#------------------------------------------------------------------------------
#$Date: 2018-06-12 05:06:52 +0300 (Tue, 12 Jun 2018) $
#$Revision: 208273 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/54/95/1549532.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_1549532
loop_
_publ_author_name
'Köferstein, Roberto'
'Robl, Christian'
_publ_section_title
;
 Synthesis, Crystal Structure, and Hydrogen Bonding of
 μ-Hydroxo-μ-peroxo-bis[bis(ethylenediamine)cobalt(III)] Squarate
;
_journal_issue                   7
_journal_name_full
'Zeitschrift für anorganische und allgemeine Chemie'
_journal_page_first              560
_journal_paper_doi               10.1002/zaac.201600080
_journal_volume                  642
_journal_year                    2016
_chemical_formula_sum            'C14 H41 Co2 N8 O13'
_chemical_formula_weight         647.41
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                100.282(5)
_cell_angle_beta                 94.515(7)
_cell_angle_gamma                95.596(6)
_cell_formula_units_Z            2
_cell_length_a                   8.0020(8)
_cell_length_b                   12.2548(7)
_cell_length_c                   14.0384(9)
_cell_measurement_temperature    293(2)
_cell_volume                     1341.57(18)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_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  0.0137
_diffrn_reflns_av_sigmaI/netI    0.0261
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5821
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    1.310
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_F_000             678
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.457
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.706
_refine_ls_goodness_of_fit_obs   1.776
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         4561
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.689
_refine_ls_restrained_S_obs      1.776
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_obs          0.0345
_refine_ls_shift/esd_max         -0.008
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0000P)²+0.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0679
_refine_ls_wR_factor_obs         0.0665
_reflns_number_observed          4139
_reflns_number_total             4715
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            Co2enq4_neu.cif
_cod_data_source_block           coquen2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. A new data item '_refine_ls_weighting_details' was
created with the value set to
'w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.5000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 5642 2017-10-24 12:04:52Z antanas 
;
_cod_original_cell_volume        1341.6(2)
_cod_database_code               1549532
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Co1 Co 0.41225(5) 0.97739(3) 0.79213(3) 0.02549(10) Uani 1 d . .
Co2 Co 0.41503(5) 0.70803(3) 0.74973(3) 0.02505(10) Uani 1 d . .
C1 C 0.0419(4) 0.5253(3) 0.9398(2) 0.0418(8) Uani 1 d . .
C2 C 0.0218(4) 0.4199(3) 0.9724(2) 0.0418(8) Uani 1 d . .
C3 C 0.0872(4) 0.2030(3) 0.5645(2) 0.0383(7) Uani 1 d . .
C4 C -0.0357(4) 0.1610(3) 0.4789(2) 0.0389(8) Uani 1 d . .
C5 C 0.0958(4) 0.1828(3) 0.4166(2) 0.0378(7) Uani 1 d . .
C6 C 0.2162(4) 0.2264(3) 0.5005(2) 0.0365(7) Uani 1 d . .
C7 C 0.6694(5) 1.1018(4) 0.7155(3) 0.0743(13) Uani 1 d . .
H1 H 0.6727(5) 1.1767(4) 0.7530(3) 0.063(3) Uiso 1 calc R .
H2 H 0.7742(5) 1.0964(4) 0.6855(3) 0.063(3) Uiso 1 calc R .
C8 C 0.5296(5) 1.0808(4) 0.6414(3) 0.0645(11) Uani 1 d . .
H3 H 0.5457(5) 1.0170(4) 0.5925(3) 0.063(3) Uiso 1 calc R .
H4 H 0.5253(5) 1.1449(4) 0.6100(3) 0.063(3) Uiso 1 calc R .
C9 C 0.1089(4) 1.0415(3) 0.8630(2) 0.0398(8) Uani 1 d . .
H5 H 0.0071(4) 1.0183(3) 0.8907(2) 0.063(3) Uiso 1 calc R .
H6 H 0.0829(4) 1.0938(3) 0.8211(2) 0.063(3) Uiso 1 calc R .
C10 C 0.2458(4) 1.0942(3) 0.9421(2) 0.0388(7) Uani 1 d . .
