Probing the electronic structure of [Ru(L<sup>1</sup>)<sub>2</sub>]<sup> <i>Z</i> </sup> (<i>z</i> = 0, 1+ and 2+) (H<sub>2</sub>L<sup>1</sup>: a tridentate 2-aminophenol derivative) complexes in three ligand redox levels.
Saha, Anannya; Rajput, Amit; Gupta, Puneet; Mukherjee, Rabindranath; Dalton transactions (Cambridge, England : 2003) 49 (2020) 15355–15375; doi:10.1039/d0dt03074k

data_7705634
_publ_section_title
;
 Probing the electronic structure of [Ru(L<sup>1</sup>)<sub>2</sub>]<sup>
 <i>Z</i> </sup> (<i>z</i> = 0, 1+ and 2+) (H<sub>2</sub>L<sup>1</sup>: a
 tridentate 2-aminophenol derivative) complexes in three ligand redox
 levels.
;
_journal_issue                   43
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              15355
_journal_page_last               15375
_journal_paper_doi               10.1039/d0dt03074k
_journal_volume                  49
_journal_year                    2020
_chemical_formula_moiety         'C54 H62 N2 O2 Ru S2, 2(B F4), O1.7'
_chemical_formula_sum            'C54 H62 B2 F8 N2 O3.7 Ru S2'
_chemical_formula_weight         1137.06
_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             2019-06-27
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-06-27 deposited with the CCDC.	2020-10-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.946(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.1356(3)
_cell_length_b                   21.8710(3)
_cell_length_c                   16.8585(3)
_cell_measurement_reflns_used    23042
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.0910
_cell_measurement_theta_min      2.7900
_cell_volume                     5245.92(17)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_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      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_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    -29.00 108.00   1.00    2.00    --   26.08  38.00 120.00  137
  2  \w      1.00  81.00   1.00    2.00    --   26.08 -99.00-150.00   80
  3  \w    -12.00 102.00   1.00    2.00    --   26.08  57.00 -90.00  114
  4  \w    -12.00 102.00   1.00    2.00    --   26.08  57.00  30.00  114
  5  \w    -13.00 115.00   1.00    2.50    --   67.04 -45.00-180.00  128
  6  \w     12.00 116.00   1.00    2.50    --   67.04-111.00 -30.00  104
  7  \w     30.00 144.00   1.00    2.50    --   67.04  61.00-150.00  114
  8  \w    100.00 152.00   1.00    2.50    --   67.04 111.00-150.00   52
  9  \w    100.00 152.00   1.00    2.50    --   67.04 111.00 120.00   52
 10  \w     30.00 144.00   1.00    2.50    --   67.04  61.00 -30.00  114
 11  \w     19.00 158.00   1.00    2.50    --  108.00 -89.00 -90.00  139
 12  \w    101.00 178.00   1.00    2.50    --  108.00 104.00 150.00   77
 13  \w     69.00 178.00   1.00    2.50    --  108.00  54.00  30.00  109
 14  \w     28.00 158.00   1.00    2.50    --  108.00 -43.00   0.00  130
 15  \w     23.00 151.00   1.00    2.50    --  108.00 -77.00-150.00  128
 16  \w     25.00 178.00   1.00    2.50    --  108.00  21.00   0.00  153
 17  \w     28.00 125.00   1.00    2.50    --  108.00-132.00 124.67   97
 18  \w     21.00 113.00   1.00    2.50    --  108.00-104.00  60.00   92
 19  \w     23.00 151.00   1.00    2.50    --  108.00 -77.00  90.00  128
 20  \w     65.00 178.00   1.00    2.50    --  108.00  77.00 109.94  113
 21  \w     31.00 147.00   1.00    2.50    --  108.00 -54.00-150.00  116
 22  \w     21.00 113.00   1.00    2.50    --  108.00-104.00 150.00   92
 23  \w     21.00 113.00   1.00    2.50    --  108.00-104.00  30.00   92
 24  \w     29.00 145.00   1.00    2.50    --  108.00 -65.00  90.00  116
 25  \w     65.00 178.00   1.00    2.50    --  108.00  77.00  71.31  113
 26  \w     69.00 178.00   1.00    2.50    --  108.00  54.00 -60.00  109
 27  \w    101.00 178.00   1.00    2.50    --  108.00 104.00 120.00   77
 28  \w     86.00 178.00   1.00    2.50    --  108.00 138.00  90.00   92
 29  \w     28.00 123.00   1.00    2.50    --  108.00-129.00 -14.59   95
