#------------------------------------------------------------------------------
#$Date: 2024-07-05 15:58:08 +0300 (Fri, 05 Jul 2024) $
#$Revision: 292755 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/57/17/1571728.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_1571728
loop_
_publ_author_name
'Trotta, Caterina'
'Dahiya, Pardeep'
'Baldinelli, Lorenzo'
'Menendez Rodriguez, Gabriel'
'Chakraborty, Priyanka'
'Bistoni, Giovanni'
'De Angelis, Filippo'
'Sundararaju, Basker'
'Macchioni, Alceo'
_publ_section_title
;
 A cobalt molecular catalyst for hydrogen evolution reaction with
 remarkable activity in phosphate buffered water solution
;
_journal_issue                   13
_journal_name_full               'Catalysis Science & Technology'
_journal_page_first              3699
_journal_page_last               3706
_journal_paper_doi               10.1039/D4CY00209A
_journal_volume                  14
_journal_year                    2024
_chemical_formula_moiety         'C17 H25 Co I N2, I'
_chemical_formula_sum            'C17 H25 Co I2 N2'
_chemical_formula_weight         570.144
_chemical_name_systematic        Complex-2
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_Int_Tables_number      2
_atom_sites_solution_primary     dual
_audit_creation_date             2023-09-22
_audit_creation_method
;
Olex2 1.5
(compiled 2021.08.20 svn.r13c46975 for OlexSys, GUI svn.r6394)
;
_audit_update_record
;
2023-09-27 deposited with the CCDC.	2024-05-28 downloaded from the CCDC.
;
_cell_angle_alpha                89.106(2)
_cell_angle_beta                 83.431(2)
_cell_angle_gamma                76.170(2)
_cell_formula_units_Z            2
_cell_length_a                   8.2020(7)
_cell_length_b                   9.8816(9)
_cell_length_c                   12.3164(11)
_cell_measurement_reflns_used    9707
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.390
_cell_measurement_theta_min      2.228
_cell_volume                     962.86(15)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_collection       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.5 (Bourhis et al., 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 5.6
_diffrn_detector_type            'Bruker SMART CCD 6000 area detector'
_diffrn_measured_fraction_theta_full 0.9983
_diffrn_measured_fraction_theta_max 0.9958
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART CCD 6000 area detector'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0468
_diffrn_reflns_av_unetI/netI     0.0443
_diffrn_reflns_Laue_measured_fraction_full 0.9983
_diffrn_reflns_Laue_measured_fraction_max 0.9958
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15272
_diffrn_reflns_point_group_measured_fraction_full 0.9983
_diffrn_reflns_point_group_measured_fraction_max 0.9958
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.39
_diffrn_reflns_theta_min         2.57
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_current           1.0
_diffrn_source_power             0.05
_diffrn_source_target            Mo
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_T_max  0.921
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1915 before and 0.0625 after correction.
The Ratio of minimum to maximum transmission is 0.6720.
The λ/2 correction factor is Not present.
;
_exptl_crystal_colour            'metallic greenish green'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   greenish
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    1.967
_exptl_crystal_description       needle
_exptl_crystal_F_000             547.299
_exptl_crystal_preparation       'Slow evaporation'
_exptl_crystal_recrystallization_method 'Slow evaporation'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.8570
_refine_diff_density_min         -1.1378
_refine_diff_density_rms         0.1521
_refine_ls_d_res_high            0.7474
_refine_ls_d_res_low             7.9123
_refine_ls_goodness_of_fit_ref   0.7766
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    37
_refine_ls_number_parameters     205
_refine_ls_number_reflns         4792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.7766
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.0008
_refine_ls_shift/su_mean         0.0001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0913
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              10
_reflns_limit_h_min              -10
_reflns_limit_k_max              13
_reflns_limit_k_min              -13
_reflns_limit_l_max              16
_reflns_limit_l_min              0
_reflns_number_gt                4352
_reflns_number_total             4792
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d4cy00209a2.cif
_cod_data_source_block           19sepa_1_0m
_cod_depositor_comments
'Adding full bibliography for 1571727--1571728.cif.'
_cod_database_code               1571728
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 N2(H2)
2.b Secondary CH2 refined with riding coordinates:
 C16(H16a,H16b)
2.c Aromatic/amide H refined with riding coordinates:
 C11(H11), C14(H14), C13(H13), C12(H12)
2.d Idealised Me refined as rotating group:
 C6(H6a,H6b,H6c), C7(H7a,H7b,H7c), C8(H8a,H8b,H8c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C17(H17a,H17b,H17c)
;
_olex2_exptl_crystal_mounting_method loop
_olex2_submission_original_sample_id Complex-2
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 -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_refinement_flags_posn
I1 I 0.67243(2) 0.15083(2) 0.388312(15) 0.01895(8) Uani 1.000000 .
