#------------------------------------------------------------------------------
#$Date: 2020-10-06 11:45:50 +0200 (mar 06 de oct de 2020) $
#$Revision: 257671 $
#$URL: svn://www.crystallography.net/cod/cif/7/05/97/7059704.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_7059704
loop_
_publ_author_name
'Jana, Narayan Ch.'
'Brandão, Paula'
'Panja, Anangamohan'
_publ_section_title
;
 The first report of a tetra-azide bound mononuclear cobalt(iii) complex
 and its comparative biomimetic catalytic activity with tri-azide bound
 cobalt(iii) compounds
;
_journal_issue                   27
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              11527
_journal_page_last               11536
_journal_paper_doi               10.1039/D0NJ02339F
_journal_volume                  44
_journal_year                    2020
_chemical_formula_sum            'C8 H22 Co N15'
_chemical_formula_weight         387.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-05-06 deposited with the CCDC.	2020-06-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.059(7)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.159(4)
_cell_length_b                   7.816(3)
_cell_length_c                   24.420(11)
_cell_measurement_reflns_used    312
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.12
_cell_measurement_theta_min      2.10
_cell_volume                     1726.3(13)
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.952
_diffrn_measured_fraction_theta_max 0.952
_diffrn_measurement_device_type  CCD
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1086
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.952
_diffrn_reflns_Laue_measured_fraction_max 0.952
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            11785
_diffrn_reflns_point_group_measured_fraction_full 0.952
_diffrn_reflns_point_group_measured_fraction_max 0.952
_diffrn_reflns_theta_full        23.454
_diffrn_reflns_theta_max         23.454
_diffrn_reflns_theta_min         1.689
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.022
_exptl_absorpt_correction_T_max  0.684
_exptl_absorpt_correction_T_min  0.684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.993
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.177
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.143
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     219
_refine_ls_number_reflns         2421
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.1198
_refine_ls_R_factor_gt           0.0879
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1554P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2218
_refine_ls_wR_factor_ref         0.2626
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1647
_reflns_number_total             2421
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0nj02339f2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
;Adding full bibliography for 7059704--7059706.cif.

 Adding full bibliography for 7059704--7059706.cif.
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7059704
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.82832(10) 0.14716(11) 0.66746(4) 0.0301(5) Uani 1 1 d . . . . .
N1 N 0.8782(7) 0.1514(7) 0.7479(3) 0.0344(15) Uani 1 1 d . . . . .
H1A H 0.837044 0.244808 0.759689 0.041 Uiso 1 1 calc R U . . .
H1B H 0.833753 0.062035 0.760799 0.041 Uiso 1 1 calc R U . . .
N10 N 0.6860(7) 0.3272(8) 0.6769(3) 0.0402(16) Uani 1 1 d . . . . .
N2 N 0.9780(6) -0.0430(8) 0.6638(2) 0.0338(14) Uani 1 1 d . . . . .
H2 H 0.933805 -0.144082 0.678409 0.041 Uiso 1 1 calc R U . . .
N7 N 0.7563(8) 0.1456(7) 0.5877(3) 0.0392(16) Uani 1 1 d . . . . .
N4 N 0.6834(7) -0.0333(7) 0.6769(2) 0.0361(15) Uani 1 1 d . . . . .
N13 N 0.9783(8) 0.3148(8) 0.6574(3) 0.0460(17) Uani 1 1 d . . . . .
N8 N 0.7859(7) 0.2509(9) 0.5550(3) 0.0423(16) Uani 1 1 d . . . . .
N11 N 0.6437(7) 0.4220(9) 0.6398(3) 0.0414(16) Uani 1 1 d . . . . .
C3 C 1.1215(9) -0.0219(11) 0.6999(3) 0.046(2) Uani 1 1 d . . . . .
H3A H 1.183813 -0.118623 0.694312 0.055 Uiso 1 1 calc R U . . .
H3B H 1.168893 0.080201 0.688476 0.055 Uiso 1 1 calc R U . . .
N3 N 0.7393(7) -0.3105(8) 0.4880(2) 0.0408(16) Uani 1 1 d . . . . .
H3 H 0.749967 -0.421494 0.506895 0.049 Uiso 1 1 calc R U . . .
C1 C 1.0336(8) 0.1489(9) 0.7750(3) 0.0390(18) Uani 1 1 d . . . . .
H1C H 1.037381 0.150287 0.814902 0.047 Uiso 1 1 calc R U . . .
H1D H 1.083012 0.250856 0.764623 0.047 Uiso 1 1 calc R U . . .
N5 N 0.5631(7) -0.0196(9) 0.6507(3) 0.0471(18) Uani 1 1 d . . . . .
C6 C 0.8567(9) -0.1991(11) 0.5161(3) 0.045(2) Uani 1 1 d . . . . .
H6A H 0.836805 -0.082093 0.503850 0.054 Uiso 1 1 calc R U . . .
H6B H 0.950320 -0.232912 0.505527 0.054 Uiso 1 1 calc R U . . .
N14 N 0.9832(7) 0.4495(9) 0.6807(3) 0.0456(16) Uani 1 1 d . . . . .
