Sterically demanding pyridine-quinoline anchoring ligands as building blocks for copper(I)-based dye-sensitized solar cells (DSSCs) complexes
Peppas, Anastassios; Sokalis, Demetrios; Perganti, Dorothea; Schnakenburg, Gregor; Falaras, Polycarpos; Philippopoulos, athanassios; Dalton Transactions  (2022) –; doi:10.1039/D2DT02382B

data_7711085
_publ_section_title
;
 Sterically demanding pyridine-quinoline anchoring ligands as building
 blocks for copper(I)-based dye-sensitized solar cells (DSSCs) complexes
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02382B
_journal_year                    2022
_chemical_formula_moiety         'C34 H28 Cu N4 O4, C H Cl3, F6 P, 0.13(H2 O)'
_chemical_formula_sum            'C35 H29.29 Cl3 Cu F6 N4 O4.14 P'
_chemical_formula_weight         887.09
_chemical_name_systematic        TP40
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-12-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.21 svn.r3230 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2022-07-07 deposited with the CCDC.	2022-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 118.4701(15)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   31.4899(10)
_cell_length_b                   9.7925(3)
_cell_length_c                   27.9839(10)
_cell_measurement_reflns_used    9855
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.23
_cell_measurement_theta_min      3.49
_cell_volume                     7585.7(4)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'XS (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.01
_diffrn_detector                 'Bruker Photon100 detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8-Venture'
_diffrn_measurement_method       'fine slicing \w and \f scans'
_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  0.1200
_diffrn_reflns_av_unetI/netI     0.0504
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            69447
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         67.747
_diffrn_reflns_theta_min         3.193
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.815
_exptl_absorpt_correction_T_max  0.7536
_exptl_absorpt_correction_T_min  0.3640
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1814 before and 0.1135 after correction.
The Ratio of minimum to maximum transmission is 0.4830.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'clear pink'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.554
_exptl_crystal_description       plate
_exptl_crystal_F_000             3596
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.155
_refine_diff_density_min         -1.652
_refine_diff_density_rms         0.125
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     532
_refine_ls_number_reflns         6873
_refine_ls_number_restraints     102
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1259
_refine_ls_R_factor_gt           0.0964
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1241P)^2^+89.9890P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2427
_refine_ls_wR_factor_ref         0.2710
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5034
_reflns_number_total             6873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02382b1.cif
_cod_data_source_block           cu_6CHCl3013H2O
_cod_database_code               7711085
_shelx_estimated_absorpt_t_max   0.862
_shelx_estimated_absorpt_t_min   0.563
_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, All C(H,H,H,H,H,H) groups, All O(H,H) groups
2. Uiso/Uaniso restraints and constraints
O4 \\sim O4S \\sim C29 \\sim O3 \\sim O3S \\sim C30: within 2A with sigma of
0.005 and sigma for terminal atoms of 0.01
Uanis(O4S) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(O3) \\sim Ueq, Uanis(O3S)
\\sim Ueq, Uanis(C30) \\sim Ueq, Uanis(C29) \\sim Ueq: with sigma of 0.001 and
sigma for terminal atoms of 0.002
Uanis(O5) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
3. Others
 Sof(H30D)=Sof(H30E)=Sof(H30F)=Sof(O4S)=Sof(O3S)=1-FVAR(1)
 Sof(H30A)=Sof(H30B)=Sof(H30C)=Sof(O3)=Sof(O4)=FVAR(1)
 Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(2)
 Sof(Cl3S)=Sof(H35A)=1-FVAR(3)
 Sof(Cl3)=Sof(H35)=FVAR(3)
4.a Free rotating group:
 O5(H5A,H5B)
4.b Ternary CH refined with riding coordinates:
 C35(H35), C35(H35A)
4.c Me refined with riding coordinates:
 C30(H30A,H30B,H30C), C30(H30D,H30E,H30F)
4.d Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C8(H8), C14(H14), C15(H15), C16(H16), C17(H17),
 C19(H19), C20(H20), C21(H21), C25(H25), C31(H31), C32(H32), C33(H33), C34(H34)
4.e Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C23(H23A,H23B,H23C)
;
_shelx_res_checksum              469
_shelx_hkl_checksum              52789
_shelx_shelxl_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'