Carbazole modification of Ruthenium Bipyridine–dicarboxylate Oxygen Evolution Molecular Catalyst
Otsuka, Hiroki; Kobayashi, Atsushi; Yoshida, Masaki; Kato, Masako; Dalton Transactions  (2021) –; doi:10.1039/D1DT02824C

data_7708578
_publ_section_title
;
 Carbazole modification of Ruthenium Bipyridine--dicarboxylate Oxygen
 Evolution Molecular Catalyst
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D1DT02824C
_journal_year                    2021
_chemical_formula_moiety         'C46 H30 N6 O4 Ru, 2(C H2 Cl2)'
_chemical_formula_sum            'C48 H34 Cl4 N6 O4 Ru'
_chemical_formula_weight         1001.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-08-18
_audit_creation_method
;
Olex2 1.3
(compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003)
;
_audit_update_record
;
2021-08-18 deposited with the CCDC.	2021-10-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.8950(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.08230(10)
_cell_length_b                   25.8123(5)
_cell_length_c                   20.3078(3)
_cell_measurement_reflns_used    10045
_cell_measurement_temperature    150
_cell_measurement_theta_max      76.9550
_cell_measurement_theta_min      2.7650
_cell_volume                     4226.88(12)
_computing_cell_refinement       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.45h (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector                 'CCD plate'
_diffrn_detector_type            HyPix
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.961
_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    -75.00 -50.00   0.50    2.71    --  -46.37 123.00-153.00   50
  2  \w    -87.00 -62.00   0.50    6.72    --  -84.50 123.00-153.00   50
  3  \w   -133.00 -23.00   0.50    6.72    --  -84.50 149.00   9.00  220
  4  \w    -72.00  -9.00   0.50    6.72    --  -84.50  19.00  90.00  126
  5  \w   -130.00-105.00   0.50    6.72    --  -84.50-149.00 -36.00   50
  6  \w     36.00  83.00   0.50    2.71    --   46.37-123.00 126.00   94
  7  \w     66.00 103.00   0.50    6.72    --  108.56-123.00 126.00   74
  8  \w     36.00  69.00   0.50    6.72    --  108.56 -37.00  60.00   66
  9  \w     38.00  69.00   0.50    6.72    --  108.56 -37.00   0.00   62
 10  \w     38.00  67.00   0.50    6.72    --  108.56 -37.00 -30.00   58
 11  \w     36.00  62.00   0.50    6.72    --  108.56 -37.00 -90.00   52
 12  \w     36.00  68.00   0.50    6.72    --  108.56 -37.00-120.00   64
 13  \w     41.00  76.00   0.50    6.72    --  108.56 -19.00 -90.00   70
 14  \w     36.00 131.00   0.50    6.72    --  108.56 -77.00 -90.00  190
 15  \w     85.00 129.00   0.50    6.72    --  108.56-149.00 -36.00   88
 16  \w     43.00 132.00   0.50    6.72    --  108.56 -77.00 120.00  178
 17  \w     44.00  69.00   0.50    6.72    --  108.56 -37.00  90.00   50
 18  \w     36.00  61.00   0.50    6.72    --  108.56 -37.00 -60.00   50
 19  \w     35.00  68.00   0.50    6.72    --  108.56 -19.00-120.00   66
 20  \w     23.00 117.00   0.50    2.71    --   46.37  77.00 -90.00  188
 21  \w     79.00 118.00   0.50    2.71    --   46.37 123.00-153.00   78
 22  \w     85.00 111.00   0.50    2.71    --   46.37  57.00-150.00   52
 23  \w    101.00 126.00   0.50    6.72    --  108.56 123.00-153.00   50
 24  \w     62.00  87.00   0.50    2.71    --   46.37 149.00   9.00   50
 25  \w     64.00 122.00   0.50    6.72    --  108.56 149.00   9.00  116
 26  \w     33.00  77.00   0.50    2.71    --   46.37  57.00-150.00   88
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
'XtaLAB Synergy, Single source at home/near, HyPix'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0142257000
_diffrn_orient_matrix_UB_12      -0.0577406000
_diffrn_orient_matrix_UB_13      0.0185403000
_diffrn_orient_matrix_UB_21      -0.0154734000
_diffrn_orient_matrix_UB_22      0.0139091000
_diffrn_orient_matrix_UB_23      0.0731080000
_diffrn_orient_matrix_UB_31      -0.1899570000
_diffrn_orient_matrix_UB_32      -0.0055422000
_diffrn_orient_matrix_UB_33      -0.0097766000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0570
_diffrn_reflns_av_unetI/netI     0.0482
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            32223
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.961
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         77.475
_diffrn_reflns_theta_min         2.773
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.777
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.58140
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.45h (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.574
_exptl_crystal_description       needle
_exptl_crystal_F_000             2032
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH, CH2CL2, Et2O'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.001
_refine_diff_density_max         1.456
_refine_diff_density_min         -1.264
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     568
_refine_ls_number_reflns         8639
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0754
_refine_ls_R_factor_gt           0.0648
_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^)+(0.0930P)^2^+9.1629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1679
_refine_ls_wR_factor_ref         0.1747
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7460
_reflns_number_total             8639
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt02824c2.cif
_cod_data_source_block           Rubda-C2
_cod_database_code               7708578
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'Ru C H N O'
_shelx_estimated_absorpt_t_max   0.994
_shelx_estimated_absorpt_t_min   0.206
_reflns_odcompleteness_completeness 99.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C01N(H01R,H01S), C01R(H01A,H01N)
2.b Aromatic/amide H refined with riding coordinates:
 C00K(H00K), C00M(H00M), C00N(H00N), C00O(H00O), C00P(H00P), C00Q(H00Q),
 C00R(H00R), C00S(H00S), C00T(H00T), C010(H010), C011(H011), C014(H014),
 C016(H016), C017(H017), C019(H019), C01B(H01B), C01C(H01C), C01D(H01D),
 C01E(H01E), C01F(H01F), C01G(H01G), C01H(H01H), C01I(H01I), C01J(H01J),
 C01K(H01K), C01L(H01L), C01M(H01M), C01O(H01O), C01P(H01P), C01Q(H01Q)
;
_shelx_res_checksum              1277
_shelx_hkl_checksum              85159
_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 1.400
_oxdiff_exptl_absorpt_empirical_full_min 0.694