#------------------------------------------------------------------------------
#$Date: 2019-11-23 10:20:55 +0200 (Sat, 23 Nov 2019) $
#$Revision: 232849 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/34/82/4348257.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_4348257
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 H19 Co N16 O4'
_chemical_formula_weight         390.26
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 100.07(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.510(3)
_cell_length_b                   7.4092(15)
_cell_length_c                   17.702(4)
_cell_measurement_reflns_used    11289
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      29.53
_cell_measurement_theta_min      2.34
_cell_volume                     1615.5(6)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0601
_diffrn_reflns_av_sigmaI/netI    0.0545
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10430
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.34
_exptl_absorpt_coefficient_mu    1.111
_exptl_absorpt_correction_T_max  0.4912
_exptl_absorpt_correction_T_min  0.4819
_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            red
_exptl_crystal_density_diffrn    1.605
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.731
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     243
_refine_ls_number_reflns         3973
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.119
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0577
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0530P)²+2.8642P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                3018
_reflns_number_total             3973
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4qi00094c2.cif
_cod_data_source_block           ip103
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4348257
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
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
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Co Co 0.31048(4) 0.01034(6) 0.70499(2) 0.01290(13) Uani 1 1 d . A .
N1 N 1.0232(3) 0.2860(4) 0.95346(16) 0.0166(6) Uani 1 1 d . . .
N2 N 1.0224(3) 0.2672(4) 1.02365(16) 0.0167(6) Uani 1 1 d . . .
N3 N 1.1233(3) 0.4107(4) 0.86589(16) 0.0178(6) Uani 1 1 d . . .
N4 N 1.2163(3) 0.5018(4) 0.86929(16) 0.0204(6) Uani 1 1 d . . .
N5 N 1.2601(3) 0.5260(4) 0.94185(18) 0.0217(6) Uani 1 1 d . . .
N6 N 1.1972(3) 0.4507(4) 0.98758(16) 0.0191(6) Uani 1 1 d . . .
N7 N 0.9176(3) 0.1397(4) 1.10897(17) 0.0195(6) Uani 1 1 d . . .
N8 N 0.8259(3) 0.0456(4) 1.10190(17) 0.0198(6) Uani 1 1 d . . .
N9 N 0.7855(3) 0.0212(4) 1.02831(17) 0.0199(6) Uani 1 1 d . . .
N10 N 0.8512(3) 0.0978(4) 0.98547(16) 0.0180(6) Uani 1 1 d . . .
N11 N 0.3192(3) 0.2135(5) 0.63573(19) 0.0329(9) Uani 1 1 d . . .
H11A H 0.2520 0.2373 0.6085 0.049 Uiso 1 1 calc R . .
H11B H 0.3651 0.1851 0.6029 0.049 Uiso 1 1 calc R . .
H11C H 0.3446 0.3125 0.6636 0.049 Uiso 1 1 calc R . .
N12 N 0.3405(3) -0.1565(5) 0.62497(17) 0.0238(7) Uani 1 1 d . . .
H12A H 0.2769 -0.1893 0.5948 0.036 Uiso 1 1 calc R . .
H12B H 0.3746 -0.2564 0.6473 0.036 Uiso 1 1 calc R . .
H12C H 0.3838 -0.1010 0.5957 0.036 Uiso 1 1 calc R . .
N13 N 0.2994(3) -0.1912(4) 0.77324(17) 0.0201(6) Uani 1 1 d . . .
H13A H 0.2293 -0.2291 0.7669 0.030 Uiso 1 1 calc R . .
H13B H 0.3217 -0.1557 0.8227 0.030 Uiso 1 1 calc R . .
H13C H 0.3422 -0.2833 0.7621 0.030 Uiso 1 1 calc R . .
N14 N 0.2842(3) 0.1791(5) 0.7842(2) 0.0270(7) Uani 1 1 d . . .
H14A H 0.2117 0.1998 0.7795 0.040 Uiso 1 1 calc R . .
H14B H 0.3191 0.2849 0.7789 0.040 Uiso 1 1 calc R . .
H14C H 0.3097 0.1313 0.8313 0.040 Uiso 1 1 calc R . .
N15 N 0.1534(2) -0.0061(4) 0.66589(19) 0.0241(6) Uani 1 1 d . . .