H7 H 0.2191(4) 1.1665(3) 0.9737(2) 0.063(3) Uiso 1 calc R .
H8 H 0.2566(4) 1.0473(3) 0.9905(2) 0.063(3) Uiso 1 calc R .
C11 C 0.1512(4) 0.5704(3) 0.6267(2) 0.0489(9) Uani 1 d . .
H9 H 0.0391(4) 0.5651(3) 0.5932(2) 0.063(3) Uiso 1 calc R .
H10 H 0.1649(4) 0.5003(3) 0.6477(2) 0.063(3) Uiso 1 calc R .
C12 C 0.2824(4) 0.5947(3) 0.5605(2) 0.0479(9) Uani 1 d . .
H11 H 0.2859(4) 0.5298(3) 0.5100(2) 0.063(3) Uiso 1 calc R .
H12 H 0.2557(4) 0.6566(3) 0.5297(2) 0.063(3) Uiso 1 calc R .
C13 C 0.7253(4) 0.6519(3) 0.8287(2) 0.0436(8) Uani 1 d . .
H13 H 0.8248(4) 0.6802(3) 0.8736(2) 0.063(3) Uiso 1 calc R .
H14 H 0.7567(4) 0.5978(3) 0.7758(2) 0.063(3) Uiso 1 calc R .
C14 C 0.5899(4) 0.5991(3) 0.8800(2) 0.0448(8) Uani 1 d . .
H15 H 0.6210(4) 0.5294(3) 0.8956(2) 0.063(3) Uiso 1 calc R .
H16 H 0.5739(4) 0.6485(3) 0.9399(2) 0.063(3) Uiso 1 calc R .
N1 N 0.6517(3) 1.0199(2) 0.7802(2) 0.0350(6) Uani 1 d . .
H17 H 0.7051(3) 1.0496(2) 0.8393(2) 0.050(3) Uiso 1 calc R .
H18 H 0.7000(3) 0.9589(2) 0.7560(2) 0.050(3) Uiso 1 calc R .
N2 N 0.3685(3) 1.0585(2) 0.6832(2) 0.0395(6) Uani 1 d . .
H19 H 0.2919(3) 1.0169(2) 0.6373(2) 0.050(3) Uiso 1 calc R .
H20 H 0.3277(3) 1.1232(2) 0.7053(2) 0.050(3) Uiso 1 calc R .
N3 N 0.1758(3) 0.9438(2) 0.8074(2) 0.0318(6) Uani 1 d . .
H21 H 0.1172(3) 0.9238(2) 0.7484(2) 0.050(3) Uiso 1 calc R .
H22 H 0.1625(3) 0.8860(2) 0.8387(2) 0.050(3) Uiso 1 calc R .
N4 N 0.4050(3) 1.1066(2) 0.8961(2) 0.0345(6) Uani 1 d . .
H23 H 0.4935(3) 1.1118(2) 0.9410(2) 0.050(3) Uiso 1 calc R .
H24 H 0.4116(3) 1.1696(2) 0.8713(2) 0.050(3) Uiso 1 calc R .
N5 N 0.1738(3) 0.6634(2) 0.7117(2) 0.0324(6) Uani 1 d . .
H25 H 0.1244(3) 0.6416(2) 0.7617(2) 0.050(3) Uiso 1 calc R .
H26 H 0.1246(3) 0.7218(2) 0.6964(2) 0.050(3) Uiso 1 calc R .
N6 N 0.4477(3) 0.6232(2) 0.6197(2) 0.0340(6) Uani 1 d . .
H27 H 0.5186(3) 0.6646(2) 0.5899(2) 0.050(3) Uiso 1 calc R .
H28 H 0.4935(3) 0.5603(2) 0.6261(2) 0.050(3) Uiso 1 calc R .
N7 N 0.6537(3) 0.7445(2) 0.7907(2) 0.0320(6) Uani 1 d . .
H29 H 0.7082(3) 0.7589(2) 0.7398(2) 0.050(3) Uiso 1 calc R .
H30 H 0.6696(3) 0.8064(2) 0.8372(2) 0.050(3) Uiso 1 calc R .
N8 N 0.4335(3) 0.5790(2) 0.8129(2) 0.0345(6) Uani 1 d . .
