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_7708402
_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         'C32 H37 Co2 N2 O13, 3(H2 O), C H4 O'
_chemical_formula_sum            'C33 H47 Co2 N2 O17'
_chemical_formula_weight         861.58
_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             2020-10-25
_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                99.539(2)
_cell_angle_beta                 91.887(2)
_cell_angle_gamma                92.049(2)
_cell_formula_units_Z            2
_cell_length_a                   8.8633(3)
_cell_length_b                   10.1780(3)
_cell_length_c                   19.7854(6)
_cell_measurement_reflns_used    18672
_cell_measurement_temperature    120.00(10)
_cell_measurement_theta_max      29.0290
_cell_measurement_theta_min      3.0370
_cell_volume                     1757.68(10)
_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_environment      N~2~
_diffrn_ambient_temperature      120.00(10)
_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     50.00  96.00   0.50   10.00    --    7.10  77.00-150.00   92
  2  \w     50.00  96.00   0.50   10.00    --    7.10  77.00 -30.00   92
  3  \w     50.00  96.00   0.50   10.00    --    7.10  77.00   0.00   92
  4  \w     50.00  96.00   0.50   10.00    --    7.10  77.00  60.00   92
  5  \w    -63.00  35.00   0.50   10.00    --   -7.50 -82.00  60.00  196
  6  \w    -63.00  35.00   0.50   10.00    --   -7.50 -82.00 -90.00  196
  7  \w    -48.00  81.00   0.50   10.00    --   -7.50  38.00 150.00  258
  8  \w    -63.00   9.00   0.50   10.00    --   -7.50 -82.00-150.00  144
  9  \w    -53.00  29.00   0.50   10.00    --   -7.50 -38.00-120.00  164
 10  \w    -62.00  35.00   0.50   10.00    --   -7.50 -82.00 120.00  194
;
_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      -0.0170308000
_diffrn_orient_matrix_UB_12      -0.0668133000
_diffrn_orient_matrix_UB_13      -0.0159369000
_diffrn_orient_matrix_UB_21      0.0037930000
_diffrn_orient_matrix_UB_22      0.0195717000
_diffrn_orient_matrix_UB_23      -0.0327015000
_diffrn_orient_matrix_UB_31      0.0782175000
_diffrn_orient_matrix_UB_32      -0.0124660000
_diffrn_orient_matrix_UB_33      -0.0004144000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0382
_diffrn_reflns_av_unetI/netI     0.0255
_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       -11
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            34232
_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         4.118
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.026
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80151
_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    1.628
_exptl_crystal_description       block
_exptl_crystal_F_000             898
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.034
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.650
_refine_diff_density_min         -1.109
_refine_diff_density_rms         0.081
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     509
_refine_ls_number_reflns         6186
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0444
_refine_ls_R_factor_gt           0.0407
_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/[\s^2^(Fo^2^)+(0.0593P)^2^+3.4539P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1132
_refine_ls_wR_factor_ref         0.1158
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5680
_reflns_number_total             6186
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01910d2.cif
_cod_data_source_block           3
_cod_database_code               7708402
_shelx_shelxl_version_number     2016/4
_chemical_oxdiff_formula         'C H N O Co Cl'
_reflns_odcompleteness_completeness 99.81
_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
 O00B-H00B
 0.85 with sigma of 0.01
 C00Q-H009
 1.887376 with sigma of 0.02
 Co02-H009
 2.69734 with sigma of 0.02
 C010-H00B
 1.895893 with sigma of 0.02
 Co02-H00B
 2.738534 with sigma of 0.02
3.a Free rotating group:
 O00E(H00J,H00K), O00J(H00L,H00N), O01H(H01W,H01X)
3.b Secondary CH2 refined with riding coordinates:
 C00N(H00A,H00E), C00Q(H00F,H00G), C00X(H00H,H00I), C010(H01A,H01B), C014(H01F,
 H01G), C015(H01H,H01I)
3.c Aromatic/amide H refined with riding coordinates:
 C00M(H00M), C00S(H00S), C00U(H00U), C00W(H00W), C00Y(H00Y), C011(H011),
 C016(H016), C018(H018), C019(H019), C01A(H01J), C01B(H01K), C01D(H01L)
3.d Idealised Me refined as rotating group:
 C012(H01C,H01D,H01E), C01E(H01M,H01N,H01O), C01F(H01P,H01Q,H01R), C01I(H01T,
 H01U,H01V)
3.e Idealised tetrahedral OH refined as rotating group:
 O00C(H00C), O00D(H00D), O01G(H01S)
;
_shelx_res_checksum              4865
_shelx_hkl_checksum              8291
_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 1.268
_oxdiff_exptl_absorpt_empirical_full_min 0.661