#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:20:55 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232849 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/82/4348256.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_4348256
loop_
_publ_author_name
'Deblitz, Raik'
'Hrib, Cristian G.'
'Blaurock, Steffen'
'Jones, Peter G.'
'Plenikowski, Georg'
'Edelmann, Frank T.'
_publ_section_title
;
 Explosive Werner-type cobalt(iii) complexes
;
_journal_issue                   8
_journal_name_full               'Inorg. Chem. Front.'
_journal_page_first              621
_journal_paper_doi               10.1039/C4QI00094C
_journal_volume                  1
_journal_year                    2014
_chemical_formula_sum            'C2 H24 Co2 N22 O8'
_chemical_formula_weight         602.29
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_cell_setting           triclinic
_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-97
_cell_angle_alpha                96.49(3)
_cell_angle_beta                 105.79(3)
_cell_angle_gamma                95.10(3)
_cell_formula_units_Z            1
_cell_length_a                   7.1228(14)
_cell_length_b                   7.3402(15)
_cell_length_c                   10.138(2)
_cell_measurement_reflns_used    13740
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.11
_cell_volume                     502.8(2)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      133(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_monochromator  'plane graphite'
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0566
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5276
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.11
_exptl_absorpt_coefficient_mu    1.740
_exptl_absorpt_correction_T_max  0.2628
_exptl_absorpt_correction_T_min  0.2428
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using  Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.989
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             308
_exptl_crystal_size_max          0.60
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.106
_refine_diff_density_min         -0.805
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     202
_refine_ls_number_reflns         2457
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0325
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0552P)²+0.1665P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0860
_refine_ls_wR_factor_ref         0.0875
_reflns_number_gt                2323
_reflns_number_total             2457
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00094c2.cif
_cod_data_source_block           ip99
_cod_original_cell_volume        502.79(17)
_cod_database_code               4348256
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
C1 C 0.4562(2) 0.3438(2) 0.84800(18) 0.0121(3) Uani 1 1 d
Co Co 0.02924(3) 0.25279(3) 0.25520(2) 0.00811(11) Uani 1 1 d
O1 O -0.0433(2) 0.2865(2) 0.51116(13) 0.0168(3) Uani 1 1 d
O2 O -0.27739(19) 0.3627(2) 0.35163(14) 0.0166(3) Uani 1 1 d
