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_7705635
_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), O'
_chemical_formula_sum            'C54 H62 B2 F8 N2 O3 Ru S2'
_chemical_formula_weight         1125.86
_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   mixed
_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                 110.040(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3134(5)
_cell_length_b                   22.0442(6)
_cell_length_c                   17.0690(5)
_cell_measurement_reflns_used    15731
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      66.2240
_cell_measurement_theta_min      3.3470
_cell_volume                     5413.1(3)
_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      298(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9580
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_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    -12.00 102.00   1.00    2.00    --   26.08  57.00  30.00  114
  2  \w      1.00  81.00   1.00    2.00    --   26.08 -99.00 -30.00   80
  3  \w      1.00  81.00   1.00    2.00    --   26.08 -99.00-120.00   80
  4  \w    -12.00 102.00   1.00    2.00    --   26.08  57.00 -90.00  114
  5  \w     57.00 150.00   1.00    8.00    --   67.04 178.00-180.00   93
  6  \w     30.00 144.00   1.00    8.00    --   67.04  61.00  60.00  114
  7  \w     57.00 150.00   1.00    8.00    --   67.04 178.00  90.00   93
  8  \w     20.00 147.00   1.00    8.00    --   67.04  45.00   0.00  127
  9  \w     20.00 147.00   1.00    8.00    --   67.04  45.00 -90.00  127
 10  \w     28.00 158.00   1.00    8.00    --  108.00 -43.00 120.00  130
 11  \w     23.00 151.00   1.00    8.00    --  108.00 -77.00   0.00  128
 12  \w     19.00 158.00   1.00    8.00    --  108.00 -89.00-120.00  139
 13  \w     29.00 145.00   1.00    8.00    --  108.00 -65.00 120.00  116
 14  \w     24.00 117.00   1.00    8.00    --  108.00-115.00   9.43   93
 15  \w     25.00 136.00   1.00    8.00    --  108.00  21.00 -30.00  111
 16  \w     86.00 178.00   1.00    8.00    --  108.00 138.00-180.00   92
 17  \w     21.00 113.00   1.00    8.00    --  108.00-104.00 120.00   92
 18  \w     25.00 136.00   1.00    8.00    --  108.00  21.00 -30.00  111
 19  \w     27.00  83.00   1.00    8.00    --  108.00 -21.00  60.00   56
 20  \w     72.00 125.00   1.00    8.00    --  108.00  54.00 120.00   53
 21  \w     60.00 108.00   1.00    8.00    --  108.00-104.00 -30.00   48
 22  \w     22.00  49.00   1.00    8.00    --  108.00-104.00 -30.00   27
 23  \w    126.00 152.00   1.00    8.00    --  108.00 138.00 -60.00   26
 24  \w    130.00 156.00   1.00    8.00    --  108.00 138.00-120.00   26
 25  \w     87.00 175.00   1.00    8.00    --  108.00  54.00 -30.00   88
 26  \w     48.00  94.00   1.00    8.00    --  108.00 -54.00  30.00   46
 27  \w     22.00 177.00   1.00    8.00    --  108.00  11.00 120.00  155
 28  \w    153.00 178.00   1.00    8.00    --  108.00  65.00-180.00   25
 29  \w     95.00 121.00   1.00    8.00    --  108.00  65.00  30.00   26
 30  \w     44.00 104.00   1.00    8.00    --  108.00 -94.00  61.89   60
;
_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      0.0494815000
_diffrn_orient_matrix_UB_12      -0.0070576000
_diffrn_orient_matrix_UB_13      -0.0643513000
_diffrn_orient_matrix_UB_21      -0.0883084000
_diffrn_orient_matrix_UB_22      0.0221069000
_diffrn_orient_matrix_UB_23      -0.0694307000
_diffrn_orient_matrix_UB_31      0.0350336000
_diffrn_orient_matrix_UB_32      0.0658828000
_diffrn_orient_matrix_UB_33      0.0163590000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0393
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            37375
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        66.637
_diffrn_reflns_theta_max         66.637
_diffrn_reflns_theta_min         3.351
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.670
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.39346
_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    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2328
_exptl_crystal_size_max          1.0
_exptl_crystal_size_mid          0.8
_exptl_crystal_size_min          0.5
_refine_diff_density_max         1.317
_refine_diff_density_min         -0.809
_refine_diff_density_rms         0.119
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.050
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     652
_refine_ls_number_reflns         9396
_refine_ls_number_restraints     110
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0770
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1372P)^2^+11.2071P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2107
_refine_ls_wR_factor_ref         0.2160
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8606
_reflns_number_total             9396
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03074k2.cif
_cod_data_source_block           ruox2rt
_cod_depositor_comments
'Adding full bibliography for 7705632--7705637.cif.'
_cod_database_code               7705635
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ru C N H O S B F'
_reflns_odcompleteness_completeness 97.11
_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
 C26-C25
 1.4 with sigma of 0.02
 C25-C24
 1.33 with sigma of 0.02
 C24-C23
 1.38 with sigma of 0.02
 F7-B2
 1.44 with sigma of 0.02
 F6-B2
 1.4 with sigma of 0.02
 F5-B2
 1.4 with sigma of 0.02
 F8-B2
 1.5 with sigma of 0.02
 B2-F5
 1.44 with sigma of 0.02
 B2-F6
 1.4 with sigma of 0.02
 F1-B1
 1.4 with sigma of 0.02
 B2-F8
 1.4 with sigma of 0.02
 H21B-C21
 0.99 with sigma of 0.02
 B2-F16
 1.5 with sigma of 0.02
3. Rigid bond restraints
 F8, F5
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
C24 \\sim C25: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
F5 \\sim B2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F7 \\sim B2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
B2 \\sim F6: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
F6 \\sim F5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
B2 \\sim F7: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(B1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C24) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C26) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F4) \\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(F5) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F7) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F6) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(F1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(B2) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(F7) = Uanis(F8) = Uanis(F5) = Uanis(F6)
Uanis(F6) = Uanis(F7) = Uanis(F8) = Uanis(F5) = Uanis(F16)
Uanis(F7) = Uanis(F8) = Uanis(F6) = Uanis(F5) = Uanis(F16)
Uanis(F7) = Uanis(F8) = Uanis(F5) = Uanis(F6) = Uanis(F16)
5. Others
 Fixed Sof: F5(0.5) F6(0.5)
6.a Secondary CH2 refined with riding coordinates:
 C48(H48A,H48B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C40(H40), C34(H34), C16(H16), C46(H46), C19(H19), C43(H43),
 C17(H17), C45(H45), C54(H54), C18(H18), C44(H44), C50(H50), C51(H51), C52(H52),
  C53(H53), C27(H27), C26(H26), C23(H23), C24(H24), C25(H25)
6.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C11(H11A,H11B,H11C), C4(H4A,H4B,H4C), C31(H31A,H31B,H31C),
 C12(H12A,H12B,H12C), C5(H5A,H5B,H5C), C32(H32A,H32B,H32C), C38(H38A,H38B,H38C),
  C10(H10A,H10B,H10C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C33(H33A,H33B,
 H33C)
;
_shelx_res_checksum              8309
_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 3.578
_oxdiff_exptl_absorpt_empirical_full_min 0.524