reflns_av_sigmaI/netI 0.0114
_diffrn_reflns_limit_h_max 9
_diffrn_reflns_limit_h_min -9
_diffrn_reflns_limit_k_max 10
_diffrn_reflns_limit_k_min 0
_diffrn_reflns_limit_l_max 11
_diffrn_reflns_limit_l_min -9
_diffrn_reflns_number 2978
_diffrn_reflns_theta_max 73.00
_diffrn_reflns_theta_min 5.72
_diffrn_standards_decay_% 0.0
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 8.183
_exptl_absorpt_correction_T_max 0.4306
_exptl_absorpt_correction_T_min 0.1314
_exptl_absorpt_correction_type 'Gaussian integration'
_exptl_crystal_colour yellow
_exptl_crystal_density_diffrn 1.557
_exptl_crystal_density_meas 'not measured'
_exptl_crystal_description plate
_exptl_crystal_F_000 243
_exptl_crystal_size_max 0.35
_exptl_crystal_size_mid 0.30
_exptl_crystal_size_min 0.12
_refine_diff_density_max 0.551
_refine_diff_density_min -0.340
_refine_ls_extinction_coef 0.0198(14)
_refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all 1.079
_refine_ls_goodness_of_fit_obs 1.079
_refine_ls_hydrogen_treatment 'H atoms riding (C-H 0.99, N-H 0.93\%A)'
_refine_ls_matrix_type full
_refine_ls_number_parameters 140
_refine_ls_number_reflns 1949
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.079
_refine_ls_restrained_S_obs 1.079
_refine_ls_R_factor_all 0.0306
_refine_ls_R_factor_obs 0.0300
_refine_ls_shift/esd_max 0.000
_refine_ls_shift/esd_mean 0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0473P)^2^+0.2952P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.0817
_refine_ls_wR_factor_obs 0.0811
_reflns_number_observed 1926
_reflns_number_total 1949
_reflns_observed_criterion >2\s(I)
_[local]_cod_data_source_file fg1243.cif
_[local]_cod_data_source_block 1b
_cod_original_cell_volume 498.96(15)
_cod_database_code 2006209
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Cr 0.0152(2) 0.0162(2) 0.0239(2) 0.00060(14) -0.0077(2) -0.0092(2)
Cl 0.0381(4) 0.0380(4) 0.0486(5) -0.0126(3) 0.0037(3) -0.0224(4)
S 0.0247(3) 0.0386(3) 0.0601(4) 0.0059(2) -0.0204(2) -0.0332(3)
O1 0.078(3) 0.082(3) 0.045(2) -0.041(3) 0.013(2) -0.020(2)
O2 0.099(4) 0.036(2) 0.097(4) -0.011(2) -0.013(3) -0.009(2)
O3 0.079(3) 0.097(4) 0.082(3) -0.029(3) -0.022(3) -0.051(3)
O4 0.034(2) 0.104(4) 0.137(5) 0.001(2) -0.018(3) -0.067(4)
N1 0.0268(8) 0.0311(9) 0.0286(9) -0.0056(7) -0.0106(7) -0.0042(7)
N2 0.0209(7) 0.0266(8) 0.0472(10) 0.0048(6) -0.0123(7) -0.0225(8)