H31 H 0.3435(3) 0.5684(2) 0.8461(2) 0.050(3) Uiso 1 calc R .
H32 H 0.4360(3) 0.5172(2) 0.7677(2) 0.050(3) Uiso 1 calc R .
O1 O 0.0897(4) 0.5536(2) 0.8640(2) 0.0767(9) Uani 1 d . .
O2 O 0.0502(4) 0.3230(2) 0.9382(2) 0.0697(8) Uani 1 d . .
O3 O 0.0831(3) 0.2153(2) 0.6546(2) 0.0592(7) Uani 1 d . .
O4 O -0.1882(3) 0.1264(2) 0.4642(2) 0.0594(7) Uani 1 d . .
O5 O 0.1000(3) 0.1716(2) 0.32546(15) 0.0555(7) Uani 1 d . .
O6 O 0.3664(3) 0.2684(2) 0.5121(2) 0.0556(7) Uani 1 d . .
O7 O 0.4697(2) 0.89764(15) 0.88963(13) 0.0285(4) Uani 1 d . .
O8 O 0.3687(2) 0.78846(15) 0.86951(13) 0.0292(4) Uani 1 d . .
O9 O 0.4179(3) 0.8431(2) 0.69864(13) 0.0281(4) Uani 1 d . .
OW1 O 0.1935(4) 0.8394(2) 1.0289(2) 0.0596(8) Uani 1 d . .
OW2 O 0.3190(5) 1.3119(3) 0.8261(3) 0.0767(11) Uani 1 d . .
OW3 O 0.4587(4) 0.5934(2) 0.3354(2) 0.0710(10) Uani 1 d . .
OW4 O 0.1314(5) 0.6237(3) 0.2867(3) 0.0944(12) Uani 1 d . .
H33 H 0.3502(50) 0.8391(34) 0.6544(29) 0.077(5) Uiso 1 d . .
H34 H 0.2421(53) 0.8116(35) 0.9868(30) 0.077(5) Uiso 1 d . .
H35 H 0.1184(53) 0.7875(34) 1.0401(29) 0.077(5) Uiso 1 d . .
H36 H 0.2761(66) 1.3177(44) 0.7836(33) 0.077(5) Uiso 1 d . .
H37 H 0.4069(56) 1.3281(42) 0.8537(35) 0.077(5) Uiso 1 d . .
H38 H 0.3648(54) 0.6097(36) 0.3261(32) 0.077(5) Uiso 1 d . .
H39 H 0.5068(55) 0.6371(36) 0.3746(31) 0.077(5) Uiso 1 d . .
H40 H 0.1691(54) 0.6886(35) 0.2545(30) 0.077(5) Uiso 1 d . .
H41 H 0.0669(58) 0.5932(39) 0.2511(33) 0.077(5) Uiso 1 d . .
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'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
O7 Co1 O9 87.99(8) . .
O7 Co1 N3 90.04(9) . .
O9 Co1 N3 93.43(9) . .
O7 Co1 N4 87.39(9) . .
O9 Co1 N4 175.14(10) . .
N3 Co1 N4 85.06(10) . .
O7 Co1 N1 90.87(9) . .
O9 Co1 N1 89.61(10) . .
N3 Co1 N1 176.86(10) . .
N4 Co1 N1 91.98(11) . .
O7 Co1 N2 175.15(10) . .
O9 Co1 N2 89.28(9) . .
N3 Co1 N2 94.13(11) . .
N4 Co1 N2 95.43(10) . .
N1 Co1 N2 85.10(11) . .
O8 Co2 O9 88.72(8) . .
O8 Co2 N7 89.06(9) . .
O9 Co2 N7 89.14(9) . .
O8 Co2 N8 87.97(9) . .
O9 Co2 N8 173.37(10) . .
N7 Co2 N8 85.07(10) . .
O8 Co2 N5 90.89(9) . .
O9 Co2 N5 94.18(9) . .
N7 Co2 N5 176.68(10) . .
N8 Co2 N5 91.61(10) . .
O8 Co2 N6 176.07(10) . .
O9 Co2 N6 90.33(9) . .
N7 Co2 N6 94.74(10) . .
