#------------------------------------------------------------------------------
#$Date: 2011-09-10 04:16:28 +0100 (Sat, 10 Sep 2011) $
#$Revision: 25271 $
#$URL: svn://www.crystallography.net/cod/cif/2/2202441.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_2202441
loop_
_publ_author_name
'Zhang, Feng'
'Zhang, Jian-Rong'
'Deng, Dao-Li'
'Hage, Ronald'
_publ_section_title
;
 (1,4,7,10,13-Pentamethyl-1,4,7,10,13-pentaazacyclopentadecane-\k^5^<i>N</i>)cobalt(II)
 perchlorate
;
_journal_issue                   12
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m1099
_journal_page_last               m1101
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Co (C15 H35 N5)] (Cl O4)2'
_chemical_formula_moiety         'C15 H35 Co N5 2+, 2Cl O4 1-'
_chemical_formula_sum            'C15 H35 Cl2 Co N5 O8'
_chemical_formula_weight         543.31
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 98.47(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4.00
_cell_length_a                   9.451(2)
_cell_length_b                   15.294(4)
_cell_length_c                   17.049(4)
_cell_measurement_reflns_used    20
_cell_measurement_temperature    293
_cell_measurement_theta_max      21.09
_cell_measurement_theta_min      13.67
_cell_volume                     2437.4(10)
_computing_cell_refinement       'MSC/AFC Diffractometer Control Software'
_computing_data_collection
;
MSC/AFC Diffractometer Control Software
(Molecular Structure Corporation, 1989)
;
_computing_data_reduction
'TEXSAN (Molecular Structure Corporation, 1989)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  TEXSAN
_computing_structure_refinement  TEXSAN
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      20.0
_diffrn_measurement_device       'Rigaku AFC-7R'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'X-ray tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0306
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            4450
_diffrn_reflns_theta_max         24.9895
_diffrn_reflns_theta_min         6.0
_diffrn_standards_decay_%        2.9
_diffrn_standards_interval_count 200
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.9711
_exptl_absorpt_correction_T_max  0.82
_exptl_absorpt_correction_T_min  0.79
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details
'(TEXSAN; Molecular Structure Corporation, 1989)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.480
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1140.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.200
_refine_diff_density_max         0.69500
_refine_diff_density_min         -0.36570
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.750
