#------------------------------------------------------------------------------
#$Date: 2016-02-20 00:18:51 +0200 (Sat, 20 Feb 2016) $
#$Revision: 176760 $
#$URL: svn://www.crystallography.net/cod/cif/2/01/71/2017109.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_2017109
loop_
_publ_author_name
'Hammershøi, Anders'
'Magnussen, Magnus'
_publ_section_title
;
 Linkage isomeric oxamate chelates:
 rac-bis(ethane-1,2-diamine)oxamatocobalt(III)
 bis(trifluoromethanesulfonate) dihydrate and
 Λ(+)₅₇₈-bis(ethane-1,2-diamine)[oxamato(2{-})]cobalt(III)
 trifluoromethanesulfonate
;
_journal_coeditor_code           MX3011
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m201
_journal_page_last               m204
_journal_paper_doi               10.1107/S0108270109013122
_journal_volume                  65
_journal_year                    2009
_chemical_formula_iupac          '[Co (C2 H N O3) (C2 H8 N2)2] (C F3 S O3)'
_chemical_formula_moiety         'C6 H17 Co1 N5 O3 + , C F3 O3 S -'
_chemical_formula_sum            'C7 H17 Co F3 N5 O6 S'
_chemical_formula_weight         415.25
_chemical_name_systematic
;
Λ(+)₅₇₈-bis(ethane-1,2-diamine)[oxamato(2-)-
κ²N,O¹]cobalt(III) trifluoromethanesulfonate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90.00
_cell_angle_beta                 96.517(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   6.6398(4)
_cell_length_b                   11.6663(8)
_cell_length_c                   9.2846(10)
_cell_measurement_reflns_used    29543
_cell_measurement_temperature    122.0(10)
_cell_measurement_theta_max      50.0
_cell_measurement_theta_min      1.74
_cell_volume                     714.56(10)
_computing_cell_refinement       'COLLECT (Nonius, 1999)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'EvalCCD (Duisenberg et al.,  2003)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      122.0(10)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Nonius KappaCCD area-detector'
_diffrn_measurement_method       'ω and φ 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  0.0332
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            35436
_diffrn_reflns_theta_full        40.13
_diffrn_reflns_theta_max         40.13
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    1.422
_exptl_absorpt_correction_T_max  0.919
_exptl_absorpt_correction_T_min  0.714
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'Gaussian integration (Coppens, 1970)'
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    1.930
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             424
_exptl_crystal_size_max          0.196
_exptl_crystal_size_mid          0.129
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.483
_refine_diff_density_min         -0.747
_refine_ls_abs_structure_details 'Flack (1983), with 4283 Friedel pairs'
_refine_ls_abs_structure_Flack   0.000(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.056
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     211
_refine_ls_number_reflns         8895
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0212
_refine_ls_R_factor_gt           0.0194
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[σ²(Fo²)+(0.0149P)²+0.1524P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0459
_refine_ls_wR_factor_ref         0.0469
_reflns_number_gt                8611
_reflns_number_total             8895
_reflns_threshold_expression     I>2σ(I)
_cod_data_source_file            mx3011.cif
_cod_data_source_block           II
_cod_original_cell_volume        714.55(10)
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               2017109
_cod_database_fobs_code          2017109
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -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_disorder_assembly
_atom_site_disorder_group
Co Co1 0.174374(13) 0.001318(8) 0.537607(10) 0.00677(2) Uani d . 1 . .
N N1 0.44856(9) -0.02313(5) 0.61600(7) 0.00922(9) Uani d . 1 . .
H H1 0.527(2) 0.0286(13) 0.6563(16) 0.011 Uiso d . 1 . .
N N2 -0.10023(9) 0.00975(7) 0.43266(7) 0.00985(9) Uani d . 1 . .
H H2A -0.1733 -0.0542 0.4524 0.012 Uiso calc R 1 . .
H H2B -0.1665 0.0734 0.4621 0.012 Uiso calc R 1 . .
N N3 0.16535(11) 0.15728(6) 0.61048(8) 0.01126(10) Uani d . 1 . .
H H3A 0.2939 0.1815 0.6443 0.014 Uiso calc R 1 . .
H H3B 0.1140 0.2058 0.5372 0.014 Uiso calc R 1 . .
N N4 0.26676(10) 0.05468(6) 0.35651(7) 0.01059(10) Uani d . 1 . .
H H4A 0.3587 0.1132 0.3757 0.013 Uiso calc R 1 . .
H H4B 0.3305 -0.0043 0.3140 0.013 Uiso calc R 1 . .
N N5 0.07523(10) -0.04527(6) 0.72081(7) 0.00990(9) Uani d . 1 . .
H H5A -0.0562 -0.0710 0.7030 0.012 Uiso calc R 1 . .
H H5B 0.1538 -0.1041 0.7623 0.012 Uiso calc R 1 . .
O O1 0.70271(8) -0.15963(5) 0.61593(7) 0.01192(9) Uani d . 1 . .