C5 C 0.8693(9) -0.2066(10) 0.5791(3) 0.0416(18) Uani 1 1 d . . . . .
H5A H 0.887064 -0.323608 0.591715 0.050 Uiso 1 1 calc R U . . .
H5B H 0.777566 -0.168222 0.590222 0.050 Uiso 1 1 calc R U . . .
N12 N 0.5991(9) 0.5207(10) 0.6058(3) 0.064(2) Uani 1 1 d . . . . .
N15 N 0.9921(10) 0.5813(11) 0.7033(4) 0.076(2) Uani 1 1 d . . . . .
C4 C 0.9970(9) -0.0920(11) 0.6056(3) 0.0448(19) Uani 1 1 d . . . . .
H4A H 1.089980 -0.152240 0.606445 0.054 Uiso 1 1 calc R U . . .
H4B H 1.000079 0.010476 0.583409 0.054 Uiso 1 1 calc R U . . .
C8 C 0.7526(12) -0.3409(12) 0.4299(4) 0.063(3) Uani 1 1 d . . . . .
H8A H 0.733427 -0.236478 0.409320 0.095 Uiso 1 1 calc R U . . .
H8B H 0.682319 -0.426299 0.414758 0.095 Uiso 1 1 calc R U . . .
H8C H 0.850780 -0.379868 0.427461 0.095 Uiso 1 1 calc R U . . .
N9 N 0.8195(9) 0.3475(9) 0.5212(3) 0.059(2) Uani 1 1 d . . . . .
C2 C 1.1141(9) -0.0082(10) 0.7587(4) 0.052(2) Uani 1 1 d . . . . .
H2A H 1.214110 -0.007166 0.779011 0.062 Uiso 1 1 calc R U . . .
H2B H 1.065260 -0.109273 0.770089 0.062 Uiso 1 1 calc R U . . .
C7 C 0.5874(10) -0.2423(13) 0.4935(4) 0.065(3) Uani 1 1 d . . . . .
H7A H 0.571282 -0.135635 0.473975 0.098 Uiso 1 1 calc R U . . .
H7B H 0.581044 -0.224864 0.531930 0.098 Uiso 1 1 calc R U . . .
H7C H 0.513496 -0.323326 0.477921 0.098 Uiso 1 1 calc R U . . .
N6 N 0.4486(10) -0.0166(13) 0.6265(4) 0.097(3) Uani 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'
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
_geom_angle_publ_flag
N13 Co1 N1 93.3(3) . . ?
N13 Co1 N10 91.5(3) . . ?
N1 Co1 N10 85.6(3) . . ?
N13 Co1 N7 90.7(3) . . ?
N1 Co1 N7 173.9(3) . . ?
N10 Co1 N7 89.7(3) . . ?
N13 Co1 N4 176.9(3) . . ?
N1 Co1 N4 87.1(2) . . ?
N10 Co1 N4 91.6(3) . . ?
N7 Co1 N4 89.1(3) . . ?
N13 Co1 N2 89.6(3) . . ?
N1 Co1 N2 90.2(2) . . ?
N10 Co1 N2 175.8(3) . . ?
N7 Co1 N2 94.3(2) . . ?
N4 Co1 N2 87.3(2) . . ?
C1 N1 Co1 120.6(4) . . ?
N11 N10 Co1 120.2(5) . . ?
C3 N2 C4 111.6(5) . . ?
C3 N2 Co1 115.9(5) . . ?
C4 N2 Co1 113.9(5) . . ?
N8 N7 Co1 125.4(5) . . ?
N5 N4 Co1 117.1(5) . . ?
N14 N13 Co1 120.6(5) . . ?
N9 N8 N7 176.1(7) . . ?
N12 N11 N10 176.1(8) . . ?
C2 C3 N2 115.1(6) . . ?
C8 N3 C6 112.5(6) . . ?
C8 N3 C7 111.1(7) . . ?
C6 N3 C7 111.5(7) . . ?
N1 C1 C2 111.7(6) . . ?
N6 N5 N4 176.0(9) . . ?
N3 C6 C5 112.4(6) . . ?
N15 N14 N13 178.1(9) . . ?
C6 C5 C4 109.5(6) . . ?
N2 C4 C5 110.6(6) . . ?
C3 C2 C1 114.8(7) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Co1 N13 1.942(7) . ?
Co1 N1 1.947(6) . ?
Co1 N10 1.956(6) . ?
Co1 N7 1.956(7) . ?
Co1 N4 1.975(6) . ?
Co1 N2 2.033(6) . ?
N1 C1 1.471(10) . ?
N10 N11 1.186(9) . ?
N2 C3 1.472(10) . ?
N2 C4 1.509(9) . ?
N7 N8 1.207(9) . ?
N4 N5 1.189(9) . ?
N13 N14 1.195(9) . ?
N8 N9 1.193(9) . ?
N11 N12 1.160(10) . ?
C3 C2 1.452(12) . ?
N3 C8 1.463(10) . ?
N3 C6 1.467(10) . ?
N3 C7 1.515(10) . ?
C1 C2 1.517(11) . ?
N5 N6 1.121(11) . ?
C6 C5 1.527(11) . ?
N14 N15 1.165(10) . ?
C5 C4 1.533(11) . ?
