#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2006208.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_2006208
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 65.777(12)
_cell_angle_beta 69.777(11)
_cell_angle_gamma 83.540(13)
_cell_formula_units_Z 1
_cell_length_a 7.7374(13)
_cell_length_b 8.5142(14)
_cell_length_c 9.0238(9)
_cell_measurement_reflns_used 25
_cell_measurement_temperature 288.0(10)
_cell_measurement_theta_max 35.40
_cell_measurement_theta_min 11.45
_cell_volume 508.41(14)
_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 288.0(10)
_diffrn_measurement_device 'Enraf-Nonius CAD-4'
_diffrn_measurement_method \q/2\q
_diffrn_radiation_monochromator graphite
_diffrn_radiation_source 'X-ray tube'
_diffrn_radiation_type 'Copper K\a'
_diffrn_radiation_wavelength 1.54180
_diffrn_reflns_av_R_equivalents 0.017
_diffrn_reflns_av_sigmaI/netI 0.0113
_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 4005
_diffrn_reflns_theta_max 73.00
_diffrn_reflns_theta_min 5.70
_diffrn_standards_decay_% 0.0
_diffrn_standards_interval_time 120
_diffrn_standards_number 3
_exptl_absorpt_coefficient_mu 8.031
_exptl_absorpt_correction_T_max 0.4343
_exptl_absorpt_correction_T_min 0.1314
_exptl_absorpt_correction_type 'Gaussian integration'
_exptl_crystal_colour orange-yellow
_exptl_crystal_density_diffrn 1.5283
_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 0.834
_refine_diff_density_min -0.612
_refine_ls_extinction_coef 0.0206(17)
_refine_ls_extinction_method 'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all 1.045
_refine_ls_goodness_of_fit_obs 1.047
_refine_ls_hydrogen_treatment 'H atoms riding (C-H 0.97, N-H 0.91\%A)'
_refine_ls_matrix_type full
_refine_ls_number_parameters 140
_refine_ls_number_reflns 2027
_refine_ls_number_restraints 0
_refine_ls_restrained_S_all 1.045
_refine_ls_restrained_S_obs 1.047
_refine_ls_R_factor_all 0.0395
_refine_ls_R_factor_obs 0.0387
_refine_ls_shift/esd_max 0.005
_refine_ls_shift/esd_mean 0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme
'calc w = 1/[\s^2^(Fo^2^)+(0.0552P)^2^+0.4159P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_wR_factor_all 0.1037
_refine_ls_wR_factor_obs 0.1029
_reflns_number_observed 1989
_reflns_number_total 2027
_reflns_observed_criterion >2\s(I)
_[local]_cod_data_source_file fg1243.cif
_[local]_cod_data_source_block 1a
_cod_database_code 2006208
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 0.0249(3) 0.0270(3) 0.0354(3) -0.0008(2) -0.0098(2) -0.0134(2)
Cl 0.0618(7) 0.0664(7) 0.0750(7) -0.0183(5) 0.0063(5) -0.0319(6)
S 0.0424(4) 0.0693(5) 0.1024(6) 0.0094(3) -0.0344(4) -0.0581(5)
O1 0.165(9) 0.169(9) 0.080(5) -0.084(8) 0.034(5) -0.043(5)
O2 0.166(9) 0.069(4) 0.178(9) -0.016(5) -0.017(7) -0.029(5)
O3 0.140(7) 0.183(9) 0.178(8) -0.034(7) -0.049(6) -0.116(8)
O4 0.063(4) 0.193(10) 0.221(12) 0.010(5) -0.038(6) -0.110(10)
N1 0.0446(12) 0.0582(14) 0.0427(12) -0.0130(10) -0.0150(10) -0.0023(10)
N2 0.0326(10) 0.0466(12) 0.081(2) 0.0068(9) -0.0177(10) -0.0394(12)
N3 0.0327(10) 0.0479(12) 0.0534(12) -0.0023(9) -0.0147(9) -0.0245(10)
C1 0.075(2) 0.050(2) 0.091(3) -0.001(2) -0.045(2) 0.013(2)
C2 0.063(2) 0.0322(14) 0.135(4) 0.0113(14) -0.039(2) -0.026(2)
C3 0.043(2) 0.110(3) 0.119(3) 0.011(2) -0.018(2) -0.096(3)
C4 0.052(2) 0.169(5) 0.072(2) -0.014(2) 0.000(2) -0.084(3)
C5 0.067(2) 0.132(4) 0.0358(14) -0.029(2) -0.0122(14) -0.023(2)
C6 0.0277(11) 0.0411(12) 0.0491(13) 0.0045(9) -0.0137(10) -0.0204(10)
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 0.0287(2) Uani d S 1 Cr
