Red-light-driven photocatalytic hydrogen evolution using a ruthenium quaterpyridine complex
E. Rousset; D. Chartrand; I. Ciofini; V. Marvaud; G. S. Hanan; Chem.Commun. 51 (2015) 9261–; doi:10.1039/C5cc02124C

data_7117210
_publ_section_title
;
 Red-light-driven photocatalytic hydrogen evolution using a ruthenium
 quaterpyridine complex
;
_journal_name_full               Chem.Commun.
_journal_page_first              9261
_journal_paper_doi               10.1039/C5cc02124C
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety
'C60 H42 N12 Ru1, 1(C4 H9 O), 2(F6 P), 2(C2 H3 N)'
_chemical_formula_sum            'C67.99 H56.99 F11.99 N14 O P2 Ru'
_chemical_formula_weight         1476.84
_chemical_name_systematic
'tris[4,4':2',2":4",4'"-quaterpyridine]ruthenium(II) bis(hexafluorophosphate) acetonitrile disolvate diethyl ether solvate'
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_update_record
;
2015-02-04 deposited with the CCDC.
2015-04-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   17.6408(12)
_cell_length_b                   17.6408(12)
_cell_length_c                   44.355(3)
_cell_measurement_reflns_used    9774
_cell_measurement_temperature    100
_cell_measurement_theta_max      64.203
_cell_measurement_theta_min      2.601
_cell_volume                     11953.9(14)
_computing_cell_refinement
'SAINT (2013) V8.34A; Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_collection
'APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_data_reduction
'SAINT (2013) V8.34A; Bruker AXS Inc., Madison, WI 53719-1173.'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector                 'CMOS Area detector'
_diffrn_detector_area_resol_mean 10.24
_diffrn_detector_type            'Bruker Photon 100 CMOS Detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'k-geometry diffractometer'
_diffrn_measurement_device_type  'Bruker Venture Metaljet'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'Helios MX Mirror Optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0761
_diffrn_reflns_av_unetI/netI     0.0307
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       53
_diffrn_reflns_limit_l_min       -53
_diffrn_reflns_number            70653
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         53.893
_diffrn_reflns_theta_min         2.600
_diffrn_source                   'Metal Jet'
_diffrn_source_target            Ga
_diffrn_source_type              'Gallium Liquid Metal Jet Source'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.721
_exptl_absorpt_correction_T_max  0.8893
_exptl_absorpt_correction_T_min  0.6936
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.1353 before and 0.0895 after correction.
The Ratio of minimum to maximum transmission is 0.7799.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_description       plate
_exptl_crystal_F_000             4517
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile/diethyl ether'
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.934
_refine_diff_density_min         -1.970
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     446
_refine_ls_number_reflns         4875
_refine_ls_number_restraints     380
_refine_ls_restrained_S_all      1.108
_refine_ls_R_factor_all          0.1188
_refine_ls_R_factor_gt           0.0872
_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^)+(0.1524P)^2^+71.5927P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2204
_refine_ls_wR_factor_ref         0.2673
_reflns_Friedel_coverage         0.000
_reflns_friedel_fraction_full    .
_reflns_friedel_fraction_max     .