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2297
_refine_ls_number_restraints     0
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.0050
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo)]'
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_ref         0.0610
_reflns_number_gt                2297
_reflns_number_total             4165
_reflns_threshold_expression     I>3\s(I)
_[local]_cod_data_source_file    cf6283.cif
_[local]_cod_data_source_block   I
_[local]_cod_cif_authors_sg_H-M  'P 21/n'
_cod_original_cell_volume        2437.0(10)
_cod_database_code               2202441
loop_
_symmetry_equiv_pos_as_xyz
'   +x,   +y,   +z'
1/2-x,1/2+y,1/2-z
'   -x,   -y,   -z'
1/2+x,1/2-y,1/2+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
Co 0.0477(5) 0.0263(4) 0.0373(5) -0.0046(5) 0.0044(4) 0.0012(4)
Cl1 0.0590(10) 0.0610(10) 0.0510(10) -0.0060(10) 0.0087(9) -0.0080(10)
Cl2 0.084(2) 0.0520(10) 0.0600(10) 0.0080(10) 0.0250(10) 0.0030(10)
O1 0.105(5) 0.063(4) 0.162(7) -0.014(4) 0.037(5) 0.005(4)
O2 0.128(5) 0.128(6) 0.056(4) -0.036(5) 0.001(4) -0.036(4)
O3 0.065(4) 0.136(6) 0.094(5) -0.006(4) 0.029(3) -0.048(4)
O4 0.095(5) 0.124(6) 0.087(5) 0.037(4) 0.014(4) 0.017(4)
O5 0.112(7) 0.205(9) 0.152(8) -0.012(6) -0.011(6) -0.078(7)
O6 0.260(10) 0.204(9) 0.141(7) 0.151(8) 0.144(8) 0.099(7)
O7 0.320(10) 0.118(7) 0.116(6) 0.064(8) 0.073(7) 0.070(6)
O8 0.105(6) 0.125(6) 0.280(10) -0.024(5) 0.042(6) -0.122(7)
N1 0.050(4) 0.038(3) 0.051(4) 0.001(3) 0.010(3) -0.002(3)
N2 0.073(4) 0.034(3) 0.054(4) -0.011(3) 0.015(3) 0.004(3)
N3 0.077(5) 0.036(3) 0.047(4) -0.006(3) 0.014(3) -0.005(3)
N4 0.041(3) 0.034(3) 0.052(3) -0.005(3) 0.013(3) 0.005(3)
N5 0.049(4) 0.048(4) 0.050(4) 0.002(3) 0.003(3) -0.006(3)
C1 0.079(6) 0.054(5) 0.061(5) 0.000(4) 0.033(4) 0.003(4)
C2 0.082(6) 0.061(5) 0.088(6) -0.021(5) 0.042(5) 0.004(5)
C3 0.090(6) 0.064(5) 0.067(6) -0.040(5) 0.010(5) -0.003(4)
C4 0.115(7) 0.052(5) 0.059(5) -0.030(5) 0.023(5) -0.016(4)
C5 0.078(6) 0.050(5) 0.043(4) -0.007(4) 0.008(4) -0.005(3)
C6 0.072(5) 0.046(5) 0.048(4) 0.003(4) 0.020(4) 0.005(3)
C7 0.064(5) 0.049(5) 0.064(5) -0.019(4) 0.016(4) -0.002(4)
C8 0.047(5) 0.061(5) 0.083(6) -0.014(4) 0.011(4) -0.012(5)
C9 0.066(5) 0.062(5) 0.065(5) -0.004(4) -0.005(4) -0.024(4)
C10 0.076(6) 0.062(5) 0.056(5) -0.002(4) 0.012(4) -0.015(4)
C11 0.078(6) 0.044(4) 0.071(5) 0.018(4) 0.025(4) 0.004(4)
C12 0.118(8) 0.051(5) 0.079(6) -0.009(5) 0.017(5) 0.010(5)
C13 0.099(7) 0.048(5) 0.074(6) 0.012(5) 0.016(5) -0.004(4)
C14 0.070(5) 0.061(5) 0.057(5) 0.019(4) 0.015(4) 0.017(4)
C15 0.077(6) 0.068(6) 0.069(5) 0.020(4) -0.024(5) -0.010(4)
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
