Tailoring Two-Electron-Donating Phenothiazines To Enable High-Concentration Redox Electrolytes for Use in Nonaqueous Redox Flow Batteries
Attanayake, N. Harsha; Kowalski, Jeffrey A.; Greco, Katharine V.; Casselman, Matthew D.; Milshtein, Jarrod D.; Chapman, Steven J.; Parkin, Sean R.; Brushett, Fikile R.; Odom, Susan A.; Chemistry of Materials 31 (2019) 4353–; doi:10.1021/acs.chemmater.8b04770

data_4003060
_publ_section_title
;
 Tailoring Two-Electron-Donating Phenothiazines To Enable
 High-Concentration Redox Electrolytes for Use in Nonaqueous Redox Flow
 Batteries
;
_journal_issue                   12
_journal_name_full               'Chemistry of Materials'
_journal_page_first              4353
_journal_paper_doi               10.1021/acs.chemmater.8b04770
_journal_volume                  31
_journal_year                    2019
_chemical_formula_moiety         'C24 H33 N O6 S, B F4'
_chemical_formula_sum            'C24 H33 B F4 N O6 S'
_chemical_formula_weight         550.38
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 98.196(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.3654(11)
_cell_length_b                   8.2286(6)
_cell_length_c                   19.8784(16)
_cell_measurement_reflns_used    9813
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      27.55
_cell_measurement_theta_min      2.62
_cell_volume                     2487.7(3)
_computing_cell_refinement       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_collection       '<i>APEX3</i> (Bruker, 2016)'
_computing_data_reduction        '<i>APEX3</i> (Bruker, 2016)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2016/6</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker D8 Venture dual source'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_unetI/netI     0.0239
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            39406
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.577
_diffrn_reflns_theta_min         2.683
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.202
_exptl_absorpt_correction_T_max  1.015
_exptl_absorpt_correction_T_min  0.921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>SADABS</i> (Krause et al., 2015)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.470
_exptl_crystal_description       plate
_exptl_crystal_F_000             1156
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.240
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.410
_refine_diff_density_min         -0.246
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         5731
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0365
_refine_ls_R_factor_gt           0.0332
_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^)+(0.0410P)^2^+1.5447P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0853
_refine_ls_wR_factor_ref         0.0877
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5275
_reflns_number_total             5731
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm8b04770_si_002.cif
_cod_data_source_block           m17029
_cod_database_code               4003060
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.942
_shelx_estimated_absorpt_t_max   0.992
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;
_shelx_res_checksum              54789
_shelx_hkl_checksum              84273