Unprecedented metal-metal bonded {Ru<sub>4</sub>(μ<sub>3</sub>-O)<sub>2</sub>} butterfly core in oxido-carboxylato bridged mixed valence cluster-structural elucidation and electronic forms in accessible redox states.
Bera, Sudip Kumar; Lahiri, Goutam Kumar; Dalton transactions (Cambridge, England : 2003) 49 (2020) 13573–13581; doi:10.1039/d0dt02741c

data_7705345
_publ_section_title
;
 Unprecedented metal-metal bonded
 {Ru<sub>4</sub>(\m<sub>3</sub>-O)<sub>2</sub>} butterfly core in
 oxido-carboxylato bridged mixed valence cluster-structural elucidation
 and electronic forms in accessible redox states.
;
_journal_issue                   39
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13573
_journal_page_last               13581
_journal_paper_doi               10.1039/d0dt02741c
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C36 H51 O20 Ru4'
_chemical_formula_sum            'C36 H51 O20 Ru4'
_chemical_formula_weight         1208.04
_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   geom
_audit_creation_date             2019-05-20
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-12-07 deposited with the CCDC.	2020-09-03 downloaded from the CCDC.
;
_cell_angle_alpha                74.4373(18)
_cell_angle_beta                 89.4963(17)
_cell_angle_gamma                80.0332(19)
_cell_formula_units_Z            2
_cell_length_a                   11.8572(3)
_cell_length_b                   13.8306(3)
_cell_length_c                   14.3293(3)
_cell_measurement_reflns_used    16388
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      30.1830
_cell_measurement_theta_min      2.2800
_cell_volume                     2227.82(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_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   -110.00  70.00   0.50    8.00    --  -20.00   0.00-108.00  360
  2  \w    -70.00  19.00   0.50    8.00    --  -20.00 -72.00  36.00  178
  3  \w    -87.00   4.00   0.50    8.00    --  -20.00 -72.00-108.00  182
  4  \w    -44.50   2.00   0.50    8.00    --  -20.00  72.00-180.00   93
  5  \w    -59.00 -28.50   0.50    8.00    --  -20.00  72.00  36.00   61
  6  \w    -22.00   8.00   0.50    8.00    --  -20.00 -72.00 108.00   60
  7  \w   -110.00  70.00   0.50    8.00    --  -20.00   0.00-180.00  360
  8  \w    -67.50   8.00   0.50    8.00    --  -20.00 -72.00 -36.00  151
  9  \w    -81.00   5.00   0.50    8.00    --  -20.00 -72.00-180.00  172
 10  \w    -58.50  -1.50   0.50    8.00    --  -20.00  72.00 108.00  114
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0265494000
_diffrn_orient_matrix_UB_12      0.0278774000
_diffrn_orient_matrix_UB_13      -0.0457247000
_diffrn_orient_matrix_UB_21      -0.0326200000
_diffrn_orient_matrix_UB_22      -0.0388496000
_diffrn_orient_matrix_UB_23      0.0018548000
_diffrn_orient_matrix_UB_31      -0.0438843000
_diffrn_orient_matrix_UB_32      0.0252906000
_diffrn_orient_matrix_UB_33      0.0234580000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0760
_diffrn_reflns_av_unetI/netI     0.0538
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            36439
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        24.998
_diffrn_reflns_theta_max         24.998
_diffrn_reflns_theta_min         2.330
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.405
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.75553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_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    1.801
_exptl_crystal_description       block
_exptl_crystal_F_000             1206
_exptl_crystal_size_max          0.161
_exptl_crystal_size_mid          0.036
_exptl_crystal_size_min          0.033
_refine_diff_density_max         0.741
_refine_diff_density_min         -0.759
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     556
_refine_ls_number_reflns         7823
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0438
_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^)+(0.0405P)^2^+2.6351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0910
_refine_ls_wR_factor_ref         0.0990
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6451
_reflns_number_total             7823
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt02741c2.cif
_cod_data_source_block           1
_cod_depositor_comments          'Adding full bibliography for 7705345.cif.'
_cod_database_code               7705345
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         CHORu
_reflns_odcompleteness_completeness 91.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     31.16
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C13(H13), C18(H18), C28(H28), C3(H3), C23(H23), C8(H8)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C30(H30A,H30B,
 H30C), C1(H1A,H1B,H1C), C15(H15A,H15B,H15C), C10(H10A,H10B,H10C), C32(H32A,
 H32B,H32C), C34(H34A,H34B,H34C), C21(H21A,H21B,H21C), C25(H25A,H25B,H25C),
 C16(H16A,H16B,H16C), C6(H6A,H6B,H6C), C26(H26A,H26B,H26C), C36(H36A,H36B,H36C)
;
_shelx_res_checksum              94035
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.803
_oxdiff_exptl_absorpt_empirical_full_min 0.710