H15A H 0.1339 0.0806 0.6297 0.036 Uiso 1 1 calc R . .
H15B H 0.1164 0.0105 0.7052 0.036 Uiso 1 1 calc R . .
H15C H 0.1375 -0.1169 0.6447 0.036 Uiso 1 1 calc R . .
C1 C 1.1146(3) 0.3824(4) 0.93894(19) 0.0155(6) Uani 1 1 d . . .
C2 C 0.9310(3) 0.1697(4) 1.03683(19) 0.0161(7) Uani 1 1 d . . .
O3 O 1.0012(2) 0.1871(4) 0.75334(15) 0.0224(6) Uani 1 1 d D . .
HW1 H 1.035(5) 0.267(7) 0.781(3) 0.07(2) Uiso 1 1 d D . .
HW2 H 0.981(4) 0.243(7) 0.7126(19) 0.040(15) Uiso 1 1 d D . .
O4 O 0.8321(2) 0.0242(4) 0.82279(15) 0.0251(6) Uani 1 1 d D . .
HW3 H 0.856(5) 0.032(8) 0.8700(13) 0.053(18) Uiso 1 1 d D . .
HW4 H 0.886(3) 0.047(8) 0.802(3) 0.043(16) Uiso 1 1 d D . .
N16 N 0.4657(3) 0.0233(5) 0.74372(18) 0.0277(7) Uani 1 1 d D . .
O1 O 0.5037(4) 0.0220(7) 0.8094(3) 0.0412(13) Uani 0.698(7) 1 d PDU A 1
O2 O 0.5261(5) 0.0271(12) 0.6924(4) 0.078(2) Uani 0.698(7) 1 d PDU A 1
O1' O 0.5198(7) -0.1055(13) 0.7513(5) 0.026(2) Uani 0.302(7) 1 d PDU . 2
O2' O 0.4955(7) 0.1726(12) 0.7730(6) 0.027(3) Uani 0.302(7) 1 d PDU . 2
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_3
N13 Co N16 89.65(15) .
N13 Co N14 90.36(14) .
N16 Co N14 89.91(15) .
N13 Co N11 179.14(16) .
N16 Co N11 91.21(16) .
N14 Co N11 89.57(16) .
N13 Co N12 90.47(14) .
N16 Co N12 88.87(15) .
N14 Co N12 178.52(16) .
N11 Co N12 89.63(16) .
N13 Co N15 89.78(15) .
N16 Co N15 179.28(14) .
N14 Co N15 90.53(15) .
N11 Co N15 89.36(16) .
N12 Co N15 90.70(14) .
N2 N1 C1 112.6(3) .
N1 N2 C2 111.7(3) .
C1 N3 N4 104.7(3) .
N5 N4 N3 108.8(3) .
N4 N5 N6 110.1(3) .
C1 N6 N5 103.8(3) .
N8 N7 C2 104.3(3) .
N9 N8 N7 109.8(3) .
N8 N9 N10 109.4(3) .
C2 N10 N9 104.1(3) .
N6 C1 N3 112.5(3) .
N6 C1 N1 129.9(3) .
N3 C1 N1 117.6(3) .
N7 C2 N10 112.4(3) .
N7 C2 N2 119.0(3) .
N10 C2 N2 128.6(3) .
O1' N16 O1 75.7(5) .
O1' N16 O2' 123.5(7) .
O1 N16 O2' 63.8(5) .
O1' N16 O2 72.3(6) .
O1 N16 O2 121.0(5) .
O2' N16 O2 96.0(6) .
O1' N16 Co 121.7(5) .
O1 N16 Co 123.6(4) .
O2' N16 Co 113.4(5) .
O2 N16 Co 115.3(4) .
N16 O1' O2' 136.5(7) 2_646
N16 O2' O1' 137.6(8) 2_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Co N13 1.941(3) .
Co N16 1.946(4) .
Co N14 1.949(3) .
Co N11 1.956(3) .
Co N12 1.965(3) .
Co N15 1.969(3) .
N1 N2 1.252(4) .
N1 C1 1.410(5) .
N2 C2 1.407(5) .
N3 C1 1.333(4) .
N3 N4 1.338(4) .
N4 N5 1.317(4) .
N5 N6 1.344(4) .
N6 C1 1.325(5) .
N7 N8 1.330(4) .
N7 C2 1.335(4) .
