#------------------------------------------------------------------------------
#$Date: 2016-02-21 02:03:34 +0200 (Sun, 21 Feb 2016) $
#$Revision: 176798 $
#$URL: svn://www.crystallography.net/cod/cif/2/23/57/2235708.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_2235708
loop_
_publ_author_name
'Tian, Ruijng'
'Yan, Yan'
'Zhang, Cailing'
'Wang, Liyan'
'Pan, Qinhe'
_publ_section_title
;
 Tris[hexaamminecobalt(III)] bis[trioxalatocobaltate(II)] chloride
 dodecahydrate
;
_journal_coeditor_code           YK2060
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              m914
_journal_page_last               m915
_journal_paper_doi               10.1107/S1600536812026414
_journal_volume                  68
_journal_year                    2012
_chemical_formula_iupac          '[Co (N H3)6] [Co (C2 O4)3] Cl, 12H2 O'
_chemical_formula_moiety
'3(Co H18 N6 3+), 2(C6 Co O12 4-), Cl -, 12(H2 O)'
_chemical_formula_sum            'C12 H78 Cl Co5 N18 O36'
_chemical_formula_weight         1381.02
_chemical_name_systematic
;
Tris[hexaamminecobalt(III)] bis[trioxalatocobaltate(II)] chloride
dodecahydrate
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            1
_cell_length_a                   12.2138(4)
_cell_length_b                   12.2138(4)
_cell_length_c                   9.9090(8)
_cell_measurement_reflns_used    7736
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      27.24
_cell_measurement_theta_min      2.06
_cell_volume                     1280.15(12)
_computing_cell_refinement       'SAINT (Bruker, 2005)'
_computing_data_collection       'APEX2 (Bruker, 2005)'
_computing_data_reduction        'SAINT (Bruker, 2005)'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 5.00
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD area-detector'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            7736
_diffrn_reflns_theta_full        27.24
_diffrn_reflns_theta_max         27.24
_diffrn_reflns_theta_min         2.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.753
_exptl_absorpt_correction_T_max  0.769
_exptl_absorpt_correction_T_min  0.737
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS; Bruker, 2005)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.791
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             716
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.613
_refine_diff_density_min         -1.088
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.159
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1923
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.159
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0482P)²+0.6892P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0993
