Re and ^99m^Tc complexes of BodP3 - multi-modality imaging probes
Laura H. Davies; Benjamin B. Kasten; Paul D. Benny; Rory L. Arrowsmith; Haobo Ge'Sofia I. Pascu; Stan W. Botchway; William Clegg; Ross W. Harrington; Lee J. Higham; Chem.Commun. 50 (2014) 15503–; doi:10.1039/C4cc06367H

data_7116059
_publ_section_title
;
 Re and ^99m^Tc complexes of BodP3 - multi-modality imaging probes
;
_journal_name_full               Chem.Commun.
_journal_page_