#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/06/2010630.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_2010630
loop_
_publ_author_name
'Farrugia, Louis J.'
'Peacock, Robert D.'
'Stewart, Brian'
_publ_section_title
;
 Redetermination of the double salt
 Λ-[tris(ethylenediamine)cobalt(III) trichloride]--sodium
 chloride--water (2/1/6)
;
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              149
_journal_page_last               151
_journal_paper_doi               10.1107/S0108270199013116
_journal_volume                  56
_journal_year                    2000
_chemical_formula_iupac          '[Co(C2 H8 N2)3]2 Cl6, Na1 Cl1, 6H2 O1'
_chemical_formula_moiety         '2C6 H24 Co N6 3+, 6Cl 1-, H12 Cl 1 Na O6'
_chemical_formula_sum            'C12 H60 Cl7 Co2 N12 Na O6'
_chemical_formula_weight         857.72
_chemical_name_systematic        ?
_space_group_IT_number           143
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'P 3'
_symmetry_space_group_name_H-M   'P 3'
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.1beta5
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            1
_cell_length_a                   11.415(4)
_cell_length_b                   11.415(4)
_cell_length_c                   8.0552(8)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      11.6
_cell_volume                     909.0(5)
_computing_cell_refinement       'CAD-4 EXPRESS'
_computing_data_collection       'CAD-4 EXPRESS (Enraf Nonius, 1992)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1996)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1993)'
_diffrn_ambient_temperature      291(2)
_diffrn_measured_fraction_theta_full .999
_diffrn_measured_fraction_theta_max .999
_diffrn_measurement_device       'Enraf Nonius Turbo CAD-4'
_diffrn_measurement_method       'non-profiled ω/2θ'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .017
_diffrn_reflns_av_sigmaI/netI    .0155
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            2484
_diffrn_reflns_theta_full        25.86
_diffrn_reflns_theta_max         25.86
_diffrn_reflns_theta_min         2.53
_diffrn_standards_decay_%        26
_diffrn_standards_interval_count 118
_diffrn_standards_interval_time  120
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    1.484
_exptl_absorpt_correction_T_max  .512
_exptl_absorpt_correction_T_min  .419
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(North et al., 1968)'
_exptl_crystal_colour            orange-brown
_exptl_crystal_density_diffrn    1.567
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description
'approximate trapezoid cleaved from larger crystal'
_exptl_crystal_F_000             448
_exptl_crystal_size_max          .7
_exptl_crystal_size_mid          .6
_exptl_crystal_size_min          .4
_refine_diff_density_max         .64
_refine_diff_density_min         -.61
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   .07(5)
_refine_ls_extinction_coef       .040(5)
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.198
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     130
_refine_ls_number_reflns         1440
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.198
_refine_ls_R_factor_all          .047
_refine_ls_R_factor_gt           .047
_refine_ls_shift/su_max          .002
_refine_ls_shift/su_mean         .000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0620P)²+3.2274P] where P = (Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         .144
_reflns_number_gt                1429
_reflns_number_total             1440
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            ka1333.cif
_cod_data_source_block           I
_cod_database_code               2010630
_cod_database_fobs_code          2010630
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
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_calc_flag
_atom_site_refinement_flags
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_type_symbol
