#------------------------------------------------------------------------------
#$Date: 2024-05-05 06:04:35 +0300 (Sun, 05 May 2024) $
#$Revision: 291644 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/71/54/7715446.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_7715446
loop_
_publ_author_name
'Jhariat, Pampa'
'Kareem, Abdul'
'Kumari, Priyanka'
'Sarfudeen, Shafeeq'
'Panda, Premchand'
'Senthilkumar, Sellappan'
'Panda, Tamas'
_publ_section_title
;
 A series of isostructural metal-organic frameworks for an enhanced
 electro-catalytic oxygen evolution reaction.
;
_journal_issue                   15
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6568
_journal_page_last               6574
_journal_paper_doi               10.1039/d4dt00210e
_journal_volume                  53
_journal_year                    2024
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H14 Co2 N9 O12, 2(C2 H6 O)'
_chemical_formula_sum            'C34 H27 Co2 N9 O14'
_chemical_formula_weight         903.51
_chemical_name_common            Co-5TIA-X
_space_group_crystal_system      orthorhombic
_space_group_IT_number           36
_space_group_name_Hall           'C 2c -2'
_space_group_name_H-M_alt        'C m c 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2020-04-23
_audit_creation_method
;
  Olex2 1.2-ac2
  (compiled Nov  7 2012 10:34:12, GUI svn.r4372)
;
_audit_update_record
;
2024-03-01 deposited with the CCDC.	2024-03-05 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   29.746(2)
_cell_length_b                   11.0402(7)
_cell_length_c                   13.3648(7)
_cell_measurement_reflns_used    2827
_cell_measurement_temperature    293
_cell_measurement_theta_max      29.2154
_cell_measurement_theta_min      3.0423
_cell_volume                     4389.0(5)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
SHELXS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      293
_diffrn_detector_area_resol_mean 16.1640
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details
;
#__ type_ start__ end____ width___ exp.time_
  1 omega  -57.00  -31.00   1.0000  118.1400
omega____ theta____ kappa____ phi______ frames
    -      -18.5831  137.0000   38.0000 26

#__ type_ start__ end____ width___ exp.time_
  2 omega  -46.00   14.00   1.0000  118.1400
omega____ theta____ kappa____ phi______ frames
    -       18.5831  -19.0000 -150.0000 60

#__ type_ start__ end____ width___ exp.time_
  3 omega  -22.00   44.00   1.0000  118.1400
omega____ theta____ kappa____ phi______ frames
    -       18.5831  -37.0000  120.0000 66
;
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_UB_11      0.0238073000
_diffrn_orient_matrix_UB_12      0.0017488000
_diffrn_orient_matrix_UB_13      0.0030292000
_diffrn_orient_matrix_UB_21      -0.0013955000
_diffrn_orient_matrix_UB_22      0.0429283000
_diffrn_orient_matrix_UB_23      0.0392969000
_diffrn_orient_matrix_UB_31      -0.0004074000
_diffrn_orient_matrix_UB_32      -0.0477179000
_diffrn_orient_matrix_UB_33      0.0355687000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0475
_diffrn_reflns_av_unetI/netI     0.0629
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            6377
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         3.05
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.826
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.765
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.16
_refine_diff_density_max         1.322
_refine_diff_density_min         -0.863
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     261
_refine_ls_number_reflns         6100
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0659
_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)+(0.1293P)²+7.1924P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1961
_refine_ls_wR_factor_ref         0.2126
_reflns_number_gt                3578
_reflns_number_total             6100
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d4dt00210e2.cif
_cod_data_source_block           CoTIA
_cod_depositor_comments
'Adding full bibliography for 7715445--7715447.cif.'