Co 0.26413(9) 0.22704(5) 0.41065(5) 0.0373 Uani
Cl1 0.7445(2) 0.17720(10) 0.57870(10) 0.0571 Uani
Cl2 0.2845(2) 0.01700(10) 0.78890(10) 0.0639 Uani
O1 0.8092(7) 0.2540(4) 0.5575(5) 0.1081 Uani
O2 0.6774(7) 0.1331(4) 0.5102(3) 0.1057 Uani
O3 0.6424(6) 0.1961(4) 0.6293(3) 0.0965 Uani
O4 0.8538(7) 0.1219(5) 0.6178(4) 0.1019 Uani
O5 0.4309(9) 0.0152(6) 0.8169(5) 0.1595 Uani
O6 0.2040(10) 0.0163(6) 0.8491(5) 0.1899 Uani
O7 0.2540(10) 0.0902(5) 0.7459(5) 0.1821 Uani
O8 0.2613(8) -0.0579(5) 0.7431(6) 0.1682 Uani
N1 0.3516(6) 0.1456(3) 0.3213(3) 0.0461 Uani
N2 0.4157(6) 0.3142(4) 0.3766(3) 0.0530 Uani
N3 0.2420(7) 0.3355(3) 0.4952(3) 0.0527 Uani
N4 0.2197(5) 0.1485(3) 0.5088(3) 0.0418 Uani
N5 0.0689(6) 0.1782(4) 0.3532(3) 0.0494 Uani
C1 0.4590(9) 0.1985(5) 0.2858(5) 0.0627 Uani
C2 0.5289(9) 0.2622(5) 0.3452(5) 0.0739 Uani
C3 0.4769(9) 0.3588(5) 0.4514(5) 0.0737 Uani
C4 0.3590(10) 0.4000(5) 0.4888(5) 0.0743 Uani
C5 0.2702(8) 0.2904(5) 0.5726(4) 0.0567 Uani
C6 0.1815(8) 0.2085(4) 0.5708(4) 0.0541 Uani
C7 0.0955(8) 0.0940(5) 0.4785(5) 0.0583 Uani
C8 -0.0064(8) 0.1421(5) 0.4169(5) 0.0637 Uani
C9 0.0993(8) 0.1079(5) 0.2969(5) 0.0659 Uani
C10 0.2283(9) 0.1279(5) 0.2607(5) 0.0648 Uani
C11 0.4180(8) 0.0632(5) 0.3531(5) 0.0626 Uani
C12 0.3520(10) 0.3781(5) 0.3168(5) 0.0821 Uani
C13 0.1053(10) 0.3818(5) 0.4893(5) 0.0733 Uani
C14 0.3356(8) 0.0901(5) 0.5454(4) 0.0623 Uani
C15 -0.0212(9) 0.2460(5) 0.3082(5) 0.0749 Uani
H1 0.4138 0.2305 0.2419 0.0715 Uiso
H2 0.5294 0.1605 0.2693 0.0715 Uiso
H3 0.5857 0.2294 0.3898 0.0873 Uiso
H4 0.5960 0.2980 0.3238 0.0715 Uiso
H5 0.5254 0.3170 0.4876 0.0715 Uiso
H6 0.5441 0.4023 0.4410 0.0715 Uiso
H7 0.3175 0.4475 0.4547 0.0734 Uiso
H8 0.3931 0.4231 0.5389 0.0715 Uiso
H9 0.3693 0.2753 0.5837 0.0715 Uiso
H10 0.2478 0.3283 0.6135 0.0715 Uiso
H11 0.1963 0.1803 0.6205 0.0715 Uiso
H12 0.0821 0.2236 0.5579 0.0715 Uiso
H13 0.0454 0.0787 0.5218 0.0715 Uiso
H14 0.1255 0.0427 0.4555 0.0715 Uiso
H15 -0.0498 0.1896 0.4423 0.0715 Uiso
H16 -0.0811 0.1036 0.3947 0.0715 Uiso
H17 0.1136 0.0543 0.3252 0.0715 Uiso
H18 0.0192 0.1022 0.2563 0.0715 Uiso
H19 0.2498 0.0801 0.2290 0.0715 Uiso
H20 0.2105 0.1786 0.2278 0.0715 Uiso
H21 0.4587 0.0328 0.3135 0.0715 Uiso
H22 0.3510 0.0275 0.3738 0.0715 Uiso
H23 0.4948 0.0767 0.3960 0.0946 Uiso
H24 0.2605 0.3982 0.3309 0.0715 Uiso
H25 0.4110 0.4277 0.3153 0.0715 Uiso
H26 0.3326 0.3522 0.2660 0.0715 Uiso
H27 0.1101 0.4247 0.5296 0.0715 Uiso
H28 0.0853 0.4090 0.4387 0.0715 Uiso
H29 0.0311 0.3412 0.4951 0.0715 Uiso
H30 0.4143 0.1242 0.5707 0.0715 Uiso
H31 0.3679 0.0546 0.5057 0.0715 Uiso
H32 0.3021 0.0537 0.5839 0.0715 Uiso
H33 -0.0387 0.2932 0.3407 0.0715 Uiso
H34 0.0353 0.2712 0.2677 0.0883 Uiso