N3 0.0207(7) 0.0286(8) 0.0346(9) 0.0008(6) -0.0107(7) -0.0158(7)
C1 0.0424(12) 0.0284(11) 0.0526(14) 0.0016(9) -0.0252(11) 0.0024(10)
C2 0.0379(12) 0.0189(9) 0.072(2) 0.0072(9) -0.0230(12) -0.0159(10)
C3 0.0270(10) 0.0580(14) 0.063(2) 0.0053(10) -0.0114(10) -0.0490(13)
C4 0.0313(11) 0.084(2) 0.0398(13) -0.0079(12) -0.0019(10) -0.0415(14)
C5 0.0382(12) 0.066(2) 0.0248(10) -0.0125(11) -0.0100(9) -0.0135(10)
C6 0.0174(8) 0.0233(9) 0.0302(10) 0.0036(7) -0.0090(7) -0.0111(8)
loop_
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_type_symbol
Cr 0.5000 0.5000 0.5000 0.01765(15) Uani d S 1 Cr
Cl 0.0000 0.0000 0.0000 0.0437(2) Uani d S 1 Cl
S 0.90396(7) 0.76365(7) 0.62567(8) 0.0350(2) Uani d . 1 S
O1 -0.1152(7) -0.0554(7) 0.1680(6) 0.0759(14) Uani d P 0.50 O
O2 -0.0080(8) 0.1897(5) -0.0897(7) 0.088(2) Uani d P 0.50 O
O3 -0.0834(7) -0.0685(7) -0.0932(7) 0.0797(14) Uani d P 0.50 O
O4 0.1806(6) -0.0416(8) -0.0357(9) 0.088(2) Uani d P 0.50 O
N1 0.5784(2) 0.6846(2) 0.2493(2) 0.0305(4) Uani d . 1 N
N2 0.3442(2) 0.6889(2) 0.5642(2) 0.0289(4) Uani d . 1 N
N3 0.7134(2) 0.5766(2) 0.5341(2) 0.0263(4) Uani d . 1 N
C1 0.4446(4) 0.8249(3) 0.2506(3) 0.0449(6) Uani d . 1 C
C2 0.4122(3) 0.8546(3) 0.4125(4) 0.0428(6) Uani d . 1 C
C3 0.3292(3) 0.6954(3) 0.7316(3) 0.0422(6) Uani d . 1 C
C4 0.2643(3) 0.5218(4) 0.8825(3) 0.0478(6) Uani d . 1 C
C5 0.4000(3) 0.3781(4) 0.8887(3) 0.0434(6) Uani d . 1 C
C6 0.7983(2) 0.6537(2) 0.5695(2) 0.0234(4) Uani d . 1 C
H1 0.6935(2) 0.7306(2) 0.2271(2) 0.037 Uiso calc R 1 H
H2 0.2243(2) 0.6690(2) 0.5717(2) 0.035 Uiso calc R 1 H
H1A 0.3264(4) 0.7911(3) 0.2487(3) 0.054 Uiso calc R 1 H
H1B 0.4953(4) 0.9324(3) 0.1468(3) 0.054 Uiso calc R 1 H
H2A 0.5290(3) 0.8951(3) 0.4111(4) 0.051 Uiso calc R 1 H
H2B 0.3193(3) 0.9441(3) 0.4192(4) 0.051 Uiso calc R 1 H
H3A 0.2406(3) 0.7843(3) 0.7520(3) 0.051 Uiso calc R 1 H
H3B 0.4515(3) 0.7297(3) 0.7251(3) 0.051 Uiso calc R 1 H
H4A 0.2321(3) 0.5389(4) 0.9919(3) 0.057 Uiso calc R 1 H
H4B 0.1494(3) 0.4831(4) 0.8788(3) 0.057 Uiso calc R 1 H
H5A 0.5220(3) 0.4208(4) 0.8744(3) 0.052 Uiso calc R 1 H
H5B 0.3560(3) 0.2807(4) 1.0036(3) 0.052 Uiso calc R 1 H
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr -0.1635 2.4439 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_diffrn_standard_refln_index_h
_diffrn_standard_refln_index_k
_diffrn_standard_refln_index_l
4 0 0
0 4 0
0 0 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
