#------------------------------------------------------------------------------
#$Date: 2019-11-23 18:10:41 +0200 (Sat, 23 Nov 2019) $
#$Revision: 234372 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/49/7124945.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_7124945
loop_
_publ_author_name
'Das, Debasree'
'Pattanayak, Santanu'
'Singh, Kundan K.'
'Garai, Bikash'
'Sen Gupta, Sayam'
_publ_section_title
;
 Electrocatalytic water oxidation by a molecular cobalt complex through a
 high valent cobalt oxo intermediate.
;
_journal_issue                   79
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              11787
_journal_page_last               11790
_journal_paper_doi               10.1039/c6cc05773j
_journal_volume                  52
_journal_year                    2016
_chemical_formula_moiety         'C17 H19 Co N5 O4, C8 H20 N'
_chemical_formula_sum            'C25 H39 Co N6 O4'
_chemical_formula_weight         546.55
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-06-12 deposited with the CCDC.
2016-08-22 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 109.316(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.5396(11)
_cell_length_b                   9.6307(6)
_cell_length_c                   20.8295(15)
_cell_measurement_reflns_used    3969
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      26.24
_cell_measurement_theta_min      3.52
_cell_volume                     2752.5(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω 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  0.0867
_diffrn_reflns_av_sigmaI/netI    0.0895
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            15659
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         27.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    0.664
_exptl_absorpt_correction_T_max  0.830
_exptl_absorpt_correction_T_min  0.756
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.319
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.502
_refine_diff_density_min         -0.816
_refine_diff_density_rms         0.117
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5985
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.1221
_refine_ls_R_factor_gt           0.0773
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1449P)²+1.5945P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2855
_reflns_number_gt                3552
_reflns_number_total             5985
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c6cc05773j2.cif
_cod_data_source_block           co-taml
_cod_original_cell_volume        2752.5(3)
_cod_original_sg_symbol_H-M      P21/n
_cod_database_code               7124945
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Co1 Co 0.32830(4) 0.39136(7) 0.67428(3) 0.0489(3) Uani 1 1 d .
N3 N 0.2678(3) 0.4238(4) 0.7347(2) 0.0467(9) Uani 1 1 d .
O2 O 0.0458(3) 0.3702(5) 0.5947(2) 0.0789(12) Uani 1 1 d .
O4 O 0.5643(3) 0.4923(5) 0.82714(18) 0.0712(11) Uani 1 1 d .
C20 C 0.2702(4) 0.9446(6) 0.4397(3) 0.0627(14) Uani 1 1 d .
H20A H 0.2063 0.9503 0.4052 0.075 Uiso 1 1 calc R
H20B H 0.2763 1.0220 0.4706 0.075 Uiso 1 1 calc R
N1 N 0.3759(3) 0.3650(4) 0.6057(2) 0.0521(10) Uani 1 1 d .
O3 O 0.2654(3) 0.4682(4) 0.84109(18) 0.0674(10) Uani 1 1 d .
N2 N 0.2099(3) 0.3625(4) 0.6114(2) 0.0528(10) Uani 1 1 d .
O1 O 0.5172(3) 0.3400(7) 0.5820(2) 0.1033(17) Uani 1 1 d .
N6 N 0.2761(3) 0.8106(4) 0.4792(2) 0.0536(10) Uani 1 1 d .
C14 C 0.1587(4) 0.4137(5) 0.7073(3) 0.0526(11) Uani 1 1 d .
C7 C 0.4729(4) 0.3655(6) 0.6207(3) 0.0631(14) Uani 1 1 d .
N5 N 0.4108(3) 0.4655(4) 0.82735(19) 0.0528(10) Uani 1 1 d .
C18 C 0.2651(4) 0.6844(6) 0.4342(3) 0.0663(14) Uani 1 1 d .
H18A H 0.3197 0.6815 0.4172 0.080 Uiso 1 1 calc R
H18B H 0.2688 0.6020 0.4617 0.080 Uiso 1 1 calc R
C15 C 0.1196(4) 0.2983(6) 0.7403(3) 0.0652(14) Uani 1 1 d .
H15A H 0.1535 0.2135 0.7386 0.098 Uiso 1 1 calc R
H15B H 0.0513 0.2861 0.7163 0.098 Uiso 1 1 calc R
H15C H 0.1292 0.3219 0.7868 0.098 Uiso 1 1 calc R
C25 C 0.1936(4) 0.8194(6) 0.5089(3) 0.0617(13) Uani 1 1 d .