N8 Co2 N6 93.36(10) . .
N5 Co2 N6 85.37(10) . .
O1 C1 C2 133.5(3) . .
O1 C1 C2 136.2(3) . 2_567
C2 C1 C2 90.3(3) . 2_567
O2 C2 C1 134.3(3) . .
O2 C2 C1 135.9(3) . 2_567
C1 C2 C1 89.7(3) . 2_567
O3 C3 C6 134.8(3) . .
O3 C3 C4 135.3(3) . .
C6 C3 C4 89.9(2) . .
O4 C4 C5 134.5(3) . .
O4 C4 C3 136.3(3) . .
C5 C4 C3 89.1(2) . .
O5 C5 C6 134.8(3) . .
O5 C5 C4 133.9(3) . .
C6 C5 C4 91.2(2) . .
O6 C6 C5 134.5(3) . .
O6 C6 C3 135.7(3) . .
C5 C6 C3 89.8(2) . .
C8 C7 N1 109.8(3) . .
C8 C7 H1 109.7(3) . .
N1 C7 H1 109.7(2) . .
C8 C7 H2 109.7(2) . .
N1 C7 H2 109.7(2) . .
H1 C7 H2 108.2 . .
C7 C8 N2 111.0(3) . .
C7 C8 H3 109.4(3) . .
N2 C8 H3 109.4(2) . .
C7 C8 H4 109.4(2) . .
N2 C8 H4 109.4(2) . .
H3 C8 H4 108.0 . .
N3 C9 C10 105.9(2) . .
N3 C9 H5 110.5(2) . .
C10 C9 H5 110.5(2) . .
N3 C9 H6 110.5(2) . .
C10 C9 H6 110.5(2) . .
H5 C9 H6 108.7 . .
N4 C10 C9 107.5(2) . .
N4 C10 H7 110.22(15) . .
C9 C10 H7 110.2(2) . .
N4 C10 H8 110.2(2) . .
C9 C10 H8 110.2(2) . .
H7 C10 H8 108.5 . .
N5 C11 C12 107.3(3) . .
N5 C11 H9 110.2(2) . .
C12 C11 H9 110.2(2) . .
N5 C11 H10 110.2(2) . .
C12 C11 H10 110.2(2) . .
H9 C11 H10 108.5 . .
N6 C12 C11 108.0(3) . .
N6 C12 H11 110.1(2) . .
C11 C12 H11 110.1(2) . .
N6 C12 H12 110.1(2) . .
C11 C12 H12 110.1(2) . .
H11 C12 H12 108.4 . .
N7 C13 C14 106.6(2) . .
N7 C13 H13 110.4(2) . .
C14 C13 H13 110.4(2) . .
N7 C13 H14 110.4(2) . .
C14 C13 H14 110.4(2) . .
H13 C13 H14 108.6 . .
N8 C14 C13 106.9(2) . .
N8 C14 H15 110.3(2) . .
C13 C14 H15 110.3(2) . .
N8 C14 H16 110.3(2) . .
C13 C14 H16 110.3(2) . .
H15 C14 H16 108.6 . .
C7 N1 Co1 110.3(2) . .
C7 N1 H17 109.6(2) . .
Co1 N1 H17 109.59(7) . .
C7 N1 H18 109.6(2) . .
Co1 N1 H18 109.59(7) . .
H17 N1 H18 108.1 . .
C8 N2 Co1 108.1(2) . .
C8 N2 H19 110.1(2) . .
Co1 N2 H19 110.07(7) . .
C8 N2 H20 110.1(2) . .
Co1 N2 H20 110.07(7) . .
H19 N2 H20 108.4 . .
C9 N3 Co1 111.0(2) . .
C9 N3 H21 109.44(15) . .
Co1 N3 H21 109.44(7) . .
C9 N3 H22 109.4(2) . .
Co1 N3 H22 109.44(7) . .
H21 N3 H22 108.0 . .
C10 N4 Co1 109.7(2) . .
C10 N4 H23 109.73(15) . .
Co1 N4 H23 109.73(7) . .
C10 N4 H24 109.7(2) . .
Co1 N4 H24 109.73(7) . .
H23 N4 H24 108.2 . .
C11 N5 Co2 109.6(2) . .
