Immobilising molecular Ru complexes on a protective ultrathin oxide layer of p-Si electrodes towards photoelectrochemical CO<sub>2</sub> reduction.
Laurans, Maxime; Wells, Jordann A. L.; Ott, Sascha; Dalton transactions (Cambridge, England : 2003) 50 (2021) 10482–10492; doi:10.1039/d1dt01331a

data_7707834
_publ_section_title
;
 Immobilising molecular Ru complexes on a protective ultrathin oxide layer
 of p-Si electrodes towards photoelectrochemical CO<sub>2</sub> reduction.
;
_journal_issue                   30
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              10482
_journal_page_last               10492
_journal_paper_doi               10.1039/d1dt01331a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C26 H21 Cl N5 O Ru, H2 O, Cl, O'
_chemical_formula_sum            'C26 H23 Cl2 N5 O3 Ru'
_chemical_formula_weight         625.46
_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
_audit_creation_date             2021-02-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-01 deposited with the CCDC.	2021-07-13 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 96.765(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.770(6)
_cell_length_b                   25.712(16)
_cell_length_c                   11.115(8)
_cell_measurement_reflns_used    3529
_cell_measurement_temperature    170.0
_cell_measurement_theta_max      26.61
_cell_measurement_theta_min      2.43
_cell_volume                     2489(3)
_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 2014/4 (Sheldrick, 2014)'
_diffrn_ambient_temperature      170.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1895
_diffrn_reflns_av_unetI/netI     0.1464
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            23121
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         2.008
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.885
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.4223
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.1647 before and 0.0989 after correction. The Ratio of minimum to maximum transmission is 0.5665. The \l/2 correction factor is 0.00150.'
_exptl_crystal_colour            'dark violet'
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.669
_exptl_crystal_description       needle
_exptl_crystal_F_000             1264
_exptl_crystal_size_max          0.363
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.076
_refine_diff_density_max         1.380
_refine_diff_density_min         -1.568
_refine_diff_density_rms         0.159
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.096
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     354
_refine_ls_number_reflns         4402
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1664
_refine_ls_R_factor_gt           0.0996
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1136P)^2^+14.1973P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2394
_refine_ls_wR_factor_ref         0.2676
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2465
_reflns_number_total             4402
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1dt01331a2.cif
_cod_data_source_block           so20002
_cod_depositor_comments
'Adding full bibliography for 7707833--7707834.cif.'
_cod_database_code               7707834
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.936
_shelx_estimated_absorpt_t_min   0.740
_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, All C(H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 O1S-H1SB = O1S-H1SA
 0.95 with sigma of 0.02
 H1SB-H1SA
 1.5 with sigma of 0.02
 O1-H1
 0.95 with sigma of 0.02
 C17-C26A \\sim C24-C26
 with sigma of 0.02
 C26A-C16 \\sim C26-C25
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C26A \\sim C16 \\sim C25 \\sim C26: within 2A with sigma of 0.04 and sigma for
terminal atoms of 0.08
N3 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15: within 2A with sigma of
0.04 and sigma for terminal atoms of 0.08
Cl0A \\sim Cl0B: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
O2SB \\sim O2SA: within 2A with sigma of 0.04 and sigma for terminal atoms of
0.08
: with sigma of 0.1 and sigma for terminal atoms of 0.2
Uanis(C26A) = Uanis(C26)
4. Rigid body (RIGU) restrains
 C26A, C16, C25, C26
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N3, C11, C12, C13, C14, C15
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 Cl0A, Cl0B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O2SB, O2SA
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: H25(0.2) H16(0.8) C26(0.8) H26A(0.8) H26B(0.8) H26C(0.8) C26A(0.2)
 H26D(0.2) H26E(0.2) H26F(0.2) Cl0A(0.75) Cl0B(0.25) O2SA(0.75) O2SB(0.25)
6.a Aromatic/amide H refined with riding coordinates:
 C7(H7), C3(H3), C13(H13), C14(H14), C12(H12), C9(H9), C2(H2), C24(H24),
 C1(H1A), C4(H4), C25(H25), C22(H22), C16(H16), C15(H15), C17(H17), C19(H19),
 C23(H23), C18(H18)
6.b Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C26A(H26D,H26E,H26F)
6.c Idealised tetrahedral OH refined as rotating group:
 O1(H1)
;
_shelx_res_checksum              49008
_olex2_submission_special_instructions 'No special instructions were received'