Strategic design of a ruthenium catalyst for both CO2 reduction and H2O oxidation: the electronic influence of the co-ligands
Das, Biswanath; Ezzedinloo, Lida; Bhadbhade, Mohan; Bucknall, Martin; Colbran, Stephen Boyd; Chem. Commun.  (2017) –; doi:10.1039/C7CC06294J

data_7120575
_publ_section_title
;
 Strategic design of a ruthenium catalyst for both CO2 reduction and H2O
 oxidation: the electronic influence of the co-ligands
;
_journal_name_full               'Chem. Commun.'
_journal_paper_doi               10.1039/C7CC06294J
_journal_year                    2017
_chemical_formula_moiety         'C40 H42 N5 O2 Ru, O, F6 P'
_chemical_formula_sum            'C40 H42 F6 N5 O3 P Ru'
_chemical_formula_weight         886.82
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2017-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2017-06-23 deposited with the CCDC.
2017-08-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.407(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.1625(9)
_cell_length_b                   9.8756(5)
_cell_length_c                   20.9277(11)
_cell_measurement_reflns_used    9956
_cell_measurement_temperature    150
_cell_measurement_theta_max      26.847
_cell_measurement_theta_min      2.306
_cell_volume                     3930.3(3)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      149.99
_diffrn_measured_fraction_theta_full 0.998
_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  0.0575
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            50154
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.987
_diffrn_reflns_theta_min         2.905
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.513
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.6734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0964 before and 0.0665 after correction. The Ratio of minimum to maximum transmission is 0.9033. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.499
_exptl_crystal_description       block
_exptl_crystal_F_000             1816
_exptl_crystal_size_max          0.143
_exptl_crystal_size_mid          0.102
_exptl_crystal_size_min          0.081
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.739
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     586
_refine_ls_number_reflns         8549
_refine_ls_number_restraints     248
_refine_ls_restrained_S_all      1.094
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0475
_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^)+(0.0751P)^2^+4.3202P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1315
_refine_ls_wR_factor_ref         0.1399
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7151
_reflns_number_total             8549
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc06294j2.cif
_cod_data_source_block           bishwanath_06srep16_0m_a
_cod_database_code               7120575
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 P1_2-F1_2 \\sim P1_2-F2_2 \\sim P1_2-F3_2 \\sim P1_2-F4_2 \\sim P1_2-F5_2
\\sim P1_2-F6_2
 with sigma of 0.02
 F1_2-F2_2 \\sim F1_2-F4_2 \\sim F1_2-F5_2 \\sim F1_2-F6_2 \\sim F3_2-F2_2
\\sim F3_2-F4_2 \\sim F3_2-
 F5_2 \\sim F3_2-F6_2 \\sim F4_2-F1_2 \\sim F4_2-F3_2 \\sim F2_2-F3_2 \\sim
F2_2-F1_2
 with sigma of 0.04
 F1_2-F3_2 \\sim F2_2-F4_2 \\sim F6_2-F5_2
 with sigma of 0.05
 C6A-C5A \\sim C22A-C20A \\sim C22'-C20A \\sim C21A-C20A \\sim C21'-C20A \\sim
C23A-C20A \\sim C23'-C20A
 with sigma of 0.02
 C18'-C16A \\sim C18A-C16A \\sim C17'-C16A \\sim C17A-C16A \\sim C19'-C16A
\\sim C19A-C16A
 with sigma of 0.02
 H21C-H23A \\sim H21A-H22B
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
P1_2 \\sim F1_2 \\sim F2_2 \\sim F3_2 \\sim F4_2 \\sim F5_2 \\sim F6_2: within
2A with sigma of 0.04 and sigma for terminal atoms of 0.08
Uanis(F5_1) = Uanis(F3_1) = Uanis(F2_1) = Uanis(F6_1) = Uanis(F1_1) =
Uanis(F4_1)
Uanis(F5_2) = Uanis(F1_2) = Uanis(F4_2) = Uanis(F6_2) = Uanis(F3_2) =
Uanis(F2_2)
4. Rigid body (RIGU) restrains
 P1_2, F1_2, F2_2, F3_2, F4_2, F5_2, F6_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1_1, F5_1, F3_1, F4_1, F1_1, F2_1, F6_1
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1_2, F4_2, F3_2, F2_2, F6_2, F1_2, F5_2
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C20A, C21'
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: C19'(0.25) H19A(0.25) H19B(0.25) H19C(0.25) C17'(0.25) H17A(0.25)
 H17B(0.25) H17C(0.25) C21'(0.25) H21A(0.25) H21B(0.25) H21C(0.25) C23'(0.25)
 H23A(0.25) H23B(0.25) H23C(0.25) C18'(0.25) H18A(0.25) H18B(0.25) H18C(0.25)
 C22'(0.25) H22A(0.25) H22B(0.25) H22C(0.25) C17A(0.75) H17D(0.75) H17E(0.75)
 H17F(0.75) C22A(0.75) H22D(0.75) H22E(0.75) H22F(0.75) C21A(0.75) H21D(0.75)
 H21E(0.75) H21F(0.75) C23A(0.75) H23D(0.75) H23E(0.75) H23F(0.75) C19A(0.75)
 H19D(0.75) H19E(0.75) H19F(0.75) C18A(0.75) H18D(0.75) H18E(0.75) H18F(0.75)
 O2W(0.5) O1W(0.5) P1(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5)
 P1(0.5) F1(0.5) F2(0.5) F3(0.5) F4(0.5) F5(0.5) F6(0.5)
6.a Aromatic/amide H refined with riding coordinates:
 C4A(H4A), C12A(H12A), C14A(H14A), C9A(H9A), C7A(H7A), C2A(H2A), C15A(H15A),
 C1A(H1A), C8B(H8B), C5B(H5B), C9B(H9B), C6B(H6B), C3B(H3B), C1B(H1B), C2B(H2B)
6.b Idealised Me refined as rotating group:
 C19'(H19A,H19B,H19C), C17'(H17A,H17B,H17C), C21'(H21A,H21B,H21C), C23'(H23A,
 H23B,H23C), C18'(H18A,H18B,H18C), C22'(H22A,H22B,H22C), C17A(H17D,H17E,H17F),
 C25A(H25A,H25B,H25C), C22A(H22D,H22E,H22F), C21A(H21D,H21E,H21F), C27A(H27A,
 H27B,H27C), C23A(H23D,H23E,H23F), C19A(H19D,H19E,H19F), C26A(H26A,H26B,H26C),
 C18A(H18D,H18E,H18F)
;
_olex2_submission_special_instructions 'No special instructions were received'