Co1 .0000 .0000 .0000 .0218(5) Uani d S 1 . . Co
Cl1 .0510(3) .2329(3) .5216(4) .0345(6) Uani d . 1 . . Cl
C11 -.1076(11) .1688(11) -.0846(13) .036(2) Uani d . 1 . . C
H11A -.1883 .1715 -.1157 .043 Uiso calc R 1 . . H
H11B -.0302 .2446 -.1366 .043 Uiso calc R 1 . . H
C12 -.0913(11) .1778(10) .1005(12) .033(2) Uani d . 1 . . C
H12A -.0682 .2672 .1395 .040 Uiso calc R 1 . . H
H12B -.1742 .1114 .1545 .040 Uiso calc R 1 . . H
N11 -.1187(6) .0394(6) -.1406(9) .0261(14) Uani d . 1 . . N
H11C -.0935 .0462 -.2476 .031 Uiso calc R 1 . . H
H11D -.2050 -.0281 -.1319 .031 Uiso calc R 1 . . H
N12 .0208(7) .1496(7) .1353(10) .0319(16) Uani d . 1 . . N
H12C .0198 .1292 .2434 .038 Uiso calc R 1 . . H
H12D .1008 .2238 .1130 .038 Uiso calc R 1 . . H
Co2 .3333 .6667 .5042(3) .0238(5) Uani d S 1 . . Co
Cl2 .2810(3) .4338(3) .0236(4) .0394(7) Uani d . 1 . . Cl
C21 .4369(12) .4978(11) .4160(12) .037(2) Uani d . 1 . . C
H21A .5154 .4925 .3808 .045 Uiso calc R 1 . . H
H21B .3571 .4237 .3656 .045 Uiso calc R 1 . . H
C22 .4245(11) .4890(11) .6063(13) .037(2) Uani d . 1 . . C
H22A .4026 .4000 .6456 .044 Uiso calc R 1 . . H
H22B .5075 .5565 .6589 .044 Uiso calc R 1 . . H
N21 .4507(7) .6265(7) .3659(10) .0339(16) Uani d . 1 . . N
H21C .4275 .6227 .2585 .041 Uiso calc R 1 . . H
H21D .5374 .6927 .3774 .041 Uiso calc R 1 . . H
N22 .3109(8) .5159(8) .6394(10) .0377(17) Uani d . 1 . . N
H22C .3103 .5354 .7475 .045 Uiso calc R 1 . . H
H22D .2314 .4417 .6153 .045 Uiso calc R 1 . . H
Na1A .6667 .3333 .2632(10) .0451(13) Uani d SP .734(16) . . Na
Na1B .6667 .3333 .7626(8) .0490(10) Uani d SP .266(16) . . Na
Cl3A .6667 .3333 .7626(8) .0490(10) Uani d SP .734(16) . . Cl
Cl3B .6667 .3333 .2632(10) .0451(13) Uani d SP .266(16) . . Cl
O1A .7740(12) .2424(13) .4532(17) .054(3) Uani d P .734(16) . . O
O1B .777(2) .251(2) .581(3) .026(6) Uiso d P .266(16) . . O
O2A .8601(12) .4447(12) .0803(14) .047(3) Uani d P .734(16) . . O
O2B .863(3) .437(3) -.031(4) .038(7) Uiso d P .266(16) . . O
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
Co Co .3494 .9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl .1484 .1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na .0362 .0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O .0106 .006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0 0 '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
7 0 -4
5 3 -3
3 0 4
-2 2 6
1 8 -2
5 4 -10
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
N12 Co1 N12 2 . 91.5(3) y
N12 Co1 N12 2 3 91.5(3) ?
N12 Co1 N12 . 3 91.5(3) ?
N12 Co1 N11 2 2 85.3(3) ?
N12 Co1 N11 . 2 174.6(3) ?
N12 Co1 N11 3 2 92.9(3) ?
N12 Co1 N11 2 . 92.9(3) y
N12 Co1 N11 . . 85.3(3) y
N12 Co1 N11 3 . 174.6(3) ?
N11 Co1 N11 2 . 90.6(3) ?
N12 Co1 N11 2 3 174.6(3) ?
N12 Co1 N11 . 3 92.9(3) y
N12 Co1 N11 3 3 85.3(3) ?
N11 Co1 N11 2 3 90.6(3) ?
N11 Co1 N11 . 3 90.6(3) ?
N11 C11 C12 . . 108.4(8) ?
N12 C12 C11 . . 105.2(8) ?
C11 N11 Co1 . . 108.9(6) ?
C12 N12 Co1 . . 110.1(6) ?
N22 Co2 N22 3_565 2_665 91.7(3) ?
N22 Co2 N22 3_565 . 91.7(3) ?
N22 Co2 N22 2_665 . 91.7(3) y
N22 Co2 N21 3_565 2_665 92.5(3) ?
N22 Co2 N21 2_665 2_665 85.1(3) ?
N22 Co2 N21 . 2_665 174.8(3) ?
N22 Co2 N21 3_565 3_565 85.1(3) ?
N22 Co2 N21 2_665 3_565 174.8(3) ?
N22 Co2 N21 . 3_565 92.5(3) ?
N21 Co2 N21 2_665 3_565 91.0(3) ?
N22 Co2 N21 3_565 . 174.8(3) ?
N22 Co2 N21 2_665 . 92.5(3) y
N22 Co2 N21 . . 85.1(3) y
N21 Co2 N21 2_665 . 91.0(3) y
N21 Co2 N21 3_565 . 91.0(3) ?
N21 C21 C22 . . 107.6(8) ?
N22 C22 C21 . . 103.0(8) ?
C21 N21 Co2 . . 109.6(6) ?
C22 N22 Co2 . . 109.8(6) ?
O2A Na1A O2A 3_665 . 86.8(4) ?
O2A Na1A O2A 3_665 2_655 86.8(4) ?
O2A Na1A O2A . 2_655 86.8(4) ?
O2A Na1A O1A 3_665 . 92.3(4) ?
O2A Na1A O1A . . 94.8(4) ?
O2A Na1A O1A 2_655 . 178.2(5) ?
O2A Na1A O1A 3_665 2_655 178.2(5) ?
O2A Na1A O1A . 2_655 92.3(4) ?
O2A Na1A O1A 2_655 2_655 94.8(4) ?
O1A Na1A O1A . 2_655 86.1(5) ?
O2A Na1A O1A 3_665 3_665 94.8(4) ?
O2A Na1A O1A . 3_665 178.2(5) ?