_refine_ls_wR_factor_ref         0.1078
_reflns_number_gt                1514
_reflns_number_total             1923
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            yk2060.cif
_cod_data_source_block           I
_cod_database_code               2235708
_cod_database_fobs_code          2235708
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
loop_
_atom_site_type_symbol
_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_symmetry_multiplicity
Co Co1 0.6667 0.3333 0.14192(6) 0.02287(18) Uani d S 1 3
Co Co2 0.6667 0.3333 0.64732(5) 0.02393(18) Uani d S 1 3
Co Co3 0.0000 0.0000 0.0000 0.0646(5) Uani d S 1 6
Cl Cl1 0.0000 0.0000 0.5000 0.085(5) Uani d SP 0.498(19) 6
Cl Cl1' 0.0000 0.0000 0.3949(17) 0.118(4) Uani d SP 0.251(9) 3
O O1 0.3041(2) 0.0971(2) 0.2657(2) 0.0530(6) Uani d . 1 1
O O2 0.6796(2) 0.65788(19) 0.0164(2) 0.0454(6) Uani d . 1 1
O O3 0.64285(18) 0.45991(18) 0.02214(18) 0.0311(4) Uani d . 1 1
O O4 0.50524(17) 0.24996(18) 0.26488(18) 0.0291(4) Uani d . 1 1
N N1 -0.1492(2) -0.0618(3) 0.1172(4) 0.0725(11) Uani d . 1 1
H H1A -0.1436 -0.1075 0.1840 0.087 Uiso calc R 1 1
H H1B -0.2187 -0.1096 0.0692 0.087 Uiso calc R 1 1
H H1C -0.1528 0.0037 0.1514 0.087 Uiso calc R 1 1
N N2 0.6170(2) 0.4327(2) 0.5344(2) 0.0328(5) Uani d . 1 1
H H2B 0.6232 0.4999 0.5808 0.039 Uiso d R 1 1
H H2A 0.5333 0.3879 0.5132 0.039 Uiso d R 1 1
H H2 0.6626 0.4599 0.4568 0.039 Uiso d R 1 1
N N3 0.5188(2) 0.2924(2) 0.7604(2) 0.0307(5) Uani d . 1 1
H H3B 0.4436 0.2449 0.7175 0.037 Uiso d R 1 1
H H3A 0.5208 0.3659 0.7815 0.037 Uiso d R 1 1
H H3 0.5185 0.2514 0.8372 0.037 Uiso d R 1 1
C C1 0.4097(3) 0.1551(3) 0.2134(3) 0.0310(6) Uani d . 1 1
C C2 0.6835(2) 0.5688(2) 0.0718(3) 0.0288(6) Uani d . 1 1
O O1W 0.3354(2) 0.2406(3) 0.5187(3) 0.0747(9) Uani d . 1 1
H H1WA 0.2644 0.2152 0.5612 0.090 Uiso d R 1 1
H H1W 0.3234 0.1853 0.4567 0.090 Uiso d R 1 1
O O2W 0.5721(2) 0.5645(2) 0.7595(2) 0.0523(6) Uani d . 1 1
H H2WA 0.5434 0.6113 0.7265 0.063 Uiso d R 1 1
H H2W 0.5970 0.5901 0.8416 0.063 Uiso d R 1 1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
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
O3 Co1 O3 3_665 2_655 90.71(7)
O3 Co1 O3 3_665 . 90.71(7)
O3 Co1 O3 2_655 . 90.71(7)
O3 Co1 O4 3_665 2_655 78.45(7)
O3 Co1 O4 2_655 2_655 104.20(7)
O3 Co1 O4 . 2_655 161.53(7)
O3 Co1 O4 3_665 3_665 104.20(7)
O3 Co1 O4 2_655 3_665 161.53(7)
O3 Co1 O4 . 3_665 78.45(7)
O4 Co1 O4 2_655 3_665 89.66(7)
O3 Co1 O4 3_665 . 161.53(7)
O3 Co1 O4 2_655 . 78.45(7)
O3 Co1 O4 . . 104.20(7)
O4 Co1 O4 2_655 . 89.66(7)
O4 Co1 O4 3_665 . 89.66(7)
N2 Co2 N2 3_665 2_655 90.56(10)
N2 Co2 N2 3_665 . 90.56(10)
N2 Co2 N2 2_655 . 90.56(10)
N2 Co2 N3 3_665 2_655 91.47(10)
N2 Co2 N3 2_655 2_655 87.31(10)