_cod_database_code               7715446
_reflns_odcompleteness_completeness 99.44
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  H14 of C14, H1A of N1, H5 of C5, H4 of C4, H8 of C8, H1 of C1, {H12B,H12A}
  of C12, H10 of C10, H9 of C9
 At 1.5 times of:
  H1B of O1, {H18B,H18C,H18A} of C18
2. Uiso/Uaniso restraints and constraints
Uanis(C18) = Uanis(C12) = Uanis(O1)
3.a Secondary CH2 refined with riding coordinates:
 C12(H12B,H12A)
3.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C1(H1), N1(H1A), C4(H4), C5(H5), C8(H8), C9(H9), C10(H10)
3.c Idealised Me refined as rotating group:
 C18(H18B,H18C,H18A)
3.d Idealised tetrahedral OH refined as rotating group:
 O1(H1B)
;
loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 'x, y, z'
2 '-x, -y, z+1/2'
3 '-x, y, z'
4 'x, -y, z+1/2'
5 'x+1/2, y+1/2, z'
6 '-x+1/2, -y+1/2, z+1/2'
7 '-x+1/2, y+1/2, z'
8 '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
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.17155(2) 0.06203(6) 0.35435(6) 0.0243(2) Uani 1 1 d . . .
O3 O 0.18062(17) 0.2008(4) 0.4419(4) 0.0369(10) Uani 1 1 d . . .
N4 N 0.17348(16) -0.0856(5) 0.4459(4) 0.0289(11) Uani 1 1 d . . .
O5 O 0.1664(2) 0.3313(5) 0.3189(4) 0.0441(14) Uani 1 1 d . . .
O6 O 0.11853(15) 0.0660(5) 0.2626(4) 0.0403(11) Uani 1 1 d . . .
C7 C 0.1791(2) 0.3044(6) 0.4042(5) 0.0305(14) Uani 1 1 d . . .
O8 O 0.25411(19) 0.1822(4) 0.2586(4) 0.0454(13) Uani 1 1 d . . .
O9 O 0.21810(14) 0.0062(4) 0.2630(4) 0.0389(11) Uani 1 1 d . . .
O10 O 0.08533(18) 0.0879(7) 0.4091(4) 0.0572(17) Uani 1 1 d . . .
C11 C 0.1948(2) 0.4067(6) 0.4764(5) 0.0307(13) Uani 1 1 d . . .
N12 N 0.18606(17) 0.7374(5) 0.5123(4) 0.0274(10) Uani 1 1 d . . .
C13 C 0.0407(2) 0.1032(7) 0.2624(5) 0.0345(14) Uani 1 1 d . . .
C14 C 0.1861(2) 0.5273(6) 0.4571(4) 0.0279(12) Uani 1 1 d . . .
H14 H 0.1717 0.5503 0.3983 0.033 Uiso 1 1 calc R . .
C15 C 0.1989(2) 0.6125(5) 0.5258(5) 0.0283(12) Uani 1 1 d . . .
C16 C 0.0836(2) 0.0868(7) 0.3163(6) 0.0379(15) Uani 1 1 d . . .
C1 C 0.2208(2) 0.5822(6) 0.6135(5) 0.0264(12) Uani 1 1 d . . .
H1 H 0.2290 0.6418 0.6592 0.032 Uiso 1 1 calc R . .
C3 C 0.26983(19) 0.0395(6) 0.1321(4) 0.0264(12) Uani 1 1 d . . .
N1 N 0.1550(2) -0.0871(5) 0.5410(4) 0.0335(11) Uani 1 1 d . . .
H1A H 0.1404 -0.0291 0.5692 0.040 Uiso 1 1 calc R . .
C4 C 0.1638(2) 0.8085(6) 0.5797(5) 0.0323(13) Uani 1 1 d . . .
H4 H 0.1561 0.7850 0.6442 0.039 Uiso 1 1 calc R . .
C5 C 0.1917(2) -0.1907(5) 0.4309(5) 0.0290(12) Uani 1 1 d . . .
H5 H 0.2064 -0.2136 0.3725 0.035 Uiso 1 1 calc R . .
C6 C 0.2466(2) 0.0812(6) 0.2260(5) 0.0273(12) Uani 1 1 d . . .
N7 N 0.0000 0.1742(9) 0.0071(6) 0.048(2) Uani 1 2 d S . .
C8 C 0.0000 0.0953(10) 0.3125(7) 0.037(2) Uani 1 2 d S . .
H8 H 0.0000 0.0845 0.3815 0.045 Uiso 1 2 calc SR . .
