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_7705636
_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, F6.05 P, C Cl2 O0.3, 0.7(O1)'
_chemical_formula_sum            'C55 H66 Cl2 F5.99 N2 O3 P Ru S2'
_chemical_formula_weight         1183.96
_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                 110.007(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.6743(2)
_cell_length_b                   21.9974(2)
_cell_length_c                   17.5755(2)
_cell_measurement_reflns_used    21815
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      66.0830
_cell_measurement_theta_min      3.2660
_cell_volume                     5694.21(13)
_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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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    -50.00  64.00   1.00    3.00    --   26.33 -57.00-150.00  114
  2  \w    -17.00 111.00   1.00    3.00    --   26.33  77.00 -30.00  128
  3  \w    -50.00  64.00   1.00    3.00    --   26.33 -57.00 -60.00  114
  4  \w     57.00 121.00   1.00    3.00    --   26.33 178.00  30.00   64
  5  \w     57.00 150.00   1.00    6.00    --   67.17 178.00-150.00   93
  6  \w     -9.00 104.00   1.00    6.00    --   67.17 -61.00 -90.00  113
  7  \w     20.00 147.00   1.00    6.00    --   67.17  45.00  30.00  127
  8  \w    -18.00 110.00   1.00    6.00    --   67.17 -77.00 -90.00  128
  9  \w     30.00 144.00   1.00    6.00    --   67.17  61.00  90.00  114
 10  \w     25.00 152.00   1.00    6.00    --   67.17  76.00 138.59  127
 11  \w     86.00 178.00   1.00   12.00    --  108.00 138.00   0.00   92
 12  \w     29.00 145.00   1.00   12.00    --  108.00 -65.00 -90.00  116
 13  \w     21.00 113.00   1.00   12.00    --  108.00-104.00 -30.00   92
 14  \w     31.00 147.00   1.00   12.00    --  108.00 -54.00 -90.00  116
 15  \w     86.00 178.00   1.00   12.00    --  108.00 138.00-120.00   92
 16  \w     71.00 178.00   1.00   12.00    --  108.00  65.00 120.00  107
 17  \w     25.00 178.00   1.00   12.00    --  108.00  21.00 120.00  153
 18  \w     71.00 178.00   1.00   12.00    --  108.00  65.00  30.00  107
 19  \w     25.00 119.00   1.00   12.00    --  108.00-119.00 104.35   94
 20  \w     29.00 145.00   1.00   12.00    --  108.00 -65.00  90.00  116
 21  \w     71.00 178.00   1.00   12.00    --  108.00  65.00 -30.00  107
 22  \w     23.00 151.00   1.00   12.00    --  108.00 -77.00  90.00  128
 23  \w     71.00 178.00   1.00   12.00    --  108.00  61.00  -1.04  107
 24  \w    152.00 178.00   1.00   12.00    --  108.00  11.00 -90.00   26
 25  \w     66.00 113.00   1.00   12.00    --  108.00-104.00 -90.00   47
 26  \w    102.00 147.00   1.00   12.00    --  108.00  11.00 -90.00   45
 27  \w     42.00  68.00   1.00   12.00    --  108.00  11.00 -90.00   26
 28  \w     59.00  99.00   1.00   12.00    --  108.00 -53.00  93.92   40
 29  \w     74.00  99.00   1.00   12.00    --  108.00  61.00  -1.04   25
 30  \w     64.00  90.00   1.00   12.00    --  108.00-104.00-180.00   26
 31  \w     76.00 115.00   1.00   12.00    --  108.00-113.00  76.46   39
 32  \w     31.00  57.00   1.00   12.00    --  108.00 -90.00  92.62   26
;
_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      -0.0593298000
_diffrn_orient_matrix_UB_12      0.0078174000
_diffrn_orient_matrix_UB_13      0.0534345000
_diffrn_orient_matrix_UB_21      -0.0861461000
_diffrn_orient_matrix_UB_22      -0.0044645000
_diffrn_orient_matrix_UB_23      -0.0757005000
_diffrn_orient_matrix_UB_31      -0.0011519000
_diffrn_orient_matrix_UB_32      -0.0694384000
_diffrn_orient_matrix_UB_33      0.0108596000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0220
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            45423
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.177
_diffrn_reflns_theta_max         66.177
_diffrn_reflns_theta_min         3.346
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.568
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66597
_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            purple
_exptl_crystal_density_diffrn    1.381
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2452
_refine_diff_density_max         1.356
_refine_diff_density_min         -0.837
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.018
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     680
_refine_ls_number_reflns         9940
_refine_ls_number_restraints     34
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0672
_refine_ls_R_factor_gt           0.0632
_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^)+(0.1499P)^2^+5.0503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1976
_refine_ls_wR_factor_ref         0.2036
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8943
_reflns_number_total             9940
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt03074k2.cif
_cod_data_source_block           ruox1rep_rt
_cod_depositor_comments
'Adding full bibliography for 7705632--7705637.cif.'
_cod_database_code               7705636
_shelx_shelxl_version_number     2017/1
_chemical_oxdiff_formula         'Ru C H N S P F O'
_reflns_odcompleteness_completeness 97.74
_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
 Cl2-Cl1
 2.5 with sigma of 0.02
 O0AA-O3
 0.99 with sigma of 0.02
 C25-C24
 1.38 with sigma of 0.02
3. Rigid bond restraints
 Cl1, C55
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 Cl2, Cl1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
Cl2 \\sim Cl1: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Cl1 \\sim Cl2: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
C24 \\sim C25: within 1.7A with sigma of 0.04 and sigma for terminal atoms of
0.08
Uanis(Cl1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cl2) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O3) \\sim Ueq, Uanis(O0AA) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5. Others
 Fixed Sof: F5(0.67) O3(0.7) O0AA(0.3)
6.a Secondary CH2 refined with riding coordinates:
 C21(H21A,H21B), C48(H48A,H48B)
6.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C13(H13), C40(H40), C34(H34), C16(H16), C19(H19), C46(H46), C43(H43),
 C50(H50), C17(H17), C45(H45), C44(H44), C18(H18), C51(H51), C54(H54), C27(H27),
  C52(H52), C53(H53), C23(H23), C26(H26), C25(H25), C24(H24)
6.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C11(H11A,H11B,H11C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C32(H32A,H32B,H32C), C31(H31A,H31B,H31C), C33(H33A,H33B,H33C), C12(H12A,H12B,
 H12C), C4(H4A,H4B,H4C), C39(H39A,H39B,H39C), C37(H37A,H37B,H37C), C38(H38A,
 H38B,H38C)
;
_shelx_res_checksum              58113
_olex2_date_sample_data_collection 2019-04-13
_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 1.301
_oxdiff_exptl_absorpt_empirical_full_min 0.748