N2 Co2 N3 . 2_655 177.07(9)
N2 Co2 N3 3_665 3_665 87.31(10)
N2 Co2 N3 2_655 3_665 177.07(9)
N2 Co2 N3 . 3_665 91.47(10)
N3 Co2 N3 2_655 3_665 90.74(9)
N2 Co2 N3 3_665 . 177.07(9)
N2 Co2 N3 2_655 . 91.47(10)
N2 Co2 N3 . . 87.31(10)
N3 Co2 N3 2_655 . 90.74(9)
N3 Co2 N3 3_665 . 90.74(9)
N1 Co3 N1 3 6 180.0(2)
N1 Co3 N1 3 5 91.36(15)
N1 Co3 N1 6 5 88.64(15)
N1 Co3 N1 3 . 88.64(15)
N1 Co3 N1 6 . 91.36(15)
N1 Co3 N1 5 . 91.36(15)
N1 Co3 N1 3 2 88.64(15)
N1 Co3 N1 6 2 91.36(15)
N1 Co3 N1 5 2 180.0(2)
N1 Co3 N1 . 2 88.64(15)
N1 Co3 N1 3 4 91.36(15)
N1 Co3 N1 6 4 88.64(15)
N1 Co3 N1 5 4 88.64(15)
N1 Co3 N1 . 4 180.0(2)
N1 Co3 N1 2 4 91.36(15)
Cl1' Cl1 Cl1' 4_556 . 180.000(2)
C2 O3 Co1 . . 115.64(17)
C1 O4 Co1 . . 114.93(16)
Co3 N1 H1A . . 109.5
Co3 N1 H1B . . 109.5
H1A N1 H1B . . 109.5
Co3 N1 H1C . . 109.5
H1A N1 H1C . . 109.5
H1B N1 H1C . . 109.5
Co2 N2 H2B . . 111.0
Co2 N2 H2A . . 111.2
H2B N2 H2A . . 102.8
Co2 N2 H2 . . 112.7
H2B N2 H2 . . 109.7
H2A N2 H2 . . 108.8
Co2 N3 H3B . . 113.7
Co2 N3 H3A . . 108.2
H3B N3 H3A . . 104.8
Co2 N3 H3 . . 111.6
H3B N3 H3 . . 108.4
H3A N3 H3 . . 109.9
O1 C1 O4 . . 125.1(3)
O1 C1 C2 . 2_655 119.5(2)
O4 C1 C2 . 2_655 115.4(2)
O2 C2 O3 . . 125.7(3)
O2 C2 C1 . 3_665 118.7(2)
O3 C2 C1 . 3_665 115.5(2)
H1WA O1W H1W . . 108.3
H2WA O2W H2W . . 107.4
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
Co1 O3 3_665 2.0817(18)
Co1 O3 2_655 2.0817(18)
Co1 O3 . 2.0817(18)
Co1 O4 2_655 2.0979(18)
Co1 O4 3_665 2.0979(18)
Co1 O4 . 2.0979(18)
Co2 N2 3_665 1.957(2)
Co2 N2 2_655 1.957(2)
Co2 N2 . 1.957(2)
Co2 N3 2_655 1.966(2)
Co2 N3 3_665 1.966(2)
Co2 N3 . 1.966(2)
Co3 N1 3 1.965(3)
Co3 N1 6 1.965(3)
Co3 N1 5 1.965(3)
Co3 N1 . 1.965(3)
Co3 N1 2 1.965(3)
Co3 N1 4 1.965(3)
Cl1 Cl1' 4_556 1.041(17)
Cl1 Cl1' . 1.041(17)
Cl1' Cl1' 4_556 2.08(3)
O1 C1 . 1.233(3)
O2 C2 . 1.240(3)
O3 C2 . 1.264(3)
O4 C1 . 1.270(3)
N1 H1A . 0.8900
N1 H1B . 0.8900
N1 H1C . 0.8900
N2 H2B . 0.9101
N2 H2A . 0.9100
N2 H2 . 0.9100
N3 H3B . 0.9100
N3 H3A . 0.9099
N3 H3 . 0.9100
C1 C2 2_655 1.553(4)
C2 C1 3_665 1.553(4)
O1W H1WA . 0.8700
O1W H1W . 0.8700
O2W H2WA . 0.8699
O2W H2W . 0.8700
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
N1 H1A Cl1' . 0.89 2.62 3.176(15) 121.4
N1 H1A O1 3 0.89 2.27 3.055(4) 146.6
N1 H1B O2 5_455 0.89 2.40 2.950(4) 120.1
N1 H1B O2 1_445 0.89 2.52 3.151(4) 128.4
N2 H2 O4 3_665 0.91 2.09 2.993(3) 170.7
N2 H2A O1W . 0.91 2.18 3.047(4) 160.1
N2 H2B O2W . 0.91 2.15 2.958(3) 146.8
N3 H3 O3 2_656 0.91 2.09 2.988(3) 171.6
N3 H3A O2W . 0.91 2.19 3.051(3) 157.0
N3 H3B O1W . 0.91 2.36 3.120(4) 141.3
O1W H1W O1 . 0.87 2.13 2.971(4) 162.3
O1W H1WA O1 6_556 0.87 2.32 2.973(4) 132.2
O2W H2W O2 1_556 0.87 1.97 2.830(3) 171.3
O2W H2WA O4 4_666 0.87 2.06 2.868(3) 154.4