H25A H 0.2045 0.9001 0.5384 0.074 Uiso 1 1 calc R
H25B H 0.1330 0.8342 0.4720 0.074 Uiso 1 1 calc R
N4 N 0.4522(3) 0.4220(4) 0.7283(2) 0.0529(10) Uani 1 1 d .
C17 C 0.1314(4) 0.3807(5) 0.6314(3) 0.0550(12) Uani 1 1 d .
C5 C 0.2401(5) 0.3014(6) 0.4224(3) 0.0659(15) Uani 1 1 d .
H5 H 0.2491 0.2901 0.3806 0.079 Uiso 1 1 calc R
C3 C 0.1303(4) 0.3163(6) 0.4859(3) 0.0652(14) Uani 1 1 d .
H3 H 0.0673 0.3144 0.4878 0.078 Uiso 1 1 calc R
C19 C 0.1722(5) 0.6789(8) 0.3746(4) 0.0865(19) Uani 1 1 d .
H19A H 0.1184 0.6624 0.3905 0.130 Uiso 1 1 calc R
H19B H 0.1761 0.6052 0.3446 0.130 Uiso 1 1 calc R
H19C H 0.1629 0.7657 0.3506 0.130 Uiso 1 1 calc R
C4 C 0.1471(5) 0.2994(6) 0.4255(3) 0.0749(17) Uani 1 1 d .
H4 H 0.0947 0.2863 0.3858 0.090 Uiso 1 1 calc R
C2 C 0.2104(4) 0.3363(5) 0.5444(2) 0.0541(12) Uani 1 1 d .
C23 C 0.4014(5) 0.9201(10) 0.5818(4) 0.098(2) Uani 1 1 d .
H23A H 0.4063 1.0018 0.5567 0.147 Uiso 1 1 calc R
H23B H 0.4633 0.9020 0.6160 0.147 Uiso 1 1 calc R
H23C H 0.3529 0.9342 0.6032 0.147 Uiso 1 1 calc R
C11 C 0.4811(4) 0.4605(5) 0.7943(2) 0.0524(11) Uani 1 1 d .
C12 C 0.4507(4) 0.5055(7) 0.8994(3) 0.0736(16) Uani 1 1 d .
H12A H 0.4706 0.6010 0.9027 0.110 Uiso 1 1 calc R
H12B H 0.5059 0.4481 0.9220 0.110 Uiso 1 1 calc R
H12C H 0.4017 0.4934 0.9204 0.110 Uiso 1 1 calc R
C8 C 0.5249(4) 0.4131(6) 0.6945(3) 0.0605(13) Uani 1 1 d .
C16 C 0.1114(4) 0.5529(6) 0.7128(3) 0.0713(16) Uani 1 1 d .
H16A H 0.1238 0.5749 0.7599 0.107 Uiso 1 1 calc R
H16B H 0.0424 0.5470 0.6899 0.107 Uiso 1 1 calc R
H16C H 0.1383 0.6242 0.6922 0.107 Uiso 1 1 calc R
C6 C 0.3206(4) 0.3197(5) 0.4801(3) 0.0622(13) Uani 1 1 d .
H6 H 0.3832 0.3205 0.4774 0.075 Uiso 1 1 calc R
C1 C 0.3061(4) 0.3368(5) 0.5420(3) 0.0563(12) Uani 1 1 d .
C24 C 0.1819(6) 0.6956(7) 0.5485(4) 0.092(2) Uani 1 1 d .
H24A H 0.1597 0.6183 0.5182 0.139 Uiso 1 1 calc R
H24B H 0.1351 0.7157 0.5706 0.139 Uiso 1 1 calc R
H24C H 0.2434 0.6731 0.5820 0.139 Uiso 1 1 calc R
C22 C 0.3731(4) 0.7987(8) 0.5342(3) 0.0813(19) Uani 1 1 d .
H22A H 0.3727 0.7160 0.5607 0.098 Uiso 1 1 calc R
H22B H 0.4228 0.7859 0.5131 0.098 Uiso 1 1 calc R
C9 C 0.5718(5) 0.5526(9) 0.6905(4) 0.094(2) Uani 1 1 d .
H9A H 0.5220 0.6218 0.6744 0.142 Uiso 1 1 calc R
H9B H 0.6083 0.5459 0.6598 0.142 Uiso 1 1 calc R
H9C H 0.6146 0.5781 0.7349 0.142 Uiso 1 1 calc R
C10 C 0.6028(5) 0.3019(8) 0.7277(3) 0.091(2) Uani 1 1 d .
