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_7117211
_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 Ru, 2(Cl), 5(O)'
_chemical_formula_sum            'C60 H42 Cl2 N12 O5 Ru'
_chemical_formula_weight         1183.02
_chemical_name_systematic
'tris[4,4':2',2":4",4'"-quaterpyridine]ruthenium(II) bis(chloride) n hydrate'
_space_group_crystal_system      cubic
_space_group_IT_number           213
_space_group_name_Hall           'P 4bd 2ab 3'
_space_group_name_H-M_alt        'P 41 3 2'
_symmetry_space_group_name_Hall  'P 4bd 2ab 3'
_symmetry_space_group_name_H-M   'P 41 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2015-01-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_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                90
_cell_formula_units_Z            4
_cell_length_a                   21.1118(3)
_cell_length_b                   21.1118(3)
_cell_length_c                   21.1118(3)
_cell_measurement_reflns_used    9803
_cell_measurement_temperature    100
_cell_measurement_theta_max      69.26
_cell_measurement_theta_min      2.96
_cell_volume                     9409.7(2)
_computing_cell_refinement       'SAINT v7.68A (Bruker, 2009)'
_computing_data_collection
;
APEX 2 (2013) Bruker AXS Inc., Madison, WI 53719-1173.
;
_computing_data_reduction        'SAINT v7.68A (Bruker, 2009)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_collimation    'Focusing mirrors'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0978
_diffrn_reflns_av_unetI/netI     0.0251
_diffrn_reflns_laue_measured_fraction_full 0.997
_diffrn_reflns_laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            94438
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.568
_diffrn_reflns_theta_min         3.626
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_target            Ga
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.168
_exptl_absorpt_correction_T_max  0.7534
_exptl_absorpt_correction_T_min  0.6230
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.0900 before and 0.0791 after correction.
The Ratio of minimum to maximum transmission is 0.8269.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    0.835
_exptl_crystal_density_meas      .
_exptl_crystal_description       prism
_exptl_crystal_F_000             2416
_exptl_crystal_preparation       Luminescent
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: water\'ediethyl ether'
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.747
_refine_diff_density_min         -0.512
_refine_diff_density_rms         0.097
_refine_ls_abs_structure_details
;
 Flack x determined using 1021 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.029(8)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         3021
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      1.005
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0634
_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^)+(0.1426P)^2^+2.2050P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1737
_refine_ls_wR_factor_ref         0.1776
_reflns_Friedel_coverage         0.662
_reflns_friedel_fraction_full    1.000
_reflns_friedel_fraction_max     0.993
_reflns_number_gt                2708
_reflns_number_total             3021
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc02124c2.cif
_cod_data_source_block           dane33_0m
_cod_original_cell_volume        9409.7(4)
_cod_database_code               7117211
_shelxl_version_number           2014/6
_publcif_datablock.id            {0cca4185-8c33-485d-a41b-837cd438fcd4}
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
N2 \\sim C6 \\sim C7 \\sim C9 \\sim C10: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Others
 Fixed Sof: Cl2(0.16667) O2(0.5) O1(0.333)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C4(H4), C5(H5), C6(H6), C7(H7), C9(H9), C10(H10)
;
_olex2_submission_special_instructions 'No special instructions were received'
_platon_squeeze_void_probe_radius 1.20