N8 N9 1.325(4) .
N9 N10 1.338(4) .
N10 C2 1.338(5) .
N16 O1' 1.164(9) .
N16 O1 1.176(5) .
N16 O2' 1.251(8) .
N16 O2 1.279(6) .
O1' O2' 1.702(13) 2_646
O2' O1' 1.702(13) 2_656
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
N11 H11A N6 0.91 2.55 3.047(4) 115.3 4_465
N11 H11C O1 0.91 2.43 3.213(6) 143.9 2_656
N12 H12A N10 0.91 2.51 3.353(5) 155.1 2_646
N12 H12A N6 0.91 2.66 3.151(4) 114.9 4_465
N12 H12B O1 0.91 2.28 3.167(6) 165.4 2_646
N13 H13A O4 0.91 2.45 3.011(4) 119.7 2_646
N13 H13B N8 0.91 2.59 3.118(4) 117.5 3_657
N13 H13C O2 0.91 2.21 3.004(7) 145.9 2_646
N14 H14A N3 0.91 2.57 3.179(5) 125.1 1_455
N14 H14A O3 0.91 2.59 3.487(5) 167.2 1_455
N14 H14C N8 0.91 2.59 3.115(5) 117.6 3_657
N15 H15A N2 0.91 2.41 3.273(4) 157.7 4_465
N15 H15B O3 0.91 2.22 3.017(4) 145.5 1_455
N15 H15C N1 0.91 2.52 3.176(4) 129.2 2_646
O3 HW1 N3 0.83(2) 2.01(3) 2.825(4) 166(7) .
O3 HW2 N7 0.83(2) 2.06(2) 2.887(4) 174(6) 4_565
O4 HW3 N10 0.84(2) 2.11(3) 2.899(4) 157(6) .
O4 HW4 O3 0.85(2) 2.07(3) 2.891(4) 162(6) .
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
C1 N1 N2 C2 -179.6(3) .
C1 N3 N4 N5 -0.2(4) .
N3 N4 N5 N6 0.4(4) .
N4 N5 N6 C1 -0.4(4) .
C2 N7 N8 N9 -0.4(4) .
N7 N8 N9 N10 0.7(4) .
N8 N9 N10 C2 -0.6(4) .
N5 N6 C1 N3 0.3(4) .
N5 N6 C1 N1 179.5(3) .
N4 N3 C1 N6 -0.1(4) .
N4 N3 C1 N1 -179.4(3) .
N2 N1 C1 N6 1.1(5) .
N2 N1 C1 N3 -179.8(3) .
N8 N7 C2 N10 0.0(4) .
N8 N7 C2 N2 -179.8(3) .
N9 N10 C2 N7 0.4(4) .
N9 N10 C2 N2 -179.9(3) .
N1 N2 C2 N7 -179.3(3) .
N1 N2 C2 N10 1.0(5) .
N13 Co N16 O1' 45.6(6) .
N14 Co N16 O1' 135.9(6) .
N11 Co N16 O1' -134.5(6) .
N12 Co N16 O1' -44.9(6) .
N15 Co N16 O1' 9(11) .
N13 Co N16 O1 -48.0(4) .
N14 Co N16 O1 42.4(4) .
N11 Co N16 O1 131.9(4) .
N12 Co N16 O1 -138.5(4) .
N15 Co N16 O1 -85(11) .
N13 Co N16 O2' -121.1(6) .
N14 Co N16 O2' -30.7(6) .
N11 Co N16 O2' 58.9(6) .
N12 Co N16 O2' 148.5(6) .
N15 Co N16 O2' -158(11) .
N13 Co N16 O2 129.7(5) .
N14 Co N16 O2 -140.0(5) .
N11 Co N16 O2 -50.4(5) .
N12 Co N16 O2 39.2(5) .
N15 Co N16 O2 93(11) .
O1 N16 O1' O2' 130.1(12) 2_646
O2' N16 O1' O2' 174.3(7) 2_646
O2 N16 O1' O2' -100.3(12) 2_646
Co N16 O1' O2' 9.1(14) 2_646
O1' N16 O2' O1' 143.3(8) 2_656
O1 N16 O2' O1' -167.7(13) 2_656
O2 N16 O2' O1' 70.6(12) 2_656
Co N16 O2' O1' -50.4(13) 2_656