H35 -0.1046 0.2235 0.2800 0.0715 Uiso
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C 0.003 0.002 'International Tables'
H 0.000 0.000 'International Tables'
N 0.006 0.003 'International Tables'
O 0.011 0.006 'International Tables'
Co 0.349 0.972 'International Tables'
Cl 0.148 0.159 'International Tables'
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
N1 Co N2 80.1(2) y
N1 Co N3 160.4(2) y
N1 Co N4 110.9(2) y
N1 Co N5 82.6(2) y
N2 Co N3 80.7(2) y
N2 Co N4 142.1(2) y
N2 Co N5 133.4(2) y
N3 Co N4 82.2(2) y
N3 Co N5 114.1(2) y
N4 Co N5 84.6(2) y
O(1) Cl(1) O(2) 110.3(4) no
O(1) Cl(1) O(3) 110.5(4) no
O(1) Cl(1) O(4) 107.8(4) no
O(2) Cl(1) O(3) 109.7(4) no
O(2) Cl(1) O(4) 108.0(4) no
O(3) Cl(1) O(4) 110.4(4) no
O(5) Cl(2) O(6) 112.0(6) no
O(5) Cl(2) O(7) 108.8(7) no
O(5) Cl(2) O(8) 104.1(5) no
O(6) Cl(2) O(7) 108.7(5) no
O(6) Cl(2) O(8) 111.1(6) no
O(7) Cl(2) O(8) 112.2(6) no
Co N(1) C(1) 108.5(4) no
Co N(1) C(10) 104.4(4) no
Co N(1) C(11) 114.1(4) no
C(1) N(1) C(10) 109.4(6) no
C(1) N(1) C(11) 109.5(6) no
C(10) N(1) C(11) 110.7(6) no
Co N(2) C(2) 108.3(4) no
Co N(2) C(3) 104.4(4) no
Co N(2) C(12) 112.6(5) no
C(2) N(2) C(3) 110.0(6) no
C(2) N(2) C(12) 110.3(6) no
C(3) N(2) C(12) 111.0(6) no
Co N(3) C(4) 107.7(4) no
Co N(3) C(5) 102.1(4) no
Co N(3) C(13) 118.8(5) no
C(4) N(3) C(5) 109.6(6) no
C(4) N(3) C(13) 109.1(6) no
C(5) N(3) C(13) 109.2(6) no
Co N(4) C(6) 107.8(4) no
Co N(4) C(7) 106.3(4) no
Co N(4) C(14) 116.6(4) no
C(6) N(4) C(7) 109.6(5) no
C(6) N(4) C(14) 108.5(5) no
C(7) N(4) C(14) 108.0(6) no
Co N(5) C(8) 105.9(4) no
Co N(5) C(9) 108.5(4) no
Co N(5) C(15) 113.0(4) no
C(8) N(5) C(9) 111.1(6) no
C(8) N(5) C(15) 109.7(6) no
C(9) N(5) C(15) 108.6(6) no
N(1) C(1) C(2) 109.9(6) no
N(2) C(2) C(1) 108.8(6) no
N(2) C(3) C(4) 109.6(7) no
N(3) C(4) C(3) 110.8(6) no
N(3) C(5) C(6) 110.1(6) no
N(4) C(6) C(5) 109.7(5) no
N(4) C(7) C(8) 111.3(6) no
N(5) C(8) C(7) 111.3(6) no
N(5) C(9) C(10) 111.6(6) no
N(1) C(10) C(9) 111.4(6) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_publ_flag
Co N1 2.220(5) y
Co N2 2.101(5) y
Co N3 2.228(5) y
Co N4 2.151(5) y
Co N5 2.095(5) y
Cl(1) O(1) 1.396(6) no
Cl(1) O(2) 1.414(5) no
Cl(1) O(3) 1.416(5) no
Cl(1) O(4) 1.423(6) no
Cl(2) O(5) 1.397(8) no
Cl(2) O(6) 1.363(7) no
Cl(2) O(7) 1.346(7) no
Cl(2) O(8) 1.384(7) no
N1 C1 1.493(9) y
N1 C10 1.464(9) y
N1 C11 1.474(8) y
N2 C2 1.494(9) y
N2 C3 1.486(9) y
N2 C12 1.476(10) y
N3 C4 1.495(9) y
N3 C5 1.477(8) y
N3 C13 1.464(9) y
N4 C6 1.483(8) y
N4 C7 1.470(8) y
N4 C14 1.479(8) y
N5 C8 1.489(9) y
N5 C9 1.497(9) y
N5 C15 1.482(9) y
C(1) C(2) 1.490(10) no
C(3) C(4) 1.510(10) no
C(5) C(6) 1.505(9) no
C(7) C(8) 1.510(10) no
C(9) C(10) 1.480(10) no