#------------------------------------------------------------------------------
#$Date: 2017-07-10 18:33:26 +0300 (Mon, 10 Jul 2017) $
#$Revision: 198601 $
#$URL: file:///home/coder/svn-repositories/cod/cif/2/00/75/2007550.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_2007550
loop_
_publ_author_name
'Hideaki Kanno'
'Shunji Utsuno'
'Junnosuke Fujita'
'Kinya Iijima'
_publ_section_title
;Absolute Configuration of (+)₅₈₉-(4,4'-Dimethoxy-2,2'-bipyridine
 1,1'-dioxide-O,O')bis(ethylene-diamine-N,N')cobalt(III)
 Triperchlorate
;
_journal_issue                   8
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1083
_journal_page_last               1085
_journal_paper_doi               10.1107/S0108270198002959
_journal_volume                  54
_journal_year                    1998
_chemical_formula_moiety         '[Co (C2 H8 N2)2 (C12 H12 N2 O4)] (ClO4)3'
_chemical_formula_sum            'C16 H28 Cl3 Co N6 O16'
_chemical_formula_weight         725.7
_space_group_IT_number           18
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2bc 2'
_symmetry_space_group_name_H-M   'P 2 21 21'
_atom_type_scat_source           IntTabC
_cell_angle_alpha                90.
_cell_angle_beta                 90.
_cell_angle_gamma                90.
_cell_formula_units_Z            2
_cell_length_a                   11.280(3)
_cell_length_b                   13.417(2)
_cell_length_c                   8.986(2)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    298
_cell_measurement_theta_max      17.5
_cell_measurement_theta_min      15.6
_cell_volume                     1360.0(5)
_computing_cell_refinement
'MXC Operation Manual (Mac Science Co. Ltd, 1989)'
_computing_data_collection       'MXC Operation Manual'
_computing_data_reduction        'CRYSTAN-GM (Gilmore & Brown, 1988)'
_computing_molecular_graphics    CRYSTAN-GM
_computing_publication_material  CRYSTAN-GM
_computing_structure_refinement  CRYSTAN-GM
_computing_structure_solution    CRYSTAN-GM
_diffrn_measurement_device       'Mac Science MXC3'
_diffrn_measurement_method       2θ/ω
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3618
_diffrn_reflns_theta_max         26.47
_diffrn_standards_decay_%        <1
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.012
_exptl_absorpt_correction_T_max  0.833
_exptl_absorpt_correction_T_min  0.749
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_density_meas      1.80
_exptl_crystal_density_method
'flotation in a mixture of chloroform and 1,2-dibromoethane'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.11
_refine_diff_density_min         -0.52
_refine_ls_abs_structure_details
; all Bijvoet pairs of reflections were measured and used for
  determination of the absolute structure; the final absolute
  structure is the one which converged the Rogers parameter, η, to
  1.01(6)
;
_refine_ls_abs_structure_Rogers  '\h = 1.01(6)'
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.433
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     192
_refine_ls_number_reflns         3180
_refine_ls_R_factor_gt           0.056
_refine_ls_shift/su_max          0.0029
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[σ²(F) + 0.005F²]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.070
_reflns_number_gt                3180
_reflns_number_total             3618
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            oa1050.cif
_cod_data_source_block           oa1050
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value '\y scan' was replaced with
the value 'psi-scan' as specified in the replacement file
'src/cod-tools/trunk/data/replacement-values/replacement_values.lst'.

Automatic conversion script
Id: cif_fix_values 5376 2017-05-30 11:51:03Z andrius 
;