O O2 0.18307(8) -0.15761(5) 0.48554(6) 0.00942(8) Uani d . 1 . .
O O3 0.38798(9) -0.30953(5) 0.51618(7) 0.01139(9) Uani d . 1 . .
C C2 0.35527(10) -0.20579(6) 0.52516(8) 0.00804(9) Uani d . 1 . .
C C1 0.52292(10) -0.12468(6) 0.59115(8) 0.00829(10) Uani d . 1 . .
C C21 -0.08354(11) 0.01674(7) 0.27406(8) 0.01256(12) Uani d . 1 . .
H H21A -0.2104 0.0476 0.2219 0.015 Uiso calc R 1 . .
H H21B -0.0585 -0.0602 0.2348 0.015 Uiso calc R 1 . .
C C31 0.03376(12) 0.15925(7) 0.72986(9) 0.01249(11) Uani d . 1 . .
H H31A -0.1109 0.1582 0.6898 0.015 Uiso calc R 1 . .
H H31B 0.0595 0.2295 0.7889 0.015 Uiso calc R 1 . .
C C41 0.09210(13) 0.09580(7) 0.25582(9) 0.01359(12) Uani d . 1 . .
H H41A 0.1252 0.0936 0.1545 0.016 Uiso calc R 1 . .
H H41B 0.0576 0.1756 0.2796 0.016 Uiso calc R 1 . .
C C51 0.08452(13) 0.05417(7) 0.82150(9) 0.01278(11) Uani d . 1 . .
H H51A 0.2219 0.0612 0.8746 0.015 Uiso calc R 1 . .
H H51B -0.0142 0.0445 0.8928 0.015 Uiso calc R 1 . .
S S1 0.58537(3) 0.297614(17) 0.86318(2) 0.01214(3) Uani d . 1 . .
O O11 0.57971(13) 0.17529(6) 0.84105(9) 0.02082(13) Uani d . 1 . .
O O12 0.46085(12) 0.36143(7) 0.75216(8) 0.02138(13) Uani d . 1 . .
O O13 0.78102(11) 0.34777(8) 0.90628(10) 0.02459(15) Uani d . 1 . .
C C11 0.45637(13) 0.31675(8) 1.02577(9) 0.01527(13) Uani d . 1 . .
F F11 0.44080(12) 0.42713(6) 1.05828(8) 0.02451(13) Uani d . 1 . .
F F12 0.56277(12) 0.26538(7) 1.13906(7) 0.02750(14) Uani d . 1 . .
F F13 0.27067(11) 0.27239(8) 1.01103(8) 0.02872(15) Uani d . 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'
Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
S S 0.1246 0.1234 '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
_geom_angle_publ_flag
N1 Co1 O2 . . 84.07(3) ?
N1 Co1 N3 . . 94.19(3) ?
O2 Co1 N3 . . 174.22(3) ?
N1 Co1 N4 . . 89.81(3) ?
O2 Co1 N4 . . 93.99(3) ?
N3 Co1 N4 . . 91.51(3) ?
N1 Co1 N5 . . 91.57(3) ?
O2 Co1 N5 . . 88.48(3) ?
N3 Co1 N5 . . 86.05(3) ?
N4 Co1 N5 . . 177.28(3) ?
N1 Co1 N2 . . 171.06(3) ?
O2 Co1 N2 . . 88.64(3) ?
N3 Co1 N2 . . 93.56(3) ?
N4 Co1 N2 . . 85.52(3) ?
N5 Co1 N2 . . 93.42(3) ?
C1 N1 Co1 . . 115.47(5) ?
C1 N1 H1 . . 119.3(10) ?
Co1 N1 H1 . . 124.9(10) ?
C21 N2 Co1 . . 108.83(4) ?
C21 N2 H2A . . 109.9 ?
Co1 N2 H2A . . 109.9 ?
C21 N2 H2B . . 109.9 ?
Co1 N2 H2B . . 109.9 ?
H2A N2 H2B . . 108.3 ?
C31 N3 Co1 . . 108.52(5) ?
C31 N3 H3A . . 110.0 ?
Co1 N3 H3A . . 110.0 ?
C31 N3 H3B . . 110.0 ?
Co1 N3 H3B . . 110.0 ?
H3A N3 H3B . . 108.4 ?
C41 N4 Co1 . . 110.21(5) ?
C41 N4 H4A . . 109.6 ?
Co1 N4 H4A . . 109.6 ?
C41 N4 H4B . . 109.6 ?
Co1 N4 H4B . . 109.6 ?
H4A N4 H4B . . 108.1 ?
C51 N5 Co1 . . 109.50(5) ?
C51 N5 H5A . . 109.8 ?
Co1 N5 H5A . . 109.8 ?
C51 N5 H5B . . 109.8 ?
Co1 N5 H5B . . 109.8 ?
H5A N5 H5B . . 108.2 ?
C2 O2 Co1 . . 113.60(5) ?