H10A H 0.6390 0.3295 0.7734 0.136 Uiso 1 1 calc R
H10B H 0.6463 0.2926 0.7019 0.136 Uiso 1 1 calc R
H10C H 0.5714 0.2145 0.7285 0.136 Uiso 1 1 calc R
C21 C 0.3446(6) 0.9598(8) 0.4062(4) 0.099(2) Uani 1 1 d .
H21A H 0.4084 0.9556 0.4398 0.148 Uiso 1 1 calc R
H21B H 0.3363 1.0475 0.3831 0.148 Uiso 1 1 calc R
H21C H 0.3376 0.8861 0.3739 0.148 Uiso 1 1 calc R
C13 C 0.3079(3) 0.4533(5) 0.8012(2) 0.0479(10) 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'
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
N3 Co1 N1 173.12(17)
N3 Co1 N4 98.94(18)
N1 Co1 N4 87.18(18)
N3 Co1 N2 87.94(18)
N1 Co1 N2 85.85(18)
N4 Co1 N2 172.85(18)
C13 N3 C14 116.7(4)
C13 N3 Co1 128.1(3)
C14 N3 Co1 115.2(3)
C21 C20 N6 115.0(5)
C7 N1 C1 126.6(5)
C7 N1 Co1 117.8(4)
C1 N1 Co1 115.4(3)
C17 N2 C2 127.3(5)
C17 N2 Co1 117.2(4)
C2 N2 Co1 115.2(3)
C22 N6 C18 107.0(4)
C22 N6 C20 110.5(4)
C18 N6 C20 111.9(4)
C22 N6 C25 111.2(4)
C18 N6 C25 111.2(4)
C20 N6 C25 105.2(4)
N3 C14 C15 112.6(4)
N3 C14 C16 111.1(4)
C15 C14 C16 111.3(5)
N3 C14 C17 106.7(4)
C15 C14 C17 107.9(4)
C16 C14 C17 106.9(4)
O1 C7 N1 126.5(6)
O1 C7 C8 122.0(5)
N1 C7 C8 111.4(5)
C11 N5 C13 130.8(4)
C11 N5 C12 113.7(4)
C13 N5 C12 115.0(4)
C19 C18 N6 115.0(5)
C24 C25 N6 115.4(5)
C11 N4 C8 118.6(4)
C11 N4 Co1 126.2(4)
C8 N4 Co1 115.1(3)
O2 C17 N2 125.7(5)
O2 C17 C14 121.5(5)
N2 C17 C14 112.9(4)
C4 C5 C6 121.6(5)
C4 C3 C2 117.9(6)
C3 C4 C5 121.3(5)
C3 C2 C1 121.3(5)
C3 C2 N2 127.6(5)
C1 C2 N2 111.1(4)
O4 C11 N4 124.0(5)
O4 C11 N5 117.6(5)
N4 C11 N5 118.4(4)
N4 C8 C9 112.6(5)
N4 C8 C7 107.7(4)
C9 C8 C7 106.9(5)
N4 C8 C10 111.4(5)
C9 C8 C10 111.2(5)
C7 C8 C10 106.6(5)
C1 C6 C5 118.5(6)
C6 C1 N1 128.1(5)
C6 C1 C2 119.4(5)
N1 C1 C2 112.3(4)
C23 C22 N6 115.4(5)
O3 C13 N3 126.4(5)
O3 C13 N5 116.5(4)
N3 C13 N5 117.1(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Co1 N3 1.785(4)
Co1 N1 1.799(4)
Co1 N4 1.805(4)
Co1 N2 1.807(4)
N3 C13 1.344(6)
N3 C14 1.500(6)
O2 C17 1.231(6)
O4 C11 1.215(6)
C20 C21 1.475(8)
C20 N6 1.517(7)
N1 C7 1.340(7)
N1 C1 1.406(6)
O3 C13 1.197(6)
N2 C17 1.349(7)
N2 C2 1.421(6)
O1 C7 1.212(7)
N6 C22 1.499(7)
N6 C18 1.511(7)
N6 C25 1.524(6)
C14 C15 1.513(7)
C14 C16 1.529(7)
C14 C17 1.530(7)
C7 C8 1.540(8)
N5 C11 1.409(7)
N5 C13 1.419(6)
N5 C12 1.469(6)
C18 C19 1.503(8)
C25 C24 1.490(8)
N4 C11 1.350(6)
N4 C8 1.454(7)
C5 C4 1.374(9)
C5 C6 1.384(8)
C3 C4 1.368(8)
C3 C2 1.393(7)
C2 C1 1.409(8)
C23 C22 1.499(10)
C8 C9 1.520(9)
C8 C10 1.546(8)
C6 C1 1.382(7)