Co1 Co 0.41586(5) 0.21014(4) 0.27260(3) 0.01369(10) Uani 1.000000 .
N1 N 0.2748(3) 0.2949(3) 0.40723(19) 0.0171(5) Uani 1.000000 .
N2 N 0.4335(3) 0.4075(3) 0.24668(19) 0.0179(5) Uani 1.000000 .
C1 C 0.5308(4) 0.0838(3) 0.1384(2) 0.0168(6) Uani 1.000000 .
C2 C 0.3918(4) 0.1856(3) 0.1074(2) 0.0183(6) Uani 1.000000 .
C3 C 0.2410(4) 0.1739(3) 0.1753(2) 0.0163(5) Uani 1.000000 .
C4 C 0.2877(4) 0.0548(3) 0.2426(2) 0.0173(5) Uani 1.000000 .
C5 C 0.4646(4) -0.0005(3) 0.2220(2) 0.0180(6) Uani 1.000000 .
C6 C 0.7121(4) 0.0558(3) 0.0870(2) 0.0223(6) Uani 1.000000 .
C7 C 0.3910(4) 0.2861(3) 0.0143(2) 0.0199(6) Uani 1.000000 .
C8 C 0.0672(4) 0.2595(3) 0.1675(3) 0.0222(6) Uani 1.000000 .
C9 C 0.1695(4) -0.0150(3) 0.3109(2) 0.0225(6) Uani 1.000000 .
C10 C 0.5607(4) -0.1313(3) 0.2702(3) 0.0223(6) Uani 1.000000 .
C11 C 0.1892(4) 0.2285(3) 0.4829(2) 0.0197(6) Uani 1.000000 .
C12 C 0.1125(4) 0.2879(3) 0.5815(2) 0.0221(6) Uani 1.000000 .
C13 C 0.1235(4) 0.4224(3) 0.6060(2) 0.0223(6) Uani 1.000000 .
C14 C 0.2098(4) 0.4914(3) 0.5298(2) 0.0212(6) Uani 1.000000 .
C15 C 0.2852(4) 0.4246(3) 0.4314(2) 0.0183(6) Uani 1.000000 .
C16 C 0.3954(4) 0.4874(3) 0.3513(2) 0.0191(6) Uani 1.000000 .
C17 C 0.5908(4) 0.4341(3) 0.1878(3) 0.0226(6) Uani 1.000000 .
I2 I 0.12564(2) 0.66903(2) 0.127292(15) 0.02114(9) Uani 1.000000 .
H11 H 0.1822(4) 0.1385(3) 0.4672(2) 0.0236(7) Uiso 1.000000 R
H14 H 0.2175(4) 0.5817(3) 0.5440(2) 0.0254(7) Uiso 1.000000 R
H13 H 0.0736(4) 0.4649(3) 0.6725(2) 0.0267(7) Uiso 1.000000 R
H12 H 0.0544(4) 0.2392(3) 0.6311(2) 0.0265(7) Uiso 1.000000 R
H6a H 0.7336(9) 0.1396(7) 0.0544(17) 0.0334(9) Uiso 1.000000 GR
H6b H 0.7863(4) 0.026(2) 0.1421(4) 0.0334(9) Uiso 1.000000 GR
H6c H 0.7315(9) -0.0156(18) 0.0319(14) 0.0334(9) Uiso 1.000000 GR
H7a H 0.341(3) 0.3792(4) 0.0412(4) 0.0298(9) Uiso 1.000000 GR
H7b H 0.5049(4) 0.2801(18) -0.0177(12) 0.0298(9) Uiso 1.000000 GR
H7c H 0.326(2) 0.2631(15) -0.0399(9) 0.0298(9) Uiso 1.000000 GR
H8a H 0.0001(9) 0.261(2) 0.2368(6) 0.0333(9) Uiso 1.000000 GR
H8b H 0.0720(5) 0.3529(7) 0.1477(19) 0.0333(9) Uiso 1.000000 GR
H8c H 0.0172(12) 0.2200(14) 0.1128(14) 0.0333(9) Uiso 1.000000 GR
H9a H 0.2240(12) -0.061(2) 0.3711(12) 0.0337(9) Uiso 1.000000 GR
H9b H 0.0695(14) 0.0534(5) 0.3383(17) 0.0337(9) Uiso 1.000000 GR
H9c H 0.139(3) -0.0828(19) 0.2672(6) 0.0337(9) Uiso 1.000000 GR
H10a H 0.6796(4) -0.1421(14) 0.2493(17) 0.0335(9) Uiso 1.000000 GR
H10b H 0.538(3) -0.1260(11) 0.3484(3) 0.0335(9) Uiso 1.000000 GR
H10c H 0.526(2) -0.2099(4) 0.2438(16) 0.0335(9) Uiso 1.000000 GR
H16a H 0.4999(4) 0.4871(3) 0.3811(2) 0.0230(7) Uiso 1.000000 R
