Boron-Dipyrromethene-Functionalized Hemilabile Ligands as "Turn-On" Fluorescent Probes for Coordination Changes in Weak-Link Approach Complexes
Alejo M. Lifschitz; Chad M. Shade; Alexander M. Spokoyny; Jose Mendez-Arroyo; Charlotte L. Stern; Amy A. Sarjeant; Chad A. Mirkin; Inorganic Chemistry 52 (2013) 5484–5492; doi:10.1021/ic400383t

data_4334755
_publ_section_title
;
 Boron-Dipyrromethene-Functionalized Hemilabile Ligands as "Turn-On"
 Fluorescent Probes for Coordination Changes in Weak-Link Approach
 Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5484
_journal_page_last               5492
_journal_paper_doi               10.1021/ic400383t
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         'C52 H53 B F6 N2 P2 Pt S2, 2(B F4)'
_chemical_formula_sum            'C52 H53 B3 F14 N2 P2 Pt S2'
_chemical_formula_weight         1325.54
_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   geom
_atom_sites_solution_primary     direct
_audit_creation_date             2012-11-13
_audit_creation_method
;
  Olex2 1.2
  (compiled Nov  5 2012 18:25:38, GUI svn.r4372)
;
_cell_angle_alpha                86.516(2)
_cell_angle_beta                 88.842(2)
_cell_angle_gamma                73.414(2)
_cell_formula_units_Z            4
_cell_length_a                   13.4003(5)
_cell_length_b                   17.1690(6)
_cell_length_c                   25.3152(11)
_cell_measurement_reflns_used    4679
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      67.83
_cell_measurement_theta_min      2.69
_cell_volume                     5571.6(4)
_computing_cell_refinement       'SAINT V7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2.1-4 (Bruker, 2007)'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      99.99
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.970
_diffrn_measured_fraction_theta_max 0.964
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0389
_diffrn_reflns_Laue_measured_fraction_full 0.970
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            19600
_diffrn_reflns_point_group_measured_fraction_full 0.970
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.056
_diffrn_reflns_theta_min         2.690
_diffrn_source                   microsource
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    6.695
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  0.543391
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 TWINABS-2008/4 (Bruker,2010) was used for absorption correction.
 
For component 1:
 wR2(int) was 0.0841 before and 0.0471 after correction.
 The Ratio of minimum to maximum transmission not present.
 The \l/2 correction factor is Not present
 
For component 2:
 wR2(int) was 0.0871 before and 0.0486 after correction.
 The Ratio of minimum to maximum transmission is 0.72.
 The \l/2 correction factor is Not present
;
_exptl_crystal_colour            pink
_exptl_crystal_colour_primary    pink
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_description       plate
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.275
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.099
_refine_diff_density_min         -1.406
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1384
_refine_ls_number_reflns         19600
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0525
_refine_ls_R_factor_gt           0.0443
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+13.2465P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1124
_refine_ls_wR_factor_ref         0.1209
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17037
_reflns_number_total             19600
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400383t_si_002_2.cif
_cod_data_source_block           14
_cod_database_code               4334755
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H53A,H53B} of C53, H60 of C60, {H54A,H54B} of C54, H61 of C61, H63 of C63,
  H58 of C58, H65 of C65, H64 of C64, H57 of C57, H59 of C59, H78 of C78, H77
  of C77, H76 of C76, H75 of C75, H73 of C73, H72 of C72, H71 of C71, H70 of
  C70, H69 of C69, H67 of C67, H66 of C66, {H98A,H98B} of C98, {H10G,H10H} of
  C102, H79 of C79, {H81A,H81B} of C81, {H80A,H80B} of C80, H21 of C21, H20 of
  C20, H19 of C19, H18 of C18, H17 of C17, H15 of C15, H14 of C14, H13 of C13,
  H12 of C12, H11 of C11, H9 of C9, H8 of C8, H7 of C7, H6 of C6, H5 of C5,
  {H50A,H50B} of C50, {H46A,H46B} of C46, {H29A,H29B} of C29, {H28A,H28B} of
  C28, H27 of C27, H26 of C26, H25 of C25, H24 of C24, H23 of C23, {H1A,H1B} of
  C1, {H2A,H2B} of C2
 At 1.5 times of:
  {H55A,H55B,H55C} of C55, {H99A,H99B,H99C} of C99, {H10A,H10B,H10C} of C100,
  {H10D,H10E,H10F} of C101, {H10I,H10J,H10K} of C103, {H97A,H97B,H97C} of C97,
  {H3A,H3B,H3C} of C3, {H52A,H52B,H52C} of C52, {H51A,H51B,H51C} of C51, {H49A,
  H49B,H49C} of C49, {H48A,H48B,H48C} of C48, {H47A,H47B,H47C} of C47, {H45A,
  H45B,H45C} of C45, {H10L,H10M,H10N} of C104
2.a Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C28(H28A,H28B), C29(H29A,H29B), C46(H46A,H46B),
 C50(H50A,H50B), C53(H53A,H53B), C54(H54A,H54B), C80(H80A,H80B), C81(H81A,H81B),
  C98(H98A,H98B), C102(H10G,H10H)
2.b Aromatic/amide H refined with riding coordinates:
 C5(H5), C6(H6), C7(H7), C8(H8), C9(H9), C11(H11), C12(H12), C13(H13),
 C14(H14), C15(H15), C17(H17), C18(H18), C19(H19), C20(H20), C21(H21), C23(H23),
  C24(H24), C25(H25), C26(H26), C27(H27), C57(H57), C58(H58), C59(H59),
 C60(H60), C61(H61), C63(H63), C64(H64), C65(H65), C66(H66), C67(H67), C69(H69),
  C70(H70), C71(H71), C72(H72), C73(H73), C75(H75), C76(H76), C77(H77),
 C78(H78), C79(H79)
2.c Idealised Me refined as rotating group:
 C3(H3A,H3B,H3C), C45(H45A,H45B,H45C), C47(H47A,H47B,H47C), C48(H48A,H48B,
 H48C), C49(H49A,H49B,H49C), C51(H51A,H51B,H51C), C52(H52A,H52B,H52C), C55(H55A,
 H55B,H55C), C97(H97A,H97B,H97C), C99(H99A,H99B,H99C), C100(H10A,H10B,H10C),
 C101(H10D,H10E,H10F), C103(H10I,H10J,H10K), C104(H10L,H10M,H10N)
;
_shelx_estimated_absorpt_t_max   0.878
_shelx_estimated_absorpt_t_min   0.260
_shelx_res_checksum              81095
_shelxl_version_number           2012-6