_reflns_number_gt                3687
_reflns_number_total             4875
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02124c2.cif
_cod_data_source_block           elod10_0m
_cod_depositor_comments
;
The following automatic conversions were performed:

'_diffrn_radiation_probe' value 'X-ray' changed to 'x-ray' according
to the built-in table from CIF Core dictionary named 'cif_core.dic'
version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 3392 2015-05-12 13:50:21Z andrius 
;
_cod_original_cell_volume        11954.0(19)
_cod_database_code               7117210
_shelx_estimated_absorpt_t_max   0.875
_shelx_estimated_absorpt_t_min   0.782
_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
 N1A-C1A = N1B_$1-C1B_$1
 1 with sigma of 0.02
 C1A-C2A = C1B_$1-C2B_$1
 1.45 with sigma of 0.02
 C2A-N1A = C2B_$1-N1B_$1
 2.45 with sigma of 0.02
 O1E-C1E = O1E-C3E
 1.419 with sigma of 0.05
 O1E-C2E = O1E-C4E
 2.389 with sigma of 0.1
 C2E-C1E = C4E-C3E
 1.518 with sigma of 0.05
 C1E-C3E
 2.374 with sigma of 0.1
 C2E-C4E
 4.768 with sigma of 0.2
 P1-F1 \\sim P1-F2 \\sim P1-F3 \\sim P1-F4 \\sim P1-F5 \\sim P1-F6
 with sigma of 0.01
 F1-F6 \\sim F2-F5 \\sim F3-F4
 with sigma of 0.01
 F1-F2 \\sim F1-F3 \\sim F1-F4 \\sim F1-F5 \\sim F2-F3 \\sim F2-F4 \\sim F2-F6
\\sim F3-F5 \\sim F3-F6 \\sim F4-F5
 \\sim F4-F6 \\sim F5-F6
 with sigma of 0.01
 P1A-F1A \\sim P1A-F2A \\sim P1A-F3A \\sim P1A-F4A \\sim P1A-F5A \\sim P1A-F6A
 with sigma of 0.01
 F1A-F6A \\sim F2A-F5A \\sim F3A-F4A
 with sigma of 0.01
 F1A-F2A \\sim F1A-F3A \\sim F1A-F4A \\sim F1A-F5A \\sim F2A-F3A \\sim F2A-F4A
\\sim F2A-F6A \\sim F3A-F5A
 \\sim F3A-F6A \\sim F4A-F5A \\sim F4A-F6A \\sim F5A-F6A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
N1A \\sim C1A \\sim C2A: within 1.5A with sigma of 0.02 and sigma for terminal
atoms of 0.02
O1E \\sim C1E \\sim C2E \\sim C3E \\sim C4E: within 1.5A with sigma of 0.01 and
sigma for terminal atoms of 0.01
Uanis(N1B) \\sim Ueq, Uanis(C1B) \\sim Ueq, Uanis(C2B) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.03
4. Rigid body (RIGU) restrains
 P1, F1, F2, F3, F4, F5, F6
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P1A, F1A, F2A, F3A, F4A, F5A, F6A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 N1B, C1B, C2B
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, C1E, C2E, C3E, C4E, C4E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1E, C1E, C2E, C3E, C4E
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Fixed Sof: O1E(0.333) C1E(0.333) H1EA(0.333) H1EB(0.333) C2E(0.333)
 H2EA(0.333) H2EB(0.333) H2EC(0.333) C3E(0.333) H3E(0.333) C4E(0.333)
 H4EA(0.333) H4EB(0.333) H4EC(0.333) P1A(0.166) F1A(0.166) F2A(0.166)
 F3A(0.166) F4A(0.166) F5A(0.166) F6A(0.166) P1(0.5) F1(0.5) F2(0.5) F3(0.5)
 F4(0.5) F5(0.5) F6(0.5) N1B(0.5) C1B(0.5) C2B(0.5) H2BA(0.5) H2BB(0.5)
 H2BC(0.5) N1A(0.166) C1A(0.166) C2A(0.166) H2AA(0.166) H2AB(0.166) H2AC(0.166)
6.a Secondary CH2 refined with riding coordinates:
 C1E(H1EA,H1EB)
6.b Me refined with riding coordinates:
 C2E(H2EA,H2EB,H2EC), C4E(H4EA,H4EB,H4EC)
6.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12),
 C14(H14), C17(H17), C18(H18), C19(H19), C20(H20), C3E(H3E)
6.d Idealised Me refined with riding coordinates:
 C2A(H2AA,H2AB,H2AC)
6.e Idealised Me refined as rotating group:
 C2B(H2BA,H2BB,H2BC)
;
_olex2_submission_special_instructions 'No special instructions were received'