H16b H 0.3390(4) 0.5833(3) 0.3383(2) 0.0230(7) Uiso 1.000000 R
H17a H 0.6853(6) 0.390(2) 0.2257(11) 0.0339(9) Uiso 1.000000 GR
H17b H 0.6069(17) 0.396(2) 0.1149(7) 0.0339(9) Uiso 1.000000 GR
H17c H 0.5820(13) 0.5327(3) 0.1847(18) 0.0339(9) Uiso 1.000000 GR
H2 H 0.3493(3) 0.4466(3) 0.20565(19) 0.0215(6) Uiso 1.000000 R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
_atom_type_scat_dispersion_source
C 0.00347 0.00161 2.31000 1.02000 1.58860 0.86500 20.84390 10.20750 0.56870
51.65120 0.21560 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
Co 0.35655 0.96576 12.28410 7.34090 4.00340 2.34880 4.27910 0.27840 13.53590
71.16920 1.01180 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
H 0.00000 0.00000 0.49300 0.32291 0.14019 0.04081 10.51090 26.12570 3.14236
57.79970 0.00304 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
I -0.41187 1.83264 20.14720 18.99490 7.51380 2.27350 4.34700 0.38140 27.76600
66.87760 4.07120 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
N 0.00653 0.00323 12.21260 3.13220 2.01250 1.16630 0.00570 9.89330 28.99750
0.58260 -11.52900 'International Tables Volume C Table 6.1.1.4 (pp. 500-502)'
'Henke, Gullikson and Davis, At. Data and Nucl. Data Tables, 1993, 54, 2'
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
N1 Co1 I1 87.41(7) . . ?
N2 Co1 I1 93.69(7) . . ?
N2 Co1 N1 82.17(10) . . ?
C1 Co1 I1 96.93(8) . . ?
C1 Co1 N1 165.93(10) . . ?
C1 Co1 N2 110.77(10) . . ?
C2 Co1 I1 133.57(8) . . ?
C2 Co1 N1 138.88(11) . . ?
C2 Co1 N2 90.54(10) . . ?
C2 Co1 C1 39.62(11) . . ?
C3 Co1 I1 157.71(8) . . ?
C3 Co1 N1 103.47(11) . . ?
C3 Co1 N2 106.90(11) . . ?
C3 Co1 C1 68.17(11) . . ?
C3 Co1 C2 40.49(10) . . ?
C4 Co1 I1 119.79(8) . . ?
C4 Co1 N1 99.09(10) . . ?
C4 Co1 N2 146.50(11) . . ?
C4 Co1 C1 67.13(11) . . ?
C4 Co1 C2 66.42(10) . . ?
C4 Co1 C3 39.96(11) . . ?
C5 Co1 I1 90.57(8) . . ?
C5 Co1 N1 126.40(10) . . ?
C5 Co1 N2 151.31(10) . . ?
C5 Co1 C1 40.54(10) . . ?
C5 Co1 C2 66.55(11) . . ?
C5 Co1 C3 67.27(12) . . ?
C5 Co1 C4 39.17(12) . . ?
C11 N1 Co1 126.2(2) . . ?
C15 N1 Co1 115.41(19) . . ?
C15 N1 C11 117.8(2) . . ?
C16 N2 Co1 110.24(17) . . ?
C17 N2 Co1 119.30(19) . . ?
C17 N2 C16 108.4(2) . . ?
C2 C1 Co1 70.59(16) . . ?
C5 C1 Co1 70.97(15) . . ?
C5 C1 C2 107.1(2) . . ?
C6 C1 Co1 128.5(2) . . ?
C6 C1 C2 127.2(2) . . ?
C6 C1 C5 125.4(3) . . ?
C1 C2 Co1 69.79(16) . . ?
C3 C2 Co1 68.89(15) . . ?
C3 C2 C1 109.1(2) . . ?
C7 C2 Co1 130.6(2) . . ?
C7 C2 C1 127.6(2) . . ?
C7 C2 C3 123.1(3) . . ?
C2 C3 Co1 70.63(16) . . ?
C4 C3 Co1 71.84(16) . . ?
C4 C3 C2 106.8(3) . . ?
C8 C3 Co1 127.8(2) . . ?
C8 C3 C2 126.2(3) . . ?
