<i>C</i> <sub>2</sub>-Symmetric Ru(II) bimetallic complex catalysed selective degradation and value addition of azo dyes.
Deshmukh, Gopal; Rana, Thakur Rochak Kumar; Yadav, Neha; Rajaraman, Gopalan; Murugavel, Ramaswamy; Dalton transactions (Cambridge, England : 2003) 54 (2025) 15235–15258; doi:10.1039/d5dt01813g

data_7719927
_publ_section_title
;
 <i>C</i> <sub>2</sub>-Symmetric Ru(II) bimetallic complex catalysed
 selective degradation and value addition of azo dyes.
;
_journal_issue                   40
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15235
_journal_page_last               15258
_journal_paper_doi               10.1039/d5dt01813g
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'C66 H74 Cl2 N2 O2 Ru2, [+ solvents]'
_chemical_formula_sum            'C66 H74 Cl2 N2 O2 Ru2'
_chemical_formula_weight         1200.31
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2024-08-30
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2025-03-21 deposited with the CCDC.	2025-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                85.7530(10)
_cell_angle_beta                 72.879(2)
_cell_angle_gamma                83.8210(10)
_cell_formula_units_Z            4
_cell_length_a                   17.0196(3)
_cell_length_b                   19.8132(3)
_cell_length_c                   24.9061(5)
_cell_measurement_reflns_used    35740
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      24.9980
_cell_measurement_theta_min      1.7820
_cell_volume                     7971.9(3)
_computing_cell_refinement       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.93a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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   -100.81  15.19   1.00    7.00    --   -9.84 -59.25-123.92  116
  2  \f    -90.56  38.44   1.00    7.00  81.02  -9.84  31.50    --   129
  3  \w    -65.46  -0.46   1.00    7.00    --  -19.34  94.56   1.16   65
  4  \f   -175.92  16.08   1.00    7.00  15.81  -9.84 -59.25    --   192
  5  \w    -60.88   0.12   1.00    7.00    --  -14.77  94.56 -34.84   61
  6  \w   -100.81  15.19   1.00    7.00    --   -9.84 -59.25 164.08  116
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0358201000
_diffrn_orient_matrix_UB_12      -0.0070531000
_diffrn_orient_matrix_UB_13      0.0092124000
_diffrn_orient_matrix_UB_21      0.0244727000
_diffrn_orient_matrix_UB_22      0.0125316000
_diffrn_orient_matrix_UB_23      -0.0263536000
_diffrn_orient_matrix_UB_31      -0.0059355000
_diffrn_orient_matrix_UB_32      0.0330517000
_diffrn_orient_matrix_UB_33      0.0105072000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0533
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            148349
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.027
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         1.699
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.479
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.35055
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.41.93a (Rigaku Oxford Diffraction, 2020)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'metallic reddish red'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   reddish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.000
_exptl_crystal_description       needle
_exptl_crystal_F_000             2488
_exptl_crystal_size_max          0.484
_exptl_crystal_size_mid          0.419
_exptl_crystal_size_min          0.207
_refine_diff_density_max         1.407
_refine_diff_density_min         -0.917
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1361
_refine_ls_number_reflns         28140
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.060
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0606
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0271P)^2^+37.7772P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1368
_reflns_Friedel_coverage         0.000
_reflns_number_gt                23101
_reflns_number_total             28140
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01813g4.cif
_cod_data_source_block           rm_gd_309
_cod_database_code               7719927
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.907
_shelx_estimated_absorpt_t_min   0.801
_reflns_odcompleteness_completeness 99.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     24.97
_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. Uiso/Uaniso restraints and constraints
Uanis(C36) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C28) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
Uanis(C35) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.001
3.a Ternary CH refined with riding coordinates:
 C25(H25), C29(H29), C31(H31), C34(H34), C55(H55), C64(H64), C120(H120),
 C85(H85), C94(H94), C103(H103), C106(H106), C127(H127)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C4(H4), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C15(H15),
 C17(H17), C20(H20), C24(H24), C37(H37), C40(H40), C41(H41), C43(H43), C44(H44),
  C45(H45), C46(H46), C50(H50), C51(H51), C53(H53), C54(H54), C60(H60),
 C61(H61), C63(H63), C69(H69), C70(H70), C72(H72), C73(H73), C74(H74), C75(H75),
  C77(H77), C80(H80), C81(H81), C83(H83), C84(H84), C90(H90), C92(H92),
 C98(H98), C102(H102), C109(H109), C112(H112), C113(H113), C116(H116),
 C117(H117), C118(H118), C119(H119), C122(H122), C123(H123), C125(H125),
 C126(H126)
3.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C32(H32A,H32B,H32C), C33(H33A,H33B,H33C), C35(H35A,H35B,H35C), C36(H36A,
 H36B,H36C), C48(H48A,H48B,H48C), C56(H56A,H56B,H56C), C57(H57A,H57B,H57C),
 C58(H58A,H58B,H58C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C128(H12A,H12B,
 H12C), C129(H12D,H12E,H12F), C78(H78A,H78B,H78C), C86(H86A,H86B,H86C),
 C87(H87A,H87B,H87C), C95(H95A,H95B,H95C), C96(H96A,H96B,H96C), C104(H10A,H10B,
 H10C), C105(H10D,H10E,H10F), C107(H10G,H10H,H10I), C108(H10J,H10K,H10L),
 C130(H13A,H13B,H13C), C131(H13D,H13E,H13F), C132(H13G,H13H,H13I)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 800 electrons were 
found in a volume of 3037\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 
2.5[CH2Cl2], 4[CH3CH2OH] per Asymmetric Unit 
which account for 836 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              15324
_shelx_hkl_checksum              63514
_shelx_fab_checksum              78463
_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 1.729
_oxdiff_exptl_absorpt_empirical_full_min 0.239