Development of tethered dual catalysts: synergy between photo- and transition metal catalysts for enhanced catalysis.
Wang, Danfeng; Malmberg, Robert; Pernik, Indrek; Prasad, Shyamal K. K.; Roemer, Max; Venkatesan, Koushik; Schmidt, Timothy W.; Keaveney, Sinead T.; Messerle, Barbara A.; Chemical science 11 (2020) 6256–6267; doi:10.1039/d0sc02703k

data_1558254
_publ_section_title
;
 Development of tethered dual catalysts: synergy between photo- and
 transition metal catalysts for enhanced catalysis.
;
_journal_issue                   24
_journal_name_full               'Chemical science'
_journal_page_first              6256
_journal_page_last               6267
_journal_paper_doi               10.1039/d0sc02703k
_journal_volume                  11
_journal_year                    2020
_chemical_formula_moiety
'C36 H40 B Cl F2 Ir N6, C24 H20 B, 0.5(C H2 Cl2)'
_chemical_formula_sum            'C60.5 H61 B2 Cl2 F2 Ir N6'
_chemical_formula_weight         1194.87
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2019-07-01
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-09-23 deposited with the CCDC.	2020-06-03 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.255(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.4813(8)
_cell_length_b                   27.5680(13)
_cell_length_c                   12.5577(7)
_cell_measurement_reflns_used    9056
_cell_measurement_temperature    149.62
_cell_measurement_theta_max      26.959
_cell_measurement_theta_min      2.232
_cell_volume                     5530.0(5)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      149.62
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0757
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            76548
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.130
_diffrn_reflns_theta_min         2.232
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.562
_exptl_absorpt_correction_T_max  0.7455
_exptl_absorpt_correction_T_min  0.4930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1336 before and 0.0885 after correction. The Ratio of minimum to maximum transmission is 0.6613. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_description       plate
_exptl_crystal_F_000             2420
_exptl_crystal_size_max          0.338
_exptl_crystal_size_mid          0.267
_exptl_crystal_size_min          0.114
_refine_diff_density_max         2.304
_refine_diff_density_min         -1.168
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     712
_refine_ls_number_reflns         12187
_refine_ls_number_restraints     19
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0356
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0320P)^2^+8.9442P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0830
_refine_ls_wR_factor_ref         0.0899
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10111
_reflns_number_total             12187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc02703k2.cif
_cod_data_source_block           indrek_18dec17_0ma_a
_cod_depositor_comments
;Adding full bibliography for 1558253--1558256.cif.

 Adding full bibliography for 1558253--1558256.cif.
;
_cod_original_formula_sum        'C60.50 H61 B2 Cl2 F2 Ir N6'
_cod_database_code               1558254
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.759
_shelx_estimated_absorpt_t_min   0.478
_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
2. Restrained distances
 Cl0A-C0AA = Cl3-C27 = Cl2-C27 = Cl1A-C0AA
 1.77 with sigma of 0.02
 Cl1A-Cl0A = Cl3-Cl2
 2.92 with sigma of 0.02
 Cl1A-C0AA \\sim Cl0A-C0AA
 with sigma of 0.02
 Cl2-C27 \\sim Cl3-C27
 with sigma of 0.02
 Cl1A-Cl0A \\sim Cl2-Cl3
 with sigma of 0.02
 Cl0A-C0AA \\sim Cl3-C27 \\sim Cl2-C27 \\sim Cl1A-C0AA
 with sigma of 0.02
3. Rigid bond restraints
 C0AA, Cl0A, Cl1A, Cl2, C27, Cl3
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Others
 Fixed Sof: Cl0A(0.25) Cl1A(0.25) C0AA(0.25) H0AA(0.25) H0AB(0.25) Cl2(0.25)
 Cl3(0.25) C27(0.25) H27B(0.25) H27A(0.25)
5.a Secondary CH2 refined with riding coordinates:
 C23(H23A,H23B), C0AA(H0AA,H0AB), C27(H27B,H27A)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C8(H8), C15(H15), C16(H16), C18(H18), C19(H19), C20(H20), C22(H22),
 C24(H24), C25(H25), C26(H26), C2A(H2A), C3A(H3A), C4A(H4A), C5A(H5A), C6A(H6A),
  C8A(H8A), C9A(H9A), C10A(H10G), C11A(H11D), C12A(H12D), C14A(H14A),
 C15A(H15A), C16A(H16A), C17A(H17A), C18A(H18A), C20A(H20A), C21A(H21A),
 C22A(H22A), C23A(H23C), C24A(H24A)
5.c Idealised Me refined as rotating group:
 C6CP(H6CA,H6CB,H6CC), C7CP(H7CA,H7CB,H7CC), C8CP(H8CA,H8CB,H8CC), C9CP(H9CA,
 H9CB,H9CC), C10(H10A,H10B,H10C), C10C(H10D,H10E,H10F), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C), C13(H13A,H13B,H13C)
;
_shelx_res_checksum              62800
_olex2_submission_special_instructions 'No special instructions were received'