Electrochemical properties and C-H bond oxidation activity of [Ru(tpy)(pyalk)Cl]<sup>+</sup> and [Ru(tpy)(pyalk)(OH)]<sup/>.
Nilles, Christian K.; Herath, Hashini N. K.; Fanous, Hanna; Ugrinov, Angel; Parent, Alexander R.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 9701–9708; doi:10.1039/c8dt02260g

data_7046920
_publ_section_title
;
 Electrochemical properties and C-H bond oxidation activity of
 [Ru(tpy)(pyalk)Cl]<sup>+</sup> and [Ru(tpy)(pyalk)(OH)]<sup/>.
;
_journal_issue                   29
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9701
_journal_page_last               9708
_journal_paper_doi               10.1039/c8dt02260g
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C23 H21 Cl N4 O Ru, 2(C H2 Cl2), C24 H20 B'
_chemical_formula_sum            'C49 H45 B Cl5 N4 O Ru'
_chemical_formula_weight         995.02
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2016-11-22
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.07 svn.r3352 for OlexSys, GUI svn.r5261)
;
_audit_update_record
;
2018-04-20 deposited with the CCDC.
2018-06-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.560(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.924(2)
_cell_length_b                   14.3725(17)
_cell_length_c                   17.534(2)
_cell_measurement_reflns_used    6716
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      27.46
_cell_measurement_theta_min      2.233
_cell_volume                     4487.4(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      101.12
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0916
_diffrn_reflns_av_unetI/netI     0.0748
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            57560
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.554
_diffrn_reflns_theta_min         1.821
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.690
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/2 (Bruker,2014/2) was used for absorption correction. wR2(int) was 0.0670 before and 0.0608 after correction. The Ratio of minimum to maximum transmission is 0.8899. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'clear dark red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.473
_exptl_crystal_description       block
_exptl_crystal_F_000             2036
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Dichloromethane, Diethyl ether'
_exptl_crystal_size_max          0.296
_exptl_crystal_size_mid          0.179
_exptl_crystal_size_min          0.114
_refine_diff_density_max         0.886
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     590
_refine_ls_number_reflns         10332
_refine_ls_number_restraints     604
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0931
_refine_ls_R_factor_gt           0.0519
_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^)+(0.0261P)^2^+9.3391P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0944
_refine_ls_wR_factor_ref         0.1080
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7188
_reflns_number_total             10332
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt02260g2.cif
_cod_data_source_block           p21c
_cod_depositor_comments          'Adding full bibliography for 7046920.cif.'
_cod_original_cell_volume        4487.2(9)
_cod_database_code               7046920
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid bond restraints
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
4. Others
 Sof(H1SC)=Sof(H1SD)=Sof(Cl2S)=Sof(Cl1S)=1-FVAR(1)
 Sof(Cl4S)=Sof(Cl3S)=Sof(H1SA)=Sof(H1SB)=FVAR(1)
 Sof(H2SC)=Sof(H2SD)=Sof(Cl7S)=Sof(Cl8S)=1-FVAR(2)
 Sof(Cl5S)=Sof(Cl6S)=Sof(H2SA)=Sof(H2SB)=FVAR(2)
5.a Secondary CH2 refined with riding coordinates:
 C2S(H2SA,H2SB), C2S(H2SC,H2SD), C1S(H1SA,H1SB), C1S(H1SC,H1SD)
5.b Aromatic/amide H refined with riding coordinates:
 C12(H12), C17(H17), C40(H40), C30(H30), C23(H23), C20(H20), C7(H7), C16(H16),
 C39(H39), C46(H46), C6(H6), C44(H44), C22(H22), C25(H25), C21(H21), C31(H31),
 C34(H34), C45(H45), C36(H36), C42(H42), C5(H5), C018(H018), C32(H32), C9(H9),
 C15(H15), C37(H37), C33(H33), C10(H10), C43(H43), C8(H8), C11(H11), C38(H38),
 C28(H28), C27(H27), C26(H26)
5.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C2(H2A,H2B,H2C)
;
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'