C8 C3 C4 126.6(2) . . ?
C3 C4 Co1 68.20(16) . . ?
C5 C4 Co1 70.34(16) . . ?
C5 C4 C3 108.8(2) . . ?
C9 C4 Co1 134.5(2) . . ?
C9 C4 C3 126.4(3) . . ?
C9 C4 C5 124.2(3) . . ?
C1 C5 Co1 68.49(16) . . ?
C4 C5 Co1 70.48(17) . . ?
C4 C5 C1 107.8(3) . . ?
C10 C5 Co1 131.2(2) . . ?
C10 C5 C1 126.6(3) . . ?
C10 C5 C4 125.3(3) . . ?
C12 C11 N1 123.2(3) . . ?
C13 C12 C11 118.8(3) . . ?
C14 C13 C12 118.7(3) . . ?
C15 C14 C13 119.5(3) . . ?
C14 C15 N1 122.0(3) . . ?
C16 C15 N1 115.8(3) . . ?
C16 C15 C14 121.9(3) . . ?
C15 C16 N2 110.4(2) . . ?
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
I1 Co1 2.6218(5) . ?
Co1 N1 1.983(2) . ?
Co1 N2 2.008(2) . ?
Co1 C1 2.080(3) . ?
Co1 C2 2.090(3) . ?
Co1 C3 2.067(3) . ?
Co1 C4 2.115(3) . ?
Co1 C5 2.113(3) . ?
N1 C11 1.357(3) . ?
N1 C15 1.345(4) . ?
N2 C16 1.484(3) . ?
N2 C17 1.484(3) . ?
C1 C2 1.413(4) . ?
C1 C5 1.453(4) . ?
C1 C6 1.510(4) . ?
C2 C3 1.439(4) . ?
C2 C7 1.504(4) . ?
C3 C4 1.430(4) . ?
C3 C8 1.487(4) . ?
C4 C5 1.418(4) . ?
C4 C9 1.497(4) . ?
C5 C10 1.497(4) . ?
C11 C12 1.374(4) . ?
C12 C13 1.394(4) . ?
C13 C14 1.380(4) . ?
C14 C15 1.395(4) . ?
C15 C16 1.489(4) . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Co1 N1 C11 C12 170.9(3) . . . . ?
Co1 N1 C15 C14 -172.1(2) . . . . ?
Co1 N1 C15 C16 2.4(2) . . . . ?
Co1 N2 C16 C15 -25.3(2) . . . . ?
Co1 C1 C2 C3 -57.72(17) . . . . ?
Co1 C1 C2 C7 126.29(17) . . . . ?
Co1 C1 C5 C4 59.76(18) . . . . ?
Co1 C1 C5 C10 -126.12(17) . . . . ?
Co1 C2 C1 C5 61.93(17) . . . . ?
Co1 C2 C1 C6 -124.14(17) . . . . ?
Co1 C2 C3 C4 -63.14(17) . . . . ?
Co1 C2 C3 C8 123.26(18) . . . . ?
Co1 C3 C2 C1 58.27(18) . . . . ?
Co1 C3 C2 C7 -125.52(16) . . . . ?
Co1 C3 C4 C5 -58.72(17) . . . . ?
Co1 C3 C4 C9 130.06(17) . . . . ?
Co1 C4 C3 C2 62.34(17) . . . . ?
Co1 C4 C3 C8 -124.10(18) . . . . ?
Co1 C4 C5 C1 -58.51(17) . . . . ?
Co1 C4 C5 C10 127.27(17) . . . . ?
Co1 C5 C1 C2 -61.68(18) . . . . ?
Co1 C5 C1 C6 124.26(17) . . . . ?
Co1 C5 C4 C3 57.42(17) . . . . ?
Co1 C5 C4 C9 -131.13(16) . . . . ?
N1 C11 C12 C13 -0.4(4) . . . . ?
N1 C15 C14 C13 0.9(3) . . . . ?
N1 C15 C16 N2 15.5(3) . . . . ?
N2 C16 C15 C14 -170.0(2) . . . . ?
C1 C2 C3 C4 -4.9(3) . . . . ?
C1 C2 C3 C8 -178.5(2) . . . . ?
C1 C5 C4 C3 -1.1(3) . . . . ?
C1 C5 C4 C9 170.4(2) . . . . ?
C2 C3 C4 C5 3.6(3) . . . . ?
C2 C3 C4 C9 -167.6(2) . . . . ?
C3 C4 C5 C10 -175.3(2) . . . . ?
C11 C12 C13 C14 0.5(4) . . . . ?
C12 C13 C14 C15 -0.8(4) . . . . ?
C13 C14 C15 C16 -173.3(3) . . . . ?