C9 C 0.21592(19) 0.3743(6) 0.5639(4) 0.0271(13) Uani 1 1 d . . .
H9 H 0.2207 0.2928 0.5776 0.032 Uiso 1 1 calc R . .
C10 C 0.0406(2) 0.1280(7) 0.1597(5) 0.0391(16) Uani 1 1 d . . .
H10 H 0.0676 0.1334 0.1249 0.047 Uiso 1 1 calc R . .
C17 C 0.0000 0.1444(11) 0.1096(7) 0.039(2) Uani 1 2 d S . .
C12 C 0.1136(4) 0.1467(13) 0.6182(9) 0.0850(16) Uani 1 1 d . . .
H12B H 0.1143 0.0603 0.6314 0.102 Uiso 1 1 calc R . .
H12A H 0.1271 0.1599 0.5530 0.102 Uiso 1 1 calc R . .
N2 N 0.0220(4) 0.2129(11) -0.1451(7) 0.112(4) Uani 1 1 d . . .
O1 O 0.1404(3) 0.2065(8) 0.6915(6) 0.0850(16) Uani 1 1 d . . .
H1B H 0.1667 0.1863 0.6848 0.128 Uiso 1 1 calc R . .
C18 C 0.0656(4) 0.1862(12) 0.6139(9) 0.0850(16) Uani 1 1 d . . .
H18B H 0.0600 0.2257 0.5512 0.128 Uiso 1 1 calc R . .
H18C H 0.0597 0.2416 0.6677 0.128 Uiso 1 1 calc R . .
H18A H 0.0464 0.1168 0.6202 0.128 Uiso 1 1 calc R . .
C19 C 0.0344(5) 0.1818(15) -0.0570(8) 0.101(5) 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'
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'
N N 0.0061 0.0033 '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
O3 Co1 N4 105.3(2) . . ?
O3 Co1 O6 117.5(2) . . ?
O6 Co1 N4 114.1(2) . . ?
O9 Co1 O3 121.8(2) . . ?
O9 Co1 N4 95.9(2) . . ?
O9 Co1 O6 100.6(2) . . ?
C7 O3 Co1 118.2(4) . . ?
N1 N4 Co1 123.3(4) . . ?
C5 N4 Co1 129.4(4) . . ?
C5 N4 N1 107.3(5) . . ?
C16 O6 Co1 107.4(5) . . ?
O3 C7 C11 113.8(6) . . ?
O5 C7 O3 127.0(7) . . ?
O5 C7 C11 119.2(6) . . ?
C6 O9 Co1 120.5(4) . . ?
C14 C11 C7 121.9(6) . . ?
C9 C11 C7 118.4(6) . . ?
C9 C11 C14 119.6(6) . . ?
C4 N12 C15 126.6(5) . . ?
C5 N12 C15 128.8(5) 1_565 . ?
C5 N12 C4 104.6(5) 1_565 . ?
C8 C13 C16 120.7(6) . . ?
C8 C13 C10 119.0(6) . . ?
C10 C13 C16 120.3(6) . . ?
C11 C14 H14 120.5 . . ?
C15 C14 C11 119.1(6) . . ?
C15 C14 H14 120.5 . . ?
C14 C15 N12 120.0(5) . . ?
C14 C15 C1 122.3(6) . . ?
C1 C15 N12 117.5(5) . . ?
O6 C16 C13 116.6(6) . . ?
O10 C16 O6 121.8(7) . . ?
O10 C16 C13 121.5(7) . . ?
C15 C1 H1 120.7 . . ?
C15 C1 C3 118.6(6) . 6 ?
C3 C1 H1 120.7 6 . ?
C1 C3 C6 122.4(6) 6_554 . ?
C9 C3 C1 118.9(6) 6_554 6_554 ?
C9 C3 C6 118.7(6) 6_554 . ?
N4 N1 H1A 126.3 . . ?
C4 N1 N4 107.3(5) 1_545 . ?
C4 N1 H1A 126.3 1_545 . ?
N12 C4 H4 124.8 . . ?
N1 C4 N12 110.4(6) 1_565 . ?
