Correlating cobalt redox couples to photovoltage in the dye-sensitized solar cell.
Chen, Kitty Y.; Schauer, Phil A.; Patrick, Brian O.; Berlinguette, Curtis P.; Dalton transactions (Cambridge, England : 2003) 47 (2018) 11942–11952; doi:10.1039/c8dt01921e

data_7047057
_publ_section_title
;
 Correlating cobalt redox couples to photovoltage in the dye-sensitized
 solar cell.
;
_journal_issue                   34
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              11942
_journal_page_last               11952
_journal_paper_doi               10.1039/c8dt01921e
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety         'C48 H66 Co N12, 2(F6 P), 2.85(C2 H3 N)'
_chemical_formula_sum            'C53.71 H74.56 Co F12 N14.86 P2'
_chemical_formula_weight         1277.17
_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'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-06-09
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-07-04 deposited with the CCDC.
2018-07-05 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.857(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.9787(11)
_cell_length_b                   21.384(3)
_cell_length_c                   28.322(3)
_cell_measurement_reflns_used    9968
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.34
_cell_measurement_theta_min      2.34
_cell_volume                     6551.0(13)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_collection       'APEX3 V.2017.3 (Bruker AXS, 2017)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_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    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'Bruker-Nonius Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0398
_diffrn_reflns_av_unetI/netI     0.0386
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            52651
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.351
_diffrn_reflns_theta_min         2.040
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.391
_exptl_absorpt_correction_T_max  0.943
_exptl_absorpt_correction_T_min  0.859
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0824 before and 0.0478 after correction. The Ratio of minimum to maximum transmission is 0.9110. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_description       tablet
_exptl_crystal_F_000             2663
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.347
_refine_diff_density_min         -0.456
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.199
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     933
_refine_ls_number_reflns         11914
_refine_ls_number_restraints     557
_refine_ls_restrained_S_all      1.194
_refine_ls_R_factor_all          0.0764
_refine_ls_R_factor_gt           0.0588
_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^)+(0.0064P)^2^+12.7677P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1145
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9487
_reflns_number_total             11914
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01921e2.cif
_cod_data_source_block           cb016
_cod_depositor_comments          'Adding full bibliography for 7047057.cif.'
_cod_original_cell_volume        6551.1(13)
_cod_database_code               7047057
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.944
_shelx_estimated_absorpt_t_min   0.937
_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. Restrained distances
 C37-C37A
 -0.5 with sigma of 0.01
 C37-C14 \\sim C40-C37 \\sim C39-C37 \\sim C38A-C37A \\sim C38-C37 \\sim
C37A-C40A
 with sigma of 0.01
 C38-C39 \\sim C39-C40 \\sim C40-C38 \\sim C38A-C39A \\sim C39A-C40A \\sim
C40A-C38A
 with sigma of 0.01
 P2-F11 \\sim P2-F10 \\sim P2-F8 \\sim P2-F9 \\sim P2-F7 \\sim P2-F12
 with sigma of 0.01
 N13-C49 \\sim N16-C55
 with sigma of 0.01
 C50-C49 \\sim C56-C55
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C54A \\sim N15A \\sim C53A \\sim C54 \\sim N15 \\sim C53 \\sim N14 \\sim C51
\\sim C52 \\sim C51A \\sim N14A \\sim C52A: within 1.7A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C37 \\sim C37A \\sim C38 \\sim C38A \\sim C39 \\sim C39A \\sim C40 \\sim C40A:
within 1.7A with sigma of 0.04 and sigma for terminal atoms of 0.08
C56 \\sim C55 \\sim N16: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
F8 \\sim P2 \\sim F10A \\sim F8A \\sim F12A \\sim F7A \\sim F12 \\sim F10 \\sim
F9 \\sim F11 \\sim F7: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
Uanis(C55) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 C54A, N15A, C53A, C54, N15, C53, N14, C51, C52, C51A, N14A, C52A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C37, C37A, C38, C38A, C39, C39A, C40, C40A
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 C56, C55, N16
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 F8, P2, F10A, F8A, F12A, F7A, F12, F10, F9, F11, F7
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(N14)=Sof(C51)=Sof(C52)=Sof(H52A)=Sof(H52B)=Sof(H52C)=FVAR(1)
 Sof(N15)=Sof(C53)=Sof(C54)=Sof(H54A)=Sof(H54B)=Sof(H54C)=FVAR(2)
 Sof(C37A)=Sof(C38A)=Sof(H38D)=Sof(H38E)=Sof(H38F)=Sof(C39A)=Sof(H39D)=
 Sof(H39E)=Sof(H39F)=Sof(C40A)=Sof(H40D)=Sof(H40E)=Sof(H40F)=1-FVAR(3)
 Sof(C37)=Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(H38C)=Sof(C39)=Sof(H39A)=Sof(H39B)=
 Sof(H39C)=Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(H40C)=FVAR(3)
 Sof(F7A)=Sof(F8A)=Sof(F10A)=Sof(F12A)=1-FVAR(4)
 Sof(F7)=Sof(F8)=Sof(F10)=Sof(F12)=FVAR(4)
 Sof(N14A)=Sof(C51A)=Sof(C52A)=Sof(H52D)=Sof(H52E)=Sof(H52F)=FVAR(5)
 Sof(C55)=Sof(N16)=Sof(C56)=Sof(H56A)=Sof(H56B)=Sof(H56C)=FVAR(6)
 Sof(N15A)=Sof(C53A)=Sof(C54A)=Sof(H54D)=Sof(H54E)=Sof(H54F)=FVAR(7)
 Fixed X: H52A(0.67843) H52B(0.685061) H52C(0.592509)
 Fixed Y: H52A(0.31684) H52B(0.24972) H52C(0.261001)
 Fixed Z: H52A(0.09285) H52B(0.06844) H52C(0.10555)
6.a Free rotating group:
 N14A(C51A,C52A,H52D,H52E,H52F), N15(C53,C54), N15A(C53A,C54A)
6.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8), C9(H9), C10(H10), C15(H15), C16(H16),
 C17(H17), C18(H18), C23(H23), C24(H24)
6.c Idealised Me refined as rotating group:
 C26(H26A,H26B,H26C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C30(H30A,H30B,
 H30C), C31(H31A,H31B,H31C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C35(H35A,
 H35B,H35C), C36(H36A,H36B,H36C), C38(H38A,H38B,H38C), C38A(H38D,H38E,H38F),
 C39(H39A,H39B,H39C), C39A(H39D,H39E,H39F), C40(H40A,H40B,H40C), C40A(H40D,H40E,
 H40F), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C), C46(H46A,
 H46B,H46C), C47(H47A,H47B,H47C), C48(H48A,H48B,H48C), C50(H50A,H50B,H50C),
 C54(H54A,H54B,H54C), C54A(H54D,H54E,H54F), C56(H56A,H56B,H56C)
;
_shelx_res_checksum              99976
_olex2_date_sample_data_collection 2017-08-28
_olex2_date_sample_submission    2017-08-28
_olex2_diffrn_ambient_temperature_device Kryoflex
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a mylar loop in oil'
_olex2_submission_original_sample_id KC-2-088-CODTBppm
_olex2_submission_special_instructions 'No special instructions were received'