Facile water oxidation by dinuclear mixed-valence CoIII/CoII complexes: the role of coordinated water
Dey, Atanu; Guha, Anku; Kumar, Vierandra; Bawari, Sumit; Narayanan, Tharangattu N.; Chandrasekhar, Vadapalli; Dalton Transactions  (2021) –; doi:10.1039/D1DT01910D

data_7708401
_publ_section_title
;
 Facile water oxidation by dinuclear mixed-valence CoIII/CoII complexes:
 the role of coordinated water
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT01910D
_journal_year                    2021
_chemical_formula_moiety         'C26 H35 Co2 N2 O13, C3 H7 N O, 1.5(O)'
_chemical_formula_sum            'C29 H42 Co2 N3 O15.5'
_chemical_formula_weight         798.51
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-11-23
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-01-15 deposited with the CCDC.	2021-09-02 downloaded from the CCDC.
;
_cell_angle_alpha                85.875(2)
_cell_angle_beta                 89.344(2)
_cell_angle_gamma                74.882(2)
_cell_formula_units_Z            2
_cell_length_a                   8.9294(2)
_cell_length_b                   10.1492(3)
_cell_length_c                   19.8943(5)
_cell_measurement_reflns_used    12938
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      28.9180
_cell_measurement_theta_min      3.0210
_cell_volume                     1735.99(8)
_computing_cell_refinement       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.29d (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      298
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w      3.00  41.00   0.50   21.71    --    7.10  48.00 -78.00   76
  2  \w    -56.00  -1.00   0.50   21.71    --    7.10 -48.00 133.00  110
  3  \w     -3.00  22.00   0.50   21.71    --   -7.50  48.00 -78.00   50
  4  \w    -60.00 -35.00   0.50   21.71    --   -7.50 -48.00 133.00   50
  5  \w     50.00  96.00   0.50   21.71    --    7.10  77.00-120.00   92
  6  \w     50.00  96.00   0.50   21.71    --    7.10  77.00 -60.00   92
  7  \w     50.00  95.00   0.50   21.71    --    7.10  77.00-150.00   90
  8  \w    -28.00   0.00   0.50   21.71    --   -7.50 -77.00 -90.00   56
  9  \w    -96.00  21.00   0.50   21.71    --   -7.50 -57.00   0.00  234
 10  \w    -36.00 -10.00   0.50   21.71    --   -7.50 -77.00  60.00   52
 11  \w    -63.00  35.00   0.50   21.71    --   -7.50 -82.00 120.00  196
 12  \w    -23.00  29.00   0.50   21.71    --   -7.50 -77.00 150.00  104
 13  \w    -63.00  26.00   0.50   21.71    --   -7.50 -82.00 -30.00  178
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC12 (RINC): Kappa single'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0213392000
_diffrn_orient_matrix_UB_12      0.0588674000
_diffrn_orient_matrix_UB_13      0.0187286000
_diffrn_orient_matrix_UB_21      -0.0692406000
_diffrn_orient_matrix_UB_22      -0.0174558000
_diffrn_orient_matrix_UB_23      0.0100869000
_diffrn_orient_matrix_UB_31      0.0390000000
_diffrn_orient_matrix_UB_32      -0.0386971000
_diffrn_orient_matrix_UB_33      0.0287289000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1502
_diffrn_reflns_av_unetI/netI     0.0805
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            30267
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         4.108
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.030
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.92684
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.29d (Rigaku Oxford Diffraction, 2017)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            brown
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.528
_exptl_crystal_description       block
_exptl_crystal_F_000             830
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.499
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         6097
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0715
_refine_ls_R_factor_gt           0.0642
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1143P)^2^+1.7246P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1841
_refine_ls_wR_factor_ref         0.1910
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5206
_reflns_number_total             6097
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01910d2.cif
_cod_data_source_block           1a
_cod_depositor_comments
;

2025-04-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C58 H84 Co4 N6 O31'
_cod_original_formula_weight         1597.03
_cod_original_formula_moiety         '2(C26 H35 Co2 N2 O13), 2(C3 H7 N O), 3(O)'
_cod_original_formula_units_Z            1
_cod_database_code               7708401
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         CHNCoO
_shelx_estimated_absorpt_t_max   0.886
_shelx_estimated_absorpt_t_min   0.783
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O009-H009
 0.85 with sigma of 0.01
 O00A-H00C
 0.85 with sigma of 0.01
 C00Z-H009
 1.905587 with sigma of 0.02
 Co02-H009
 2.749374 with sigma of 0.02
 C00T-H00C
 1.878578 with sigma of 0.02
 Co02-H00C
 2.658112 with sigma of 0.02
3.a Rotating group:
 O008(H00A,H00B)
3.b Secondary CH2 refined with riding coordinates:
 C00S(H00E,H00F), C00T(H00H,H00I), C00X(H00J,H00L), C00Y(H00M,H00N), C00Z(H00O,
 H00P), C013(H01A,H01B)
3.c Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00Q(H00Q), C00W(H00W), C011(H011), C012(H012), C015(H015),
 C016(H016), C017(H017), C018(H018)
3.d Idealised Me refined as rotating group:
 C014(H01C,H01D,H01E), C019(H01F,H01G,H01H), C01A(H01L,H01M,H01N), C01B(H01O,
 H01P,H01Q), C01D(H01I,H01J,H01K)
3.e Idealised tetrahedral OH refined as rotating group:
 O00B(H00D), O00G(H00G)
;
_shelx_res_checksum              37072
_shelx_hkl_checksum              88554
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.589
_oxdiff_exptl_absorpt_empirical_full_min 0.495