Tuning the Reactivity of Cofacial Porphyrin Prisms for Oxygen Reduction Using Modular Building Blocks
Crawley, Matthew R.; Zhang, Daoyang; Oldacre, Amanda N.; Beavers, Christine M.; Friedman, Alan E.; Cook, Timothy R.; Journal of the American Chemical Society  (2020) –; doi:10.1021/jacs.0c11895

data_4135441
_publ_section_title
;
 Tuning the Reactivity of Cofacial Porphyrin Prisms for Oxygen Reduction
 Using Modular Building Blocks
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_paper_doi               10.1021/jacs.0c11895
_journal_year                    2020
_chemical_formula_moiety         'C36 H36 Cl2 F6 N2 O2 Ru2, 4(C H Cl3)'
_chemical_formula_sum            'C40 H40 Cl14 F6 N2 O2 Ru2'
_chemical_formula_weight         1393.18
_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   difmap
_atom_sites_solution_primary     heavy
_audit_creation_date             2020-04-28
_audit_creation_method
;
Olex2 1.3
(compiled 2020.02.04 svn.rd84adfe8 for OlexSys, GUI svn.r6032)
;
_cell_angle_alpha                67.1523(14)
_cell_angle_beta                 70.2511(15)
_cell_angle_gamma                78.9093(15)
_cell_formula_units_Z            1
_cell_length_a                   9.1940(4)
_cell_length_b                   12.4090(5)
_cell_length_c                   13.3632(6)
_cell_measurement_reflns_used    9846
_cell_measurement_temperature    120
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.89
_cell_volume                     1319.04(10)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      120
_diffrn_detector                 'Bruker AXS CMOS-type PHOTON 100 detector'
_diffrn_detector_area_resol_mean 10.42
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker D8 Venture PHOTON 100'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'Bruker AXS TRIUMPH monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0344
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            26329
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.353
_diffrn_reflns_theta_min         2.857
_diffrn_source                   'Mo sealed tube'
_diffrn_source_current           30.0
_diffrn_source_power             1.35
_diffrn_source_type              'sealed tube'
_diffrn_source_voltage           45.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.340
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6633
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0660 before and 0.0492 after correction. The Ratio of minimum to maximum transmission is 0.8895. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.754
_exptl_crystal_description       prism
_exptl_crystal_F_000             690
_exptl_crystal_recrystallization_method 'Slow evaporation of Chloroform.'
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.358
_refine_diff_density_min         -1.545
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     406
_refine_ls_number_reflns         6559
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0484
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0282P)^2^+3.0234P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0829
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5625
_reflns_number_total             6559
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja0c11895_si_002.cif
_cod_data_source_block           mrc_dz_s4_8_0m
_cod_database_code               4135441
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.845
_shelx_estimated_absorpt_t_min   0.748
_olex2_refinement_description
;
1. Rigid body (RIGU) restrains
 F1A, F1B, F3A, F3B, F2A, F2B, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
2. Others
 Sof(F1B)=Sof(F2B)=Sof(F3B)=1-FVAR(1)
 Sof(F1A)=Sof(F2A)=Sof(F3A)=FVAR(1)
;
_shelx_res_checksum              97119
_shelx_hkl_checksum              30113
_olex2_exptl_crystal_mounting_method 'MiTeGen MicroLoop'
_olex2_submission_special_instructions 'No special instructions were received'