Structure-activity relationships in well-defined conjugated oligomer photocatalysts for hydrogen production from water
Aitchison, Catherine M.; Sachs, Michael; Little, Marc; Wilbraham, Liam; Brownbill, Nick J.; Kane, Chris; Blanc, Frédéric; Zwijnenburg, Martijn; Durrant, James; Sprick, Reiner Sebastian; Cooper, Andrew; Chemical Science  (2020) –; doi:10.1039/D0SC02675A

data_1558676
_publ_section_title
;
 Structure-activity relationships in well-defined conjugated oligomer
 photocatalysts for hydrogen production from water
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC02675A
_journal_year                    2020
_chemical_formula_moiety         '2(C30 H26)'
_chemical_formula_sum            'C60 H52'
_chemical_formula_weight         773.01
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-02-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-04-28 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                100.545(5)
_cell_angle_beta                 92.275(4)
_cell_angle_gamma                90.001(5)
_cell_formula_units_Z            1
_cell_length_a                   8.3173(13)
_cell_length_b                   9.6055(17)
_cell_length_c                   13.200(2)
_cell_measurement_reflns_used    1082
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.62
_cell_measurement_theta_min      3.14
_cell_volume                     1035.9(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'CrystalClear-SM Expert 2.0 r7 (Rigaku, 2011)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_detector_type            'Rigaku Saturn724+'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device       'AFC12 (Right): Kappa 3 circle'
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_measurement_specimen_support 'Mitegen 50um'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0868
_diffrn_reflns_av_unetI/netI     0.1043
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            11415
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        23.305
_diffrn_reflns_theta_max         23.305
_diffrn_reflns_theta_min         2.157
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_target            Mo
_diffrn_source_type              'Rotating Anode'
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.070
_exptl_absorpt_correction_T_max  0.7449
_exptl_absorpt_correction_T_min  0.4468
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       block
_exptl_crystal_F_000             412
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.091
_exptl_crystal_size_min          0.037
_refine_diff_density_max         0.183
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     352
_refine_ls_number_reflns         2982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.1297
_refine_ls_R_factor_gt           0.0700
_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^)+(0.0633P)^2^+0.5663P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1705
_refine_ls_wR_factor_ref         0.2008
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1693
_reflns_number_total             2982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02675a3.cif
_cod_data_source_block           ca_mef2_100k
_cod_database_code               1558676
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.981
_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. Others
 Sof(C7)=Sof(C19)=Sof(H19)=Sof(C3AA)=Sof(C4AA)=Sof(H4AA)=Sof(C2AA)=Sof(H2AA)=
 Sof(C12)=Sof(C8)=Sof(C9)=Sof(C6AA)=Sof(H6AA)=Sof(C15)=Sof(C8AA)=Sof(H8AA)=
 Sof(C16)=Sof(H16)=Sof(C6)=Sof(C11)=Sof(C5)=Sof(C7AA)=Sof(H7AA)=Sof(C18)=
 Sof(H18)=Sof(C4)=Sof(H4)=Sof(C10)=Sof(H10)=Sof(C13)=Sof(C17)=Sof(C2)=Sof(C5AA)=
 Sof(H5AA)=Sof(C14)=Sof(H14)=Sof(C1)=Sof(H1)=Sof(C3)=Sof(H3)=Sof(C0AA)=
 Sof(H0AA)=Sof(H0AB)=Sof(H0AC)=Sof(C1AA)=Sof(H1AA)=Sof(H1AB)=Sof(H1AC)=
 Sof(C9AA)=Sof(H9AA)=Sof(H9AB)=Sof(H9AC)=Sof(C0BA)=Sof(H0BA)=Sof(H0BB)=
 Sof(H0BC)=1-FVAR(1)
 Sof(C001)=Sof(H001)=Sof(C002)=Sof(H002)=Sof(C003)=Sof(H003)=Sof(C004)=
 Sof(H004)=Sof(C005)=Sof(C006)=Sof(H00A)=Sof(H00B)=Sof(H00C)=Sof(C007)=
 Sof(H007)=Sof(C008)=Sof(H008)=Sof(C009)=Sof(H009)=Sof(C00A)=Sof(C00B)=
 Sof(C00C)=Sof(H00H)=Sof(C00D)=Sof(C00E)=Sof(H00I)=Sof(H00J)=Sof(H00K)=
 Sof(C00F)=Sof(H00F)=Sof(C00G)=Sof(C00H)=Sof(C00I)=Sof(C00J)=Sof(C00K)=
 Sof(H00L)=Sof(C00L)=Sof(C00M)=Sof(C00N)=Sof(H00N)=Sof(C00O)=Sof(H00O)=
 Sof(C00P)=Sof(H00M)=Sof(H00P)=Sof(H00Q)=Sof(C00Q)=Sof(C00R)=Sof(C00S)=
 Sof(H00S)=Sof(C00T)=Sof(H00T)=Sof(C00U)=Sof(H00D)=Sof(H00E)=Sof(H00G)=FVAR(1)
3.a Aromatic/amide H refined with riding coordinates:
 C001(H001), C002(H002), C003(H003), C004(H004), C007(H007), C008(H008),
 C009(H009), C00C(H00H), C00F(H00F), C00K(H00L), C00N(H00N), C00O(H00O),
 C00S(H00S), C00T(H00T), C19(H19), C4AA(H4AA), C2AA(H2AA), C6AA(H6AA),
 C8AA(H8AA), C16(H16), C7AA(H7AA), C18(H18), C4(H4), C10(H10), C5AA(H5AA),
 C14(H14), C1(H1), C3(H3)
3.b Fitted hexagon refined as free rotating group:
 C7(C19,C3AA,C4AA,C2AA,C12), C9(C6AA,C15,C8AA,C16,C6), C11(C5,C7AA,C18,C4,C10),
  C17(C2,C5AA,C14,C1,C3)
3.c Idealised Me refined as rotating group:
 C006(H00A,H00B,H00C), C00E(H00I,H00J,H00K), C00P(H00M,H00P,H00Q), C00U(H00D,
 H00E,H00G), C0AA(H0AA,H0AB,H0AC), C1AA(H1AA,H1AB,H1AC), C9AA(H9AA,H9AB,H9AC),
 C0BA(H0BA,H0BB,H0BC)
;
_shelx_res_checksum              16081
_olex2_submission_special_instructions 'No special instructions were received'