O3 C2 O2 . . 124.42(7) ?
O3 C2 C1 . . 120.43(6) ?
O2 C2 C1 . . 115.12(6) ?
O1 C1 N1 . . 128.90(7) ?
O1 C1 C2 . . 120.24(6) ?
N1 C1 C2 . . 110.86(6) ?
N2 C21 C41 . . 106.78(6) ?
N2 C21 H21A . . 110.4 ?
C41 C21 H21A . . 110.4 ?
N2 C21 H21B . . 110.4 ?
C41 C21 H21B . . 110.4 ?
H21A C21 H21B . . 108.6 ?
N3 C31 C51 . . 107.17(6) ?
N3 C31 H31A . . 110.3 ?
C51 C31 H31A . . 110.3 ?
N3 C31 H31B . . 110.3 ?
C51 C31 H31B . . 110.3 ?
H31A C31 H31B . . 108.5 ?
N4 C41 C21 . . 106.85(6) ?
N4 C41 H41A . . 110.4 ?
C21 C41 H41A . . 110.4 ?
N4 C41 H41B . . 110.4 ?
C21 C41 H41B . . 110.4 ?
H41A C41 H41B . . 108.6 ?
N5 C51 C31 . . 106.78(6) ?
N5 C51 H51A . . 110.4 ?
C31 C51 H51A . . 110.4 ?
N5 C51 H51B . . 110.4 ?
C31 C51 H51B . . 110.4 ?
H51A C51 H51B . . 108.6 ?
O13 S1 O11 . . 116.75(5) ?
O13 S1 O12 . . 114.35(6) ?
O11 S1 O12 . . 113.76(5) ?
O13 S1 C11 . . 102.30(5) ?
O11 S1 C11 . . 103.36(4) ?
O12 S1 C11 . . 103.93(4) ?
F11 C11 F13 . . 107.78(8) ?
F11 C11 F12 . . 107.61(7) ?
F13 C11 F12 . . 107.87(8) ?
F11 C11 S1 . . 111.15(6) ?
F13 C11 S1 . . 112.49(6) ?
F12 C11 S1 . . 109.77(6) ?
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 N1 . 1.9039(7) y
Co1 O2 . 1.9185(6) y
Co1 N2 . 1.9699(6) y
Co1 N3 . 1.9444(7) y
Co1 N4 . 1.9558(7) y
Co1 N5 . 1.9689(7) y
C1 O1 . 1.2578(9) y
C1 N1 . 1.3139(9) y
C2 O2 . 1.2896(9) y
C2 O3 . 1.2340(9) y
N1 H1 . 0.856(15) ?
N2 C21 . 1.4915(10) ?
N2 H2A . 0.9200 ?
N2 H2B . 0.9200 ?
N3 C31 . 1.4874(11) ?
N3 H3A . 0.9200 ?
N3 H3B . 0.9200 ?
N4 C41 . 1.4843(11) ?
N4 H4A . 0.9200 ?
N4 H4B . 0.9200 ?
N5 C51 . 1.4868(11) ?
N5 H5A . 0.9200 ?
N5 H5B . 0.9200 ?
C2 C1 . 1.5347(10) ?
C21 C41 . 1.5114(11) ?
C21 H21A . 0.9900 ?
C21 H21B . 0.9900 ?
C31 C51 . 1.5084(12) ?
C31 H31A . 0.9900 ?
C31 H31B . 0.9900 ?
C41 H41A . 0.9900 ?
C41 H41B . 0.9900 ?
C51 H51A . 0.9900 ?
C51 H51B . 0.9900 ?
S1 O13 . 1.4395(8) ?
S1 O11 . 1.4416(8) ?
S1 O12 . 1.4516(8) ?
S1 C11 . 1.8320(9) ?
C11 F11 . 1.3293(11) ?
C11 F13 . 1.3299(11) ?
C11 F12 . 1.3402(11) ?
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 H1 O11 . 0.856(15) 2.421(15) 3.1733(10) 147.1(12)
N2 H2A O1 1_455 0.92 2.19 3.0029(9) 147.5
N2 H2B O3 2_556 0.92 2.03 2.9202(9) 161.3
N3 H3A O11 . 0.92 2.48 3.2955(12) 147.7
N3 H3A O12 . 0.92 2.53 3.2660(11) 137.6
N3 H3B O1 2_656 0.92 2.52 3.1887(10) 129.6
N3 H3B O2 2_556 0.92 2.53 3.2160(9) 132.1
N4 H4A O3 2_656 0.92 2.07 2.9236(9) 154.7
N4 H4B O12 2_646 0.92 2.22 3.1282(11) 167.6
N5 H5A O1 1_455 0.92 2.00 2.8809(9) 160.3
N5 H5B F12 2_647 0.92 2.51 3.4117(11) 166.2
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_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion
_geom_torsion_publ_flag
N1 C1 C2 O2 . . . . 10.18(9) y