 30  \w     23.00 151.00   1.00    2.50    --  108.00 -77.00  90.00  128
 31  \w    -50.00  64.00   1.00    2.00    --   26.08 -57.00  90.00  114
 32  \w    -17.00 111.00   1.00    2.00    --   26.08  77.00 150.00  128
 33  \w    -50.00  64.00   1.00    2.00    --   26.08 -57.00 -30.00  114
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0546655000
_diffrn_orient_matrix_UB_12      -0.0082740000
_diffrn_orient_matrix_UB_13      -0.0614409000
_diffrn_orient_matrix_UB_21      -0.0848324000
_diffrn_orient_matrix_UB_22      0.0251081000
_diffrn_orient_matrix_UB_23      -0.0725616000
_diffrn_orient_matrix_UB_31      0.0394796000
_diffrn_orient_matrix_UB_32      0.0652392000
_diffrn_orient_matrix_UB_33      0.0202034000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0585
_diffrn_reflns_av_unetI/netI     0.0366
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            49031
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.236
_diffrn_reflns_theta_max         66.236
_diffrn_reflns_theta_min         3.394
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.803
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.41463
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.440
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2350
_exptl_crystal_size_max          1.00
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         2.341
_refine_diff_density_min         -1.145
_refine_diff_density_rms         0.162
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     679
_refine_ls_number_reflns         9133
_refine_ls_number_restraints     95
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0865
_refine_ls_R_factor_gt           0.0835
_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^)+(0.1404P)^2^+33.2039P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2288
_refine_ls_wR_factor_ref         0.2324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8587
_reflns_number_total             9133
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03074k2.cif
_cod_data_source_block           ruox2lt
_cod_depositor_comments
'Adding full bibliography for 7705632--7705637.cif.'
_cod_original_formula_sum        'C54 H62 B2 F8 N2 O3.70 Ru S2'
_cod_database_code               7705634
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ru C H N O S B F Cl'
_reflns_odcompleteness_completeness 97.68
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C25-C24
 1.38 with sigma of 0.02
 C27-C22
 1.38 with sigma of 0.02
3. Rigid bond restraints
 C25, C24
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C26, C25
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 B2, C22, C27
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
F4 \\sim F3 \\sim F1 \\sim F2 \\sim B1: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
C24 \\sim C25: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
C22 \\sim C27: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(B1) \\sim Ueq, Uanis(F1) \\sim Ueq, Uanis(F3) \\sim Ueq, Uanis(F2) \\sim
Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C25) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C27) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
5. Others
 Fixed Sof: F9(0.5) F6(0.5) O4(0.7)
6.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B), C21(H21A,H21B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C34(H34), C13(H13), C40(H40), C46(H46), C45(H45), C16(H16), C19(H19),
 C50(H50), C43(H43), C18(H18), C51(H51), C17(H17), C44(H44), C54(H54), C52(H52),
  C53(H53), C23(H23), C27(H27), C26(H26), C25(H25), C24(H24)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C5(H5A,H5B,H5C), C4(H4A,H4B,H4C),
 C12(H12A,H12B,H12C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C39(H39A,H39B,
 H39C), C10(H10A,H10B,H10C), C37(H37A,H37B,H37C), C38(H38A,H38B,H38C), C33(H33A,
 H33B,H33C)
;
_shelx_res_checksum              15022
_olex2_date_sample_data_collection 2019-04-09
_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 1.824
_oxdiff_exptl_absorpt_empirical_full_min 0.535