Cl 0.0000 0.0000 0.0000 0.0729(4) Uani d S 1 Cl
S 0.89969(10) 0.76101(10) 0.62535(12) 0.0607(3) Uani d . 1 S
O1 -0.1144(18) -0.0529(15) 0.1604(11) 0.154(4) Uani d P 0.50 O
O2 -0.0044(15) 0.1856(9) -0.0898(15) 0.155(4) Uani d P 0.50 O
O3 -0.0797(13) -0.0680(14) -0.0901(14) 0.149(4) Uani d P 0.50 O
O4 0.1781(11) -0.0406(16) -0.0372(19) 0.153(4) Uani d P 0.50 O
N1 0.5781(3) 0.6787(3) 0.2504(3) 0.0533(6) Uani d . 1 N
N2 0.3427(3) 0.6901(3) 0.5581(3) 0.0493(6) Uani d . 1 N
N3 0.7106(3) 0.5800(3) 0.5317(3) 0.0427(5) Uani d . 1 N
C1 0.4443(6) 0.8186(4) 0.2485(5) 0.0813(12) Uani d . 1 C
C2 0.4098(5) 0.8521(4) 0.4060(6) 0.0785(12) Uani d . 1 C
C3 0.3266(4) 0.7005(6) 0.7219(6) 0.0764(12) Uani d . 1 C
C4 0.7374(5) 0.4696(7) 0.1266(5) 0.0893(14) Uani d . 1 C
C5 0.6029(5) 0.6123(6) 0.1160(4) 0.0808(12) Uani d . 1 C
C6 0.7951(3) 0.6546(3) 0.5678(3) 0.0384(5) Uani d . 1 C
H1 0.6894 0.7245 0.2288 0.064 Uiso calc R 1 H
H2 0.2264 0.6695 0.5655 0.059 Uiso calc R 1 H
H1A 0.3298 0.7846 0.2466 0.098 Uiso calc R 1 H
H1B 0.4937 0.9224 0.1464 0.098 Uiso calc R 1 H
H2A 0.5227 0.8930 0.4044 0.094 Uiso calc R 1 H
H2B 0.3186 0.9396 0.4100 0.094 Uiso calc R 1 H
H3A 0.2398 0.7879 0.7394 0.092 Uiso calc R 1 H
H3B 0.4454 0.7348 0.7151 0.092 Uiso calc R 1 H
H4A 0.8488 0.5086 0.1296 0.107 Uiso calc R 1 H
H4B 0.7700 0.4499 0.0219 0.107 Uiso calc R 1 H
H5A 0.6469 0.7058 0.0033 0.097 Uiso calc R 1 H
H5B 0.4849 0.5701 0.1293 0.097 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 . . 90.24(9)
N3 Cr N2 2_666 . 89.76(9)
N3 Cr N2 . 2_666 89.76(9)
N2 Cr N2 . 2_666 180.0
N3 Cr N1 . 2_666 90.60(9)
N2 Cr N1 . 2_666 94.61(11)
N3 Cr N1 . . 89.40(9)
N3 Cr N1 2_666 . 90.60(9)
N2 Cr N1 . . 85.39(11)
N2 Cr N1 2_666 . 94.61(11)
N1 Cr N1 2_666 . 180.0
O1 Cl O4 . . 121.9(6)
O1 Cl O2 . . 111.0(6)
O4 Cl O2 . . 106.7(7)
O1 Cl O3 . . 105.9(6)
O4 Cl O3 . . 106.5(6)
O2 Cl O3 . . 103.3(6)
C5 N1 C1 . . 114.5(3)
C5 N1 Cr . . 116.2(2)
C1 N1 Cr . . 105.6(2)
C2 N2 C3 . . 113.7(3)
C2 N2 Cr . . 106.3(2)
C3 N2 Cr . . 117.4(2)
C6 N3 Cr . . 160.6(2)
N1 C1 C2 . . 108.6(3)
N2 C2 C1 . . 108.4(3)
N2 C3 C4 . 2_666 111.8(3)
C5 C4 C3 . 2_666 116.4(3)
N1 C5 C4 . . 111.9(3)
N3 C6 S . . 176.3(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Cr N1 . 2.051(2)
Cr N1 2_666 2.051(2)
Cr N2 . 2.046(2)
Cr N2 2_666 2.046(2)
Cr N3 . 1.983(2)
Cr N3 2_666 1.983(2)
Cl O1 . 1.323(7)
Cl O1 2 1.323(7)
Cl O2 . 1.453(8)
Cl O2 2 1.453(8)
Cl O3 . 1.480(7)
Cl O3 2 1.480(7)
Cl O4 . 1.342(8)
Cl O4 2 1.342(8)
S C6 . 1.608(3)
N1 C1 . 1.486(5)
N1 C5 . 1.484(5)
N2 C2 . 1.473(4)
N2 C3 . 1.479(4)
N3 C6 . 1.161(3)
C1 C2 . 1.492(6)
C3 C4 2_666 1.510(6)
C4 C5 . 1.502(6)
C4 C3 2_666 1.510(6)
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 . . 127.0(2)
N3 Cr N1 C5 2_666 . -53.0(2)
N2 Cr N1 C5 . . -142.7(2)
N2 Cr N1 C5 2_666 . 37.3(2)
N3 Cr N1 C1 . . -104.8(2)
N3 Cr N1 C1 2_666 . 75.2(2)
N2 Cr N1 C1 . . -14.6(2)
N2 Cr N1 C1 2_666 . 165.4(2)
N3 Cr N2 C2 . . 74.6(2)
N3 Cr N2 C2 2_666 . -105.4(2)
N1 Cr N2 C2 2_666 . 165.2(2)
N1 Cr N2 C2 . . -14.8(2)
N3 Cr N2 C3 . . -53.9(2)
N3 Cr N2 C3 2_666 . 126.1(2)
N1 Cr N2 C3 2_666 . 36.8(2)
N1 Cr N2 C3 . . -143.2(2)
N2 Cr N3 C6 . . 9.4(6)
N2 Cr N3 C6 2_666 . -170.6(6)
N1 Cr N3 C6 2_666 . -85.2(6)
N1 Cr N3 C6 . . 94.8(6)
C5 N1 C1 C2 . . 170.7(3)
Cr N1 C1 C2 . . 41.6(3)
C3 N2 C2 C1 . . 172.4(3)
Cr N2 C2 C1 . . 41.8(3)
N1 C1 C2 N2 . . -57.2(4)
C2 N2 C3 C4 . 2_666 -178.4(3)
Cr N2 C3 C4 . 2_666 -53.6(3)
C1 N1 C5 C4 . . -179.1(3)
Cr N1 C5 C4 . . -55.5(3)
C3 C4 C5 N1 2_666 . 71.1(4)
Cr N3 C6 S . . 16.(4)