N3 Cr N3 . 2_666 180.0
N3 Cr N2 . 2_666 89.91(7)
N3 Cr N2 2_666 2_666 90.09(7)
N3 Cr N2 . . 90.09(7)
N3 Cr N2 2_666 . 89.91(7)
N2 Cr N2 2_666 . 180.0
N3 Cr N1 . . 89.48(7)
N3 Cr N1 2_666 . 90.52(7)
N2 Cr N1 2_666 . 94.66(7)
N2 Cr N1 . . 85.34(7)
N3 Cr N1 . 2_666 90.52(7)
N3 Cr N1 2_666 2_666 89.48(7)
N2 Cr N1 2_666 2_666 85.34(7)
N2 Cr N1 . 2_666 94.66(7)
N1 Cr N1 . 2_666 180.0
O4 Cl O1 . . 119.9(3)
O4 Cl O2 . . 108.2(3)
O1 Cl O2 . . 110.4(3)
O4 Cl O3 . . 107.5(3)
O1 Cl O3 . . 106.8(3)
O2 Cl O3 . . 102.7(3)
C1 N1 Cr . . 105.76(14)
C2 N2 C3 . . 113.5(2)
C2 N2 Cr . . 106.38(13)
C3 N2 Cr . . 117.61(14)
C6 N3 Cr . . 159.46(14)
N1 C1 C2 . . 108.3(2)
N2 C2 C1 . . 108.3(2)
N2 C3 C4 . . 111.7(2)
C5 C4 C3 . . 116.3(2)
N1 C5 C4 2_666 . 111.7(2)
N3 C6 S . . 176.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cr N1 . 2.060(2)
Cr N1 2_666 2.060(2)
Cr N2 . 2.048(2)
Cr N2 2_666 2.048(2)
Cr N3 . 1.985(2)
Cr N3 2_666 1.985(2)
Cl O1 . 1.363(4)
Cl O1 2 1.363(4)
Cl O2 . 1.480(4)
Cl O2 2 1.480(4)
Cl O3 . 1.511(4)
Cl O3 2 1.511(4)
Cl O4 . 1.356(4)
Cl O4 2 1.356(4)
S C6 . 1.614(2)
N1 C1 . 1.488(3)
N1 C5 2_666 1.485(3)
N2 C2 . 1.483(3)
N2 C3 . 1.484(3)
N3 C6 . 1.165(2)
C1 C2 . 1.501(4)
C3 C4 . 1.519(4)
C4 C5 . 1.512(4)
C5 N1 2_666 1.485(3)
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_site_symmetry_1
_geom_torsion_site_symmetry_4
_geom_torsion
N3 Cr N1 C5 . 2_666 127.51(15)
N3 Cr N1 C5 2_666 2_666 -52.49(15)
N2 Cr N1 C5 2_666 2_666 37.65(15)
N2 Cr N1 C5 . 2_666 -142.35(15)
N1 Cr N1 C5 2_666 2_666 -17.E1(10)
N3 Cr N1 C1 . . -104.99(14)
N3 Cr N1 C1 2_666 . 75.01(14)
N2 Cr N1 C1 2_666 . 165.14(14)
N2 Cr N1 C1 . . -14.86(14)
N1 Cr N1 C1 2_666 . -4.E1(10)
N3 Cr N2 C2 . . 74.73(14)
N3 Cr N2 C2 2_666 . -105.27(14)
N2 Cr N2 C2 2_666 . -13.E1(10)
N1 Cr N2 C2 . . -14.74(14)
N1 Cr N2 C2 2_666 . 165.26(14)
N3 Cr N2 C3 . . -53.82(15)
N3 Cr N2 C3 2_666 . 126.18(15)
N2 Cr N2 C3 2_666 . 11.E1(10)
N1 Cr N2 C3 . . -143.28(15)
N1 Cr N2 C3 2_666 . 36.72(15)
N3 Cr N3 C6 2_666 . -15.E1(10)
N2 Cr N3 C6 2_666 . -175.6(5)
N2 Cr N3 C6 . . 4.4(5)
N1 Cr N3 C6 . . 89.8(5)
N1 Cr N3 C6 2_666 . -90.2(5)
C5 N1 C1 C2 2_666 . 170.6(2)
Cr N1 C1 C2 . . 41.9(2)
C3 N2 C2 C1 . . 172.8(2)
Cr N2 C2 C1 . . 41.8(2)
N1 C1 C2 N2 . . -57.3(2)
C2 N2 C3 C4 . . -178.4(2)
Cr N2 C3 C4 . . -53.3(2)
N2 C3 C4 C5 . . 69.5(2)
C3 C4 C5 N1 . 2_666 -71.5(3)
Cr N3 C6 S . . 20.(3)