_cod_original_sg_symbol_H-M      'P 2 21 21 '
_cod_original_formula_sum        'C16 H28 O16 N6 Cl3 Co1'
_cod_database_code               2007550
_cod_database_fobs_code          2007550
loop_
_symmetry_equiv_pos_as_xyz
+X,+Y,+Z
-X,-Y+0.5,+Z+0.5
+X,-Y,-Z
-X,+Y+0.5,-Z+0.5
loop_
_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_occupancy
Co1 -.23305(6) .00000 .00000 .0253(2) Uani .500
O1 -.1147(2) .0879(2) .0767(3) .0290(10) Uani 1.000
N1 -.0253(3) .1120(2) -.0193(3) .0260(10) Uani 1.000
C1 .0640(3) .0476(3) -.0413(4) .027(2) Uani 1.000
C2 .1572(3) .0714(3) -.1345(4) .031(2) Uani 1.000
C3 .1555(4) .1642(3) -.2075(5) .033(2) Uani 1.000
C4 .0637(4) .2316(3) -.1772(5) .037(2) Uani 1.000
C5 -.0247(3) .2044(3) -.0821(5) .033(2) Uani 1.000
O2 .2369(3) .1932(2) -.3065(4) .047(2) Uani 1.000
C6 .3343(5) .1256(5) -.3400(7) .067(3) Uani 1.000
N11 -.3490(3) -.0957(3) -.0821(4) .038(2) Uani 1.000
C12 -.3474(5) -.0852(4) -.2474(6) .053(3) Uani 1.000
C13 -.3411(5) .0215(4) -.2782(6) .055(3) Uani 1.000
N14 -.2377(3) .0624(2) -.1963(3) .035(2) Uani 1.000
Cl1 -.00194(18) .00000 .50000 .0566(5) Uani .500
O11 -.0550(9) .0667(6) .5885(9) .187(8) Uani 1.000
O12 .0812(8) .0573(5) .4168(10) .153(6) Uani 1.000
Cl2 -.34114(11) .30321(9) -.33050(17) .0535(6) Uani 1.000
O21 -.2197(5) .2930(5) -.3320(7) .119(5) Uani 1.000
O22 -.3761(4) .4036(3) -.3469(10) .118(4) Uani 1.000
O23 -.3851(6) .2621(4) -.2004(6) .103(4) Uani 1.000
O24 -.3902(8) .2520(5) -.4503(7) .153(6) Uani 1.000
H2 .2217 .0258 -.1497 .060 Uiso 1.000
H4 .0638 .2960 -.2237 .060 Uiso 1.000
H5 -.0872 .2505 -.0589 .060 Uiso 1.000
H6A .3925 .1468 -.4113 .060 Uiso 1.000
H6B .29905 .06538 -.37697 .060 Uiso 1.000
H6C .37525 .11118 -.24877 .060 Uiso 1.000
H11A -.32389 -.16229 -.05853 .060 Uiso 1.000
H11B -.42639 -.08109 -.04333 .060 Uiso 1.000
H12A -.41825 -.11281 -.28970 .060 Uiso 1.000
H12B -.27985 -.11891 -.28860 .060 Uiso 1.000
H13A -.41280 .05365 -.24626 .060 Uiso 1.000
H13B -.33100 .03235 -.38306 .060 Uiso 1.000
H14A -.24798 .13303 -.18409 .060 Uiso 1.000
H14B -.16588 .04773 -.24929 .060 Uiso 1.000
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
_geom_angle_publ_flag
O1 Co1 O1 . 3_555 91.3(2) yes
O1 Co1 N11 . . 177.1(2) yes
O1 Co1 N11 . 3_555 85.8(2) yes
O1 Co1 N14 . . 94.6(2) yes
O1 Co1 N14 . 3_555 87.6(2) yes
N11 Co1 N11 . 3_555 97.1(2) yes
N11 Co1 N14 . . 85.6(2) yes
N11 Co1 N14 . 3_555 92.3(2) yes
N14 Co1 N14 . 3_555 176.9(2) yes
Co1 O1 N1 . . 115.8(3) yes
O1 N1 C1 . . 119.6(3) yes
O1 N1 C5 . . 118.8(3) yes
C1 N1 C5 . . 121.4(4) yes
N1 C1 C1 . 3_555 118.9(4) yes
N1 C1 C2 . . 120.8(4) yes
C1 C1 C2 3_555 . 120.3(4) yes
C1 C2 C3 . . 118.5(4) yes
C2 C3 C4 . . 119.4(4) yes
C2 C3 O2 . . 124.0(4) yes
C4 C3 O2 . . 116.7(4) yes
C3 C4 C5 . . 119.3(4) yes
N1 C5 C4 . . 120.5(4) yes
C3 O2 C6 . . 118.3(4) yes
Co1 N11 C12 . . 107.6(3) yes
N11 C12 C13 . . 106.3(5) yes
C12 C13 N14 . . 107.9(5) yes
Co1 N14 C13 . . 108.1(3) yes
O11 Cl1 O11 . 3_556 126.9(6) no
O11 Cl1 O12 . . 104.2(5) no
O11 Cl1 O12 . 3_556 110.1(5) no
O12 Cl1 O12 . 3_556 97.7(5) no
O21 Cl2 O22 . . 111.8(4) no
O21 Cl2 O23 . . 109.0(4) no
O21 Cl2 O24 . . 109.8(5) no
O22 Cl2 O23 . . 111.6(5) no
O22 Cl2 O24 . . 106.2(5) no
O23 Cl2 O24 . . 108.3(4) no
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 O1 . . 1.910(3) yes
Co1 N11 . . 1.976(4) yes
Co1 N14 . . 1.953(4) yes
O1 N1 . . 1.365(4) yes
N1 C1 . . 1.342(5) yes
N1 C5 . . 1.361(5) yes
C1 C1 . 3_555 1.478(5) yes
C1 C2 . . 1.381(6) yes
C2 C3 . . 1.408(6) yes
C3 C4 . . 1.401(6) yes
C3 O2 . . 1.337(6) yes
C4 C5 . . 1.364(6) yes
O2 C6 . . 1.456(7) yes
N11 C12 . . 1.492(7) yes
C12 C13 . . 1.461(8) yes
C13 N14 . . 1.484(7) yes
Cl1 O11 . . 1.338(9) no
Cl1 O12 . . 1.424(9) no
Cl2 O21 . . 1.377(6) no
Cl2 O22 . . 1.411(5) no
Cl2 O23 . . 1.385(6) no
Cl2 O24 . . 1.392(8) no