O2A Na1A O1A 2_655 3_665 92.3(4) ?
O1A Na1A O1A . 3_665 86.1(5) ?
O1A Na1A O1A 2_655 3_665 86.1(5) ?
O2A Na1A Na1B 3_665 . 127.5(3) ?
O2A Na1A Na1B . . 127.5(3) ?
O2A Na1A Na1B 2_655 . 127.5(3) ?
O1A Na1A Na1B . . 52.0(4) ?
O1A Na1A Na1B 2_655 . 52.0(4) ?
O1A Na1A Na1B 3_665 . 52.0(4) ?
O2A Na1A Na1B 3_665 1_554 52.5(3) ?
O2A Na1A Na1B . 1_554 52.5(3) ?
O2A Na1A Na1B 2_655 1_554 52.5(3) ?
O1A Na1A Na1B . 1_554 128.0(4) ?
O1A Na1A Na1B 2_655 1_554 128.0(4) ?
O1A Na1A Na1B 3_665 1_554 128.0(4) ?
Na1B Na1A Na1B . 1_554 180.0000(10) ?
O1B Na1B O1B . 3_665 86.8(8) ?
O1B Na1B O1B . 2_655 86.8(8) ?
O1B Na1B O1B 3_665 2_655 86.8(8) ?
O1B Na1B O2B . 1_556 94.0(9) ?
O1B Na1B O2B 3_665 1_556 176.2(10) ?
O1B Na1B O2B 2_655 1_556 97.0(9) ?
O1B Na1B O2B . 3_666 97.0(9) ?
O1B Na1B O2B 3_665 3_666 94.0(9) ?
O1B Na1B O2B 2_655 3_666 176.2(10) ?
O2B Na1B O2B 1_556 3_666 82.2(11) ?
O1B Na1B O2B . 2_656 176.2(10) ?
O1B Na1B O2B 3_665 2_656 97.0(9) ?
O1B Na1B O2B 2_655 2_656 94.0(9) ?
O2B Na1B O2B 1_556 2_656 82.2(11) ?
O2B Na1B O2B 3_666 2_656 82.2(11) ?
O1B Na1B Na1A . . 52.5(6) ?
O1B Na1B Na1A 3_665 . 52.5(6) ?
O1B Na1B Na1A 2_655 . 52.5(6) ?
O2B Na1B Na1A 1_556 . 130.6(7) ?
O2B Na1B Na1A 3_666 . 130.6(7) ?
O2B Na1B Na1A 2_656 . 130.6(7) ?
O1B Na1B Na1A . 1_556 127.5(6) ?
O1B Na1B Na1A 3_665 1_556 127.5(6) ?
O1B Na1B Na1A 2_655 1_556 127.5(6) ?
O2B Na1B Na1A 1_556 1_556 49.4(7) ?
O2B Na1B Na1A 3_666 1_556 49.4(7) ?
O2B Na1B Na1A 2_656 1_556 49.4(7) ?
Na1A Na1B Na1A . 1_556 180.000(2) ?
O1B O1A Na1A . . 124.9(16) ?
O1A O1B Na1B . . 130.2(18) ?
O2B O2A Na1A . . 128(2) ?
O2A O2B Na1B . 1_554 129(2) ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Co1 N12 2 1.938(7) ?
Co1 N12 . 1.938(7) y
Co1 N12 3 1.938(7) ?
Co1 N11 2 1.983(7) ?
Co1 N11 . 1.983(7) y
Co1 N11 3 1.983(7) ?
C11 N11 . 1.487(12) y
C11 C12 . 1.499(14) y
C12 N12 . 1.494(12) y
Co2 N22 3_565 1.942(8) ?
Co2 N22 2_665 1.942(8) ?
Co2 N22 . 1.942(8) y
Co2 N21 2_665 1.965(8) ?
Co2 N21 3_565 1.965(8) ?
Co2 N21 . 1.965(8) y
C21 N21 . 1.454(12) y
C21 C22 . 1.538(14) y
C22 N22 . 1.498(13) y
Na1A O2A 3_665 2.420(12) ?
Na1A O2A . 2.420(12) y
Na1A O2A 2_655 2.420(12) ?
Na1A O1A . 2.488(13) y
Na1A O1A 2_655 2.488(13) ?
Na1A O1A 3_665 2.488(13) ?
Na1A Na1B . 4.023(10) y
Na1A Na1B 1_554 4.032(10) ?
Na1B O1B . 2.41(2) y
Na1B O1B 3_665 2.41(2) ?
Na1B O1B 2_655 2.41(2) ?
Na1B O2B 1_556 2.55(3) y
Na1B O2B 3_666 2.55(3) ?
Na1B O2B 2_656 2.55(3) ?
Na1B Na1A 1_556 4.032(10) ?
O1A O1B . 1.03(3) y
O2A O2B . .90(3) y
O2B Na1B 1_554 2.55(3) ?
