Development of a Platform for Near-Infrared Photoredox Catalysis
Ravetz, Benjamin D.; Tay, Nicholas E. S.; Joe, Candice L.; Sezen-Edmonds, Melda; Schmidt, Michael A.; Tan, Yichen; Janey, Jacob M.; Eastgate, Martin D.; Rovis, Tomislav; ACS Central Science  (2020) –; doi:10.1021/acscentsci.0c00948

data_4518148
_publ_section_title
;
 Development of a Platform for Near-Infrared Photoredox Catalysis
;
_journal_name_full               'ACS Central Science'
_journal_paper_doi               10.1021/acscentsci.0c00948
_journal_year                    2020
_chemical_formula_moiety         'C42 H28 Br2 N6 Os, 2(F6 P)'
_chemical_formula_sum            'C42 H28 Br2 F12 N6 Os P2'
_chemical_formula_weight         1256.66
_space_group_crystal_system      orthorhombic
_space_group_IT_number           70
_space_group_name_Hall           '-F 2uv 2vw'
_space_group_name_H-M_alt        'F d d d :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-17
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   8.9164(3)
_cell_length_b                   49.9492(16)
_cell_length_c                   25.1934(9)
_cell_measurement_reflns_used    7604
_cell_measurement_temperature    220.00(10)
_cell_measurement_theta_max      26.2100
_cell_measurement_theta_min      3.6280
_cell_volume                     11220.3(7)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      220.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0549
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -41.00  40.00   1.00    4.00    --  -14.69  77.00 -30.00   81
  2  \w      1.00  84.00   1.00    4.00    --   17.19  57.00 120.00   83
  3  \w    -50.00  44.00   1.00    4.00    --   17.19 -77.00  90.00   94
  4  \w     -7.00  85.00   1.00    4.00    --   17.19  77.00-150.00   92
  5  \w      4.00  84.00   1.00    4.00    --   17.19  57.00  30.00   80
  6  \w      0.00  80.00   1.00    4.00    --   17.19  43.00   6.00   80
  7  \w     35.00  60.00   1.00    4.00    --   17.19 178.00   0.00   25
  8  \w    -16.00  49.00   1.00    4.00    --   17.19 -99.00-150.00   65
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0486090000
_diffrn_orient_matrix_UB_12      0.0027212000
_diffrn_orient_matrix_UB_13      0.0216242000
_diffrn_orient_matrix_UB_21      -0.0483878000
_diffrn_orient_matrix_UB_22      -0.0072113000
_diffrn_orient_matrix_UB_23      0.0171734000
_diffrn_orient_matrix_UB_31      0.0403496000
_diffrn_orient_matrix_UB_32      -0.0119242000
_diffrn_orient_matrix_UB_33      -0.0054611000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0724
_diffrn_reflns_av_unetI/netI     0.0430
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.927
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       68
_diffrn_reflns_limit_k_min       -66
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            35949
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.927
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.707
_diffrn_reflns_theta_min         3.357
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.826
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            violet
_exptl_crystal_colour_primary    violet
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_description       block
_exptl_crystal_F_000             4848
_exptl_crystal_size_max          0.207
_exptl_crystal_size_mid          0.141
_exptl_crystal_size_min          0.106
_refine_diff_density_max         0.751
_refine_diff_density_min         -1.618
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.296
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     218
_refine_ls_number_reflns         3712
_refine_ls_number_restraints     147
_refine_ls_restrained_S_all      1.280
_refine_ls_R_factor_all          0.0664
_refine_ls_R_factor_gt           0.0552
_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^)+(0.0001P)^2^+260.7611P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1119
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3227
_reflns_number_total             3712
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            oc0c00948_si_002.cif
_cod_data_source_block           ben9b
_cod_original_sg_symbol_H-M      'F d d d'
_cod_database_code               4518148
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C42 H28 Br2 N6 Os P2 F12'
_reflns_odcompleteness_completeness 99.62
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2. Uiso/Uaniso restraints and constraints
All non-hydrogen atoms have similar U: within 1A with sigma of 0.01 and sigma
for terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 C7, N8
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 P21, F22, F23, F24, F25, F26, F27, P31, F32, F33, F34, F35, F36, F37
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(P31)=Sof(F32)=Sof(F33)=Sof(F34)=Sof(F35)=Sof(F36)=Sof(F37)=0.5*(1-FVAR(2))
 Sof(P21)=Sof(F22)=Sof(F23)=Sof(F24)=Sof(F25)=Sof(F26)=Sof(F27)=0.5*FVAR(2)
5.a :
 P21(F22,F23,F24,F25,F26,F27), P31(F32,F33,F34,F35,F36,F37)
5.b Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C12(H12), C13(H13)
;
_shelx_res_checksum              25333
_shelx_hkl_checksum              74835
_shelx_fab_checksum              18651
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.940
_oxdiff_exptl_absorpt_empirical_full_min 0.666