C11 N5 H25 109.8(2) . .
Co2 N5 H25 109.76(7) . .
C11 N5 H26 109.8(2) . .
Co2 N5 H26 109.76(7) . .
H25 N5 H26 108.2 . .
C12 N6 Co2 109.2(2) . .
C12 N6 H27 109.8(2) . .
Co2 N6 H27 109.83(7) . .
C12 N6 H28 109.8(2) . .
Co2 N6 H28 109.83(7) . .
H27 N6 H28 108.3 . .
C13 N7 Co2 111.4(2) . .
C13 N7 H29 109.3(2) . .
Co2 N7 H29 109.34(7) . .
C13 N7 H30 109.3(2) . .
Co2 N7 H30 109.34(7) . .
H29 N7 H30 108.0 . .
C14 N8 Co2 109.1(2) . .
C14 N8 H31 109.9(2) . .
Co2 N8 H31 109.86(7) . .
C14 N8 H32 109.9(2) . .
Co2 N8 H32 109.86(7) . .
H31 N8 H32 108.3 . .
O8 O7 Co1 109.33(12) . .
O7 O8 Co2 109.47(13) . .
Co2 O9 Co1 115.82(9) . .
Co2 O9 H33 113.0(31) . .
Co1 O9 H33 111.0(30) . .
H34 OW1 H35 106.7(39) . .
H36 OW2 H37 139.3(62) . .
H38 OW3 H39 108.7(44) . .
H40 OW4 H41 101.2(49) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co1 O7 1.873(2) .
Co1 O9 1.919(2) .
Co1 N3 1.933(2) .
Co1 N4 1.962(2) .
Co1 N1 1.965(2) .
Co1 N2 1.994(2) .
Co2 O8 1.875(2) .
Co2 O9 1.917(2) .
Co2 N7 1.936(2) .
Co2 N8 1.958(2) .
Co2 N5 1.959(2) .
Co2 N6 1.983(2) .
C1 O1 1.253(4) .
C1 C2 1.444(4) .
C1 C2 1.450(4) 2_567
C2 O2 1.249(4) .
C2 C1 1.450(4) 2_567
C3 O3 1.251(4) .
C3 C6 1.461(4) .
C3 C4 1.473(4) .
C4 O4 1.241(4) .
C4 C5 1.454(4) .
C5 O5 1.266(3) .
C5 C6 1.448(4) .
C6 O6 1.246(4) .
C7 C8 1.437(5) .
C7 N1 1.473(4) .
C7 H1 0.97 .
C7 H2 0.97 .
C8 N2 1.479(4) .
C8 H3 0.97 .
C8 H4 0.97 .
C9 N3 1.478(4) .
C9 C10 1.505(4) .
C9 H5 0.97 .
C9 H6 0.97 .
C10 N4 1.479(4) .
C10 H7 0.97 .
C10 H8 0.97 .
C11 N5 1.481(4) .
C11 C12 1.499(4) .
C11 H9 0.97 .
C11 H10 0.97 .
C12 N6 1.482(4) .
C12 H11 0.97 .
C12 H12 0.97 .
C13 N7 1.481(4) .
C13 C14 1.504(5) .
C13 H13 0.97 .
C13 H14 0.97 .
C14 N8 1.478(4) .
C14 H15 0.97 .
C14 H16 0.97 .
N1 H17 0.90 .
N1 H18 0.90 .
N2 H19 0.90 .
N2 H20 0.90 .
N3 H21 0.90 .
N3 H22 0.90 .
N4 H23 0.90 .
N4 H24 0.90 .
N5 H25 0.90 .
N5 H26 0.90 .
N6 H27 0.90 .
N6 H28 0.90 .
N7 H29 0.90 .
N7 H30 0.90 .
N8 H31 0.90 .
N8 H32 0.90 .
O7 O8 1.464(2) .
O9 H33 0.78(4) .
OW1 H34 0.78(4) .
OW1 H35 0.88(4) .
OW2 H36 0.68(4) .
OW2 H37 0.77(4) .
OW3 H38 0.80(4) .
OW3 H39 0.75(4) .
OW4 H40 1.01(4) .
OW4 H41 0.71(4) .
