Radical Cations of Phenoxazine and Dihydrophenazine Photoredox Catalysts and Their Role as Deactivators in Organocatalyzed Atom Transfer Radical Polymerization
Corbin, Daniel A.; McCarthy, Blaine G.; van de Lindt, Zach; Miyake, Garret M.; Macromolecules 54 (2021) 4726–4738; doi:10.1021/acs.macromol.1c00640

data_1562359
_publ_section_title
;
 Radical Cations of Phenoxazine and Dihydrophenazine Photoredox Catalysts
 and Their Role as Deactivators in Organocatalyzed Atom Transfer Radical
 Polymerization
;
_journal_issue                   10
_journal_name_full               Macromolecules
_journal_page_first              4726
_journal_page_last               4738
_journal_paper_doi               10.1021/acs.macromol.1c00640
_journal_volume                  54
_journal_year                    2021
_chemical_formula_moiety         'C26 H22 N2 O2, Cl6 Sb, C6 H6'
_chemical_formula_sum            'C32 H28 Cl6 N2 O2 Sb'
_chemical_formula_weight         807.01
_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   geom
_audit_creation_date             2020-09-04
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_cell_angle_alpha                100.421(2)
_cell_angle_beta                 95.385(2)
_cell_angle_gamma                106.067(2)
_cell_formula_units_Z            1
_cell_length_a                   7.9631(3)
_cell_length_b                   10.0144(4)
_cell_length_c                   11.2341(5)
_cell_measurement_reflns_used    9963
_cell_measurement_temperature    100.0
_cell_measurement_theta_max      28.59
_cell_measurement_theta_min      2.54
_cell_volume                     836.80(6)
_computing_cell_refinement       'SAINT V8.40A (Bruker, 2019)'
_computing_data_reduction        'SAINT V8.40A (Bruker, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100.0
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.0870
_diffrn_reflns_av_unetI/netI     0.0429
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            45173
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.575
_diffrn_reflns_theta_min         2.168
_diffrn_source_current           30.0
_diffrn_source_power             1.5
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.336
_exptl_absorpt_correction_T_max  0.7465
_exptl_absorpt_correction_T_min  0.6712
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016) was used for absorption correction.
wR2(int) was 0.0751 before and 0.0669 after correction.
The Ratio of minimum to maximum transmission is 0.8991.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            blue
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_description       rod
_exptl_crystal_F_000             403
_exptl_crystal_size_max          0.137
_exptl_crystal_size_mid          0.096
_exptl_crystal_size_min          0.087
_refine_diff_density_max         0.756
_refine_diff_density_min         -0.443
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     197
_refine_ls_number_reflns         4678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0327
_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^)+(0.0441P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0704
_refine_ls_wR_factor_ref         0.0750
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3953
_reflns_number_total             4678
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ma1c00640_si_002.cif
_cod_data_source_block           gm105_0m_20200904_a
_cod_depositor_comments
'Adding full bibliography for 1562359--1562360.cif.'
_cod_database_code               1562359
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.893
_shelx_estimated_absorpt_t_min   0.838
_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.a Aromatic/amide H refined with riding coordinates:
 C008(H008), C009(H009), C00A(H00A), C00D(H00D), C00E(H00E), C00F(H00F),
 C00H(H00H), C00J(H00J), C00K(H00K), C00L(H00L), C00M(H00M)
2.b Idealised Me refined as rotating group:
 C00I(H00B,H00C,H00G)
;
_shelx_res_checksum              72361
_shelx_hkl_checksum              60475
_olex2_submission_special_instructions 'No special instructions were received'