O3 O 0.3340(2) 0.1555(2) 0.15056(14) 0.0183(3) Uani 1 1 d
O4 O 0.0810(2) 0.20591(19) -0.00626(13) 0.0163(3) Uani 1 1 d
N1 N 0.4228(2) 0.4647(2) 0.95465(15) 0.0132(3) Uani 1 1 d
N2 N 0.3059(2) 0.2393(2) 0.75434(15) 0.0147(3) Uani 1 1 d
N3 N 0.3870(2) 0.1522(2) 0.66448(17) 0.0176(3) Uani 1 1 d
N4 N 0.5794(2) 0.2046(2) 0.70443(18) 0.0195(3) Uani 1 1 d
N5 N 0.6278(2) 0.3259(2) 0.82132(17) 0.0179(3) Uani 1 1 d
N6 N -0.1153(2) 0.3061(2) 0.38851(15) 0.0115(3) Uani 1 1 d
N7 N 0.1648(2) 0.1990(2) 0.11691(15) 0.0117(3) Uani 1 1 d
N8 N -0.2175(2) 0.1413(2) 0.12054(16) 0.0125(3) Uani 1 1 d
H8A H -0.225(5) 0.176(4) 0.048(3) 0.029(7) Uiso 1 1 d
H8B H -0.233(4) 0.022(5) 0.101(3) 0.026(7) Uiso 1 1 d
H8C H -0.321(5) 0.166(5) 0.146(3) 0.032(8) Uiso 1 1 d
N9 N -0.0095(2) 0.4923(2) 0.19447(16) 0.0119(3) Uani 1 1 d
H9A H -0.110(4) 0.486(4) 0.118(3) 0.022(6) Uiso 1 1 d
H9B H 0.092(4) 0.539(4) 0.170(3) 0.018(6) Uiso 1 1 d
H9C H -0.032(5) 0.569(4) 0.260(3) 0.028(7) Uiso 1 1 d
N10 N 0.2761(2) 0.3655(2) 0.39016(16) 0.0135(3) Uani 1 1 d
H10A H 0.373(5) 0.340(4) 0.366(3) 0.028(7) Uiso 1 1 d
H10B H 0.278(5) 0.329(5) 0.460(4) 0.044(10) Uiso 1 1 d
H10C H 0.278(5) 0.477(6) 0.411(4) 0.041(9) Uiso 1 1 d
N11 N 0.0810(2) 0.0183(2) 0.32312(17) 0.0137(3) Uani 1 1 d
H11A H 0.113(4) 0.040(4) 0.412(3) 0.022(7) Uiso 1 1 d
H11B H 0.175(5) -0.027(5) 0.295(3) 0.038(8) Uiso 1 1 d
H11C H -0.025(5) -0.069(5) 0.293(3) 0.036(8) Uiso 1 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'
Co Co 0.3494 0.9721 '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'
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
N2 C1 N5 112.51(16) .
N2 C1 N1 120.23(15) .
N5 C1 N1 127.13(16) .
N7 Co N6 177.95(6) .
N7 Co N9 89.24(7) .
N6 Co N9 90.04(7) .
N7 Co N8 89.29(7) .
N6 Co N8 88.80(7) .
N9 Co N8 90.63(7) .
N7 Co N11 90.78(7) .
N6 Co N11 90.03(7) .
N9 Co N11 177.01(6) .
N8 Co N11 92.35(8) .
N7 Co N10 90.81(7) .
N6 Co N10 91.10(7) .
N9 Co N10 89.16(8) .
N8 Co N10 179.77(6) .
N11 Co N10 87.86(8) .
N1 N1 C1 113.37(18) 2_667
C1 N2 N3 104.69(15) .
N4 N3 N2 109.05(16) .
N3 N4 N5 109.80(16) .
C1 N5 N4 103.95(15) .
O2 N6 O1 120.21(15) .
O2 N6 Co 119.98(12) .
O1 N6 Co 119.80(12) .
O4 N7 O3 119.88(15) .
O4 N7 Co 119.64(12) .
O3 N7 Co 120.47(12) .
Co N8 H8A 110(2) .
Co N8 H8B 116(2) .
H8A N8 H8B 104(3) .
Co N8 H8C 113(2) .
H8A N8 H8C 108(3) .
H8B N8 H8C 104(3) .
Co N9 H9A 112.7(18) .
Co N9 H9B 111.6(17) .
H9A N9 H9B 104(2) .
Co N9 H9C 110.3(19) .
H9A N9 H9C 108(3) .
H9B N9 H9C 110(3) .
Co N10 H10A 112(2) .
Co N10 H10B 107(3) .
H10A N10 H10B 111(3) .
Co N10 H10C 112(3) .
H10A N10 H10C 112(3) .
H10B N10 H10C 102(3) .
Co N11 H11A 106.8(19) .
Co N11 H11B 111(2) .
H11A N11 H11B 111(3) .
Co N11 H11C 113(2) .
H11A N11 H11C 109(3) .
H11B N11 H11C 107(3) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N2 1.331(2) .
C1 N5 1.336(2) .
C1 N1 1.405(2) .
Co N7 1.9319(15) .
Co N6 1.9359(15) .
Co N9 1.9452(16) .
Co N8 1.9514(17) .
Co N11 1.9531(16) .
Co N10 1.9555(18) .
O1 N6 1.239(2) .
O2 N6 1.238(2) .
O3 N7 1.241(2) .
O4 N7 1.238(2) .
N1 N1 1.251(3) 2_667
N2 N3 1.339(2) .