N1 C4 H4 124.8 1_565 . ?
N4 C5 N12 110.4(5) . 1_545 ?
N4 C5 H5 124.8 . . ?
N12 C5 H5 124.8 1_545 . ?
O8 C6 O9 125.0(6) . . ?
O8 C6 C3 119.6(6) . . ?
O9 C6 C3 115.3(5) . . ?
C19 N7 C17 129.6(6) . . ?
C19 N7 C17 129.6(6) 3 . ?
C19 N7 C19 99.9(12) 3 . ?
C13 C8 C13 121.7(8) . 3 ?
C13 C8 H8 119.2 3 . ?
C13 C8 H8 119.2 . . ?
C11 C9 C3 121.5(6) . 6 ?
C11 C9 H9 119.3 . . ?
C3 C9 H9 119.3 6 . ?
C13 C10 H10 120.1 . . ?
C17 C10 C13 119.9(6) . . ?
C17 C10 H10 120.1 . . ?
C10 C17 N7 119.9(4) . . ?
C10 C17 N7 119.9(4) 3 . ?
C10 C17 C10 120.3(8) 3 . ?
H12B C12 H12A 107.5 . . ?
O1 C12 H12B 108.5 . . ?
O1 C12 H12A 108.5 . . ?
O1 C12 C18 115.2(10) . . ?
C18 C12 H12B 108.5 . . ?
C18 C12 H12A 108.5 . . ?
C19 N2 N2 106.7(8) . 3 ?
C12 O1 H1B 109.5 . . ?
C12 C18 H18B 109.5 . . ?
C12 C18 H18C 109.5 . . ?
C12 C18 H18A 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H18B C18 H18A 109.5 . . ?
H18C C18 H18A 109.5 . . ?
N2 C19 N7 112.6(12) . . ?
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 O3 1.947(5) . ?
Co1 N4 2.038(6) . ?
Co1 O6 1.998(5) . ?
Co1 O9 1.946(4) . ?
O3 C7 1.250(9) . ?
N4 N1 1.385(8) . ?
N4 C5 1.296(8) . ?
O5 C7 1.238(8) . ?
O6 C16 1.284(9) . ?
C7 C11 1.557(9) . ?
O8 C6 1.218(8) . ?
O9 C6 1.284(7) . ?
O10 C16 1.241(9) . ?
C11 C14 1.381(9) . ?
C11 C9 1.375(9) . ?
N12 C15 1.443(8) . ?
N12 C4 1.365(8) . ?
N12 C5 1.358(8) 1_565 ?
C13 C16 1.477(9) . ?
C13 C8 1.387(7) . ?
C13 C10 1.399(9) . ?
C14 H14 0.9300 . ?
C14 C15 1.368(9) . ?
C15 C1 1.381(8) . ?
C1 H1 0.9300 . ?
C1 C3 1.395(9) 6 ?
C3 C1 1.395(9) 6_554 ?
C3 C6 1.505(8) . ?
C3 C9 1.384(9) 6_554 ?
N1 H1A 0.8600 . ?
N1 C4 1.290(8) 1_545 ?
C4 N1 1.290(8) 1_565 ?
C4 H4 0.9300 . ?
C5 N12 1.358(8) 1_545 ?
C5 H5 0.9300 . ?
N7 C17 1.409(12) . ?
N7 C19 1.338(13) . ?
N7 C19 1.338(13) 3 ?
C8 C13 1.387(7) 3 ?
C8 H8 0.9300 . ?
C9 C3 1.384(9) 6 ?
C9 H9 0.9300 . ?
C10 H10 0.9300 . ?
C10 C17 1.394(7) . ?
C17 C10 1.394(7) 3 ?
C12 H12B 0.9700 . ?
C12 H12A 0.9700 . ?
C12 O1 1.425(14) . ?
C12 C18 1.493(17) . ?
N2 N2 1.31(2) 3 ?
N2 C19 1.281(15) . ?
O1 H1B 0.8200 . ?
C18 H18B 0.9600 . ?
C18 H18C 0.9600 . ?
C18 H18A 0.9600 . ?
