Spectroelectrochemical studies of a ruthenium complex containing the pH sensitive 4,4'-dihydroxy-2,2'-bipyridine ligand.
Viere, Erin J.; Kuhn, Ashley E.; Roeder, Margaret H.; Piro, Nicholas A.; Kassel, W. Scott; Dudley, Timothy J.; Paul, Jared J.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4149–4161; doi:10.1039/c7dt04554a

data_7045664
_publ_section_title
;
 Spectroelectrochemical studies of a ruthenium complex containing the pH
 sensitive 4,4'-dihydroxy-2,2'-bipyridine ligand.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4149
_journal_page_last               4161
_journal_paper_doi               10.1039/c7dt04554a
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'Ce N6 O18, C32 H28 N6 O2 Ru'
_chemical_formula_sum            'C32 H28 Ce N12 O20 Ru'
_chemical_formula_weight         1141.85
_space_group_crystal_system      orthorhombic
_space_group_IT_number           52
_space_group_name_Hall           '-P 2a 2bc'
_space_group_name_H-M_alt        'P n n a'
_symmetry_space_group_name_Hall  '-P 2a 2bc'
_symmetry_space_group_name_H-M   'P n n a'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2016-01-21
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2017-11-02 deposited with the CCDC.
2018-02-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0979(9)
_cell_length_b                   19.8019(9)
_cell_length_c                   12.9663(6)
_cell_measurement_reflns_used    9961
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      37.629
_cell_measurement_theta_min      2.368
_cell_volume                     4903.5(4)
_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)'
_diffrn_ambient_temperature      100.
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0418
_diffrn_reflns_av_unetI/netI     0.0123
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            382827
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         37.039
_diffrn_reflns_theta_min         1.877
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.306
_exptl_absorpt_correction_T_max  0.7474
_exptl_absorpt_correction_T_min  0.5484
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0865 before and 0.0549 after correction.
The Ratio of minimum to maximum transmission is 0.7337.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.547
_exptl_crystal_description       block
_exptl_crystal_F_000             2264
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: methanol'
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.326
_refine_diff_density_min         -1.217
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         12513
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0453
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0319P)^2^+7.8163P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0805
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10392
_reflns_number_total             12513
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt04554a2.cif
_cod_data_source_block           paul058
_cod_depositor_comments          'Adding full bibliography for 7045664.cif.'
_cod_database_code               7045664
_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.a Aromatic/amide H refined with riding coordinates:
 C2AA(H2AA), C8(H8), C1AA(H1AA), C0AA(H0AA), C17(H17), C15(H15), C16(H16),
 C14(H14), C11(H11), C9(H9), C10(H10)
2.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C)
;
_shelx_res_checksum              27688
_shelx_shelxl_version_number     2014/7
_olex2_exptl_crystal_mounting_method
'Mounted in NVH imersion oil on a nylon fiber.'
_olex2_submission_special_instructions 'No special instructions were received'