N3 N4 1.326(2) .
N4 N5 1.342(2) .
N8 H8A 0.80(3) .
N8 H8B 0.86(3) .
N8 H8C 0.87(3) .
N9 H9A 0.89(3) .
N9 H9B 0.88(3) .
N9 H9C 0.88(3) .
N10 H10A 0.82(3) .
N10 H10B 0.79(4) .
N10 H10C 0.82(4) .
N11 H11A 0.86(3) .
N11 H11B 0.87(3) .
N11 H11C 0.90(4) .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
N8 H8A O4 0.80(3) 2.39(3) 2.801(2) 113(3) .
N8 H8A N5 0.80(3) 2.65(3) 3.410(3) 159(3) 1_454
N8 H8B O4 0.86(3) 2.33(3) 3.028(2) 138(3) 2
N8 H8B O3 0.86(3) 2.61(3) 3.174(2) 124(2) 2
N8 H8B N2 0.86(3) 2.64(3) 3.276(2) 131(2) 2_556
N8 H8C O2 0.87(3) 2.32(3) 2.849(2) 119(3) .
N8 H8C O3 0.87(3) 2.46(3) 3.300(2) 161(3) 1_455
N9 H9A N1 0.89(3) 2.22(3) 2.984(2) 143(2) 2_566
N9 H9B N5 0.88(3) 2.12(3) 2.973(2) 162(2) 2_666
N9 H9C O1 0.88(3) 2.34(3) 3.142(2) 152(3) 2_566
N9 H9C N2 0.88(3) 2.49(3) 3.117(2) 129(2) 2_566
N10 H10A O3 0.82(3) 2.37(3) 2.874(2) 120(3) .
N10 H10A O2 0.82(3) 2.53(3) 3.310(2) 160(3) 1_655
N10 H10B O1 0.79(4) 2.48(4) 2.909(2) 116(3) .
N10 H10B N3 0.79(4) 2.55(4) 3.289(2) 158(3) .
N10 H10C O2 0.82(4) 2.56(4) 3.104(2) 125(3) 2_566
N11 H11A O1 0.86(3) 2.47(3) 2.945(2) 116(2) .
N11 H11B N4 0.87(3) 2.28(3) 3.095(2) 157(3) 2_656
N11 H11B O3 0.87(3) 2.51(3) 3.019(2) 118(3) .
N11 H11C N2 0.90(4) 2.17(4) 3.057(2) 168(3) 2_556
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
_geom_torsion_site_symmetry_4
N2 C1 N1 N1 170.91(19) 2_667
N5 C1 N1 N1 -13.6(3) 2_667
N5 C1 N2 N3 -0.2(2) .
N1 C1 N2 N3 175.97(15) .
C1 N2 N3 N4 -0.1(2) .
N2 N3 N4 N5 0.3(2) .
N2 C1 N5 N4 0.4(2) .
N1 C1 N5 N4 -175.45(17) .
N3 N4 N5 C1 -0.4(2) .
N7 Co N6 O2 -19.9(16) .
N9 Co N6 O2 49.57(14) .
N8 Co N6 O2 -41.07(14) .
N11 Co N6 O2 -133.42(14) .
N10 Co N6 O2 138.72(14) .
N7 Co N6 O1 161.4(15) .
N9 Co N6 O1 -129.13(14) .
N8 Co N6 O1 140.24(14) .
N11 Co N6 O1 47.89(14) .
N10 Co N6 O1 -39.97(14) .
N6 Co N7 O4 13.2(16) .
N9 Co N7 O4 -56.36(14) .
N8 Co N7 O4 34.28(14) .
N11 Co N7 O4 126.63(14) .
N10 Co N7 O4 -145.51(14) .
N6 Co N7 O3 -166.0(15) .
N9 Co N7 O3 124.51(15) .
N8 Co N7 O3 -144.85(15) .
N11 Co N7 O3 -52.51(15) .
N10 Co N7 O3 35.36(14) .
