Redox Switchable Catalysis Utilizing a Fluorescent Dye
Thompson, Brena L.; Simons, Casey R.; Heiden, Zachariah M.; Chemical Communications  (2019) –; doi:10.1039/C9CC05836B

data_7124086
_publ_section_title
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 Redox Switchable Catalysis Utilizing a Fluorescent Dye
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/C9CC05836B
_journal_year                    2019
_chemical_formula_moiety
'C45 H46 B F2 N3 P2 Rh, B F4, C H2 Cl2, C0.5 H2 Cl'
_chemical_formula_sum            'C46.5 H50 B2 Cl3 F6 N3 P2 Rh'
_chemical_formula_weight         1057.72
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_atom_sites_solution_secondary   difmap
_audit_creation_date             2019-06-06
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2019-07-09 deposited with the CCDC.    2019-08-29 downloaded from the CCDC.
;
_cell_angle_alpha                104.8493(16)
_cell_angle_beta                 92.7741(17)
_cell_angle_gamma                90.2091(17)
_cell_formula_units_Z            2
_cell_length_a                   11.0246(6)
_cell_length_b                   11.1262(6)
_cell_length_c                   18.8022(10)
_cell_measurement_reflns_used    9453
_cell_measurement_temperature    107
_cell_measurement_theta_max      26.03
_cell_measurement_theta_min      2.98
_cell_volume                     2226.4(2)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      107
_diffrn_detector_area_resol_mean 10.5
_diffrn_detector_type            'CMOS area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device       'Fixed Chi Three-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0567
_diffrn_reflns_av_unetI/netI     0.0382
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            65374
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         2.98
_diffrn_source                   'fine-focus sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.700
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.7149
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/4 (Bruker,2014/4) was used for absorption correction.
wR2(int) was 0.0555 before and 0.0528 after correction.
The Ratio of minimum to maximum transmission is 0.9591.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.578
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.700
_refine_diff_density_min         -0.629
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     541
_refine_ls_number_reflns         7857
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0377
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+4.0466P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0773
_refine_ls_wR_factor_ref         0.0834
_reflns_number_gt                6382
_reflns_number_total             7857
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c9cc05836b2.cif
_cod_data_source_block           wsu_zh17
_cod_original_formula_sum        'C46.50 H50 B2 Cl3 F6 N3 P2 Rh'
_cod_database_code               7124086
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
2. Others
 Fixed Sof: Cl2A(0.5) Cl2B(0.5) C47(0.5)
3.a Everything fixed:
 C46, H46, H46A, Cl1, Cl2A, Cl2B, Cl3, C47, H47A, H47B
3.b Fixed occupancy and ADP/Uiso:
 H3, H11A, H11B
3.c Ternary CH refined with riding coordinates:
 C38(H38), C39(H39), C42(H42), C43(H43)
3.d Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C12(H12A,H12B), C13(H13A,H13B), C40(H40A,H40B), C41(H41A,
 H41B), C44(H44A,H44B), C45(H45A,H45B)
3.e Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C7(H7), C8(H8), C9(H9), C15(H15), C16(H16), C17(H17),
 C18(H18), C19(H19), C21(H21), C22(H22), C23(H23), C24(H24), C25(H25), C27(H27),
  C28(H28), C29(H29), C30(H30), C31(H31), C33(H33), C34(H34), C35(H35),
 C36(H36), C37(H37)
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_olex2_submission_special_instructions 'No special instructions were received'