Deactivation of signal amplification by reversible exchange catalysis, progress towards in vivo application.
Mewis, Ryan E.; Fekete, Marianna; Green, Gary G. R.; Whitwood, Adrian C.; Duckett, Simon B.; Chemical communications (Cambridge, England) 51 (2015) 9857–9859; doi:10.1039/c5cc01896j

data_7117283
_publ_section_title
;
 Deactivation of signal amplification by reversible exchange catalysis,
 progress towards in vivo application.
;
_journal_issue                   48
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              9857
_journal_page_last               9859
_journal_paper_doi               10.1039/c5cc01896j
_journal_volume                  51
_journal_year                    2015
_chemical_formula_moiety         'C36 H39 Ir N5, 2(C6 H6), B F4'
_chemical_formula_sum            'C48 H51 B F4 Ir N5'
_chemical_formula_weight         976.94
_chemical_name_systematic
;
 ?
;
_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   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2015-04-02
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_audit_update_record
;
2015-05-08 deposited with the CCDC.
2015-05-13 downloaded from the CCDC.
;
_cell_angle_alpha                95.673(3)
_cell_angle_beta                 95.753(3)
_cell_angle_gamma                98.925(3)
_cell_formula_units_Z            2
_cell_length_a                   10.3919(3)
_cell_length_b                   13.6438(4)
_cell_length_c                   15.4722(6)
_cell_measurement_reflns_used    10303
_cell_measurement_temperature    110.05(10)
_cell_measurement_theta_max      30.2430
_cell_measurement_theta_min      3.6570
_cell_volume                     2141.59(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution
;
Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008;
Palatinus et al., 2012)
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      110.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 16.1450
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.872
_diffrn_measurement_details
;
  1 omega  -39.00   38.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204  -57.0000  -60.0000 77

  2 omega   -8.00   18.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204  -99.0000   60.0000 26

  3 omega   26.00   61.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204  -99.0000   60.0000 35

  4 omega  -18.00   91.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204   19.0000  120.0000 109

  5 omega    2.00   85.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204   57.0000 -180.0000 83

  6 omega   65.00   90.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204   77.0000  -90.0000 25

  7 omega   -8.00   47.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -       20.3204   77.0000  -90.0000 55

  8 omega  -68.00  -43.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9454  119.0000  -98.0000 25

  9 omega  -90.00  -64.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      -20.9454  157.0000   57.0000 26
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0376897000
_diffrn_orient_matrix_UB_12      -0.0042111000
_diffrn_orient_matrix_UB_13      -0.0355467000
_diffrn_orient_matrix_UB_21      -0.0584447000
_diffrn_orient_matrix_UB_22      -0.0150170000
_diffrn_orient_matrix_UB_23      -0.0292050000
_diffrn_orient_matrix_UB_31      -0.0020618000
_diffrn_orient_matrix_UB_32      0.0506371000
_diffrn_orient_matrix_UB_33      -0.0059673000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0346
_diffrn_reflns_av_unetI/netI     0.0596
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.872
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            22046
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.872
_diffrn_reflns_theta_full        25.241
_diffrn_reflns_theta_max         30.366
_diffrn_reflns_theta_min         3.351
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.175
_exptl_absorpt_correction_T_max  0.855
_exptl_absorpt_correction_T_min  0.798
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.34 (release 22-05-2014 CrysAlis171 .NET)
(compiled May 22 2014,16:03:01)
Analytical numeric absorption correction using a multifaceted crystal
            model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.515
_exptl_crystal_description       block
_exptl_crystal_F_000             984
_exptl_crystal_size_max          0.2126
_exptl_crystal_size_mid          0.1703
_exptl_crystal_size_min          0.1364
_refine_diff_density_max         1.436
_refine_diff_density_min         -0.933
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     553
_refine_ls_number_reflns         11269
_refine_ls_number_restraints     54
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0408
_refine_ls_R_factor_gt           0.0331
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0243P)^2^+0.3604P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0663
_refine_ls_wR_factor_ref         0.0713
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10020
_reflns_number_total             11269
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5cc01896j2.cif
_cod_data_source_block           sbd1505
_cod_database_code               7117283
_shelxl_version_number           2013-4
_chemical_oxdiff_formula         'C38 H45 B F4 Ir N6 O'
_chemical_oxdiff_usercomment     'Marianna IrBPY'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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. Uiso/Uaniso restraints and constraints
Uanis(C46A) \\sim Ueq, Uanis(C46) \\sim Ueq, Uanis(C47A) \\sim Ueq, Uanis(C47)
\\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C45A) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
Uanis(F2) \\sim Ueq, Uanis(F4) \\sim Ueq, Uanis(F1) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C43) = Uanis(C43A)
Uanis(C48) = Uanis(C48A)
Uanis(C47) = Uanis(C47A)
Uanis(C46) = Uanis(C46A)
Uanis(C45) = Uanis(C45A)
Uanis(C44) = Uanis(C44A)
3. Others
 Sof(C43A)=Sof(H43A)=Sof(C48A)=Sof(H48A)=Sof(C47A)=Sof(H47A)=Sof(C46A)=
 Sof(H46A)=Sof(C45A)=Sof(H45A)=Sof(C44A)=Sof(H44A)=1-FVAR(1)
 Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=Sof(H45)=Sof(C46)=Sof(H46)=
 Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C6(H6), C8(H8), C15(H15), C17(H17), C22(H22), C23(H23),
 C24(H24), C25(H25), C28(H28), C29(H29), C30(H30), C31(H31), C32(H32), C33(H33),
  C34(H34), C35(H35), C36(H36), C43(H43), C43A(H43A), C48A(H48A), C47A(H47A),
 C46A(H46A), C45A(H45A), C44A(H44A), C44(H44), C45(H45), C46(H46), C47(H47),
 C48(H48), C37(H37), C38(H38), C39(H39), C40(H40), C41(H41), C42(H42)
4.b Fitted hexagon refined as free rotating group:
 C43A(C48A,C47A,C46A,C45A,C44A)
4.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C19(H19A,H19B,
 H19C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C)
;
_olex2_date_sample_data_collection 2015-03-31
_olex2_date_sample_submission    2015-03-18
_olex2_exptl_crystal_mounting_method 'oil on micromount'
_olex2_submission_original_sample_id iRbpy
_olex2_submission_special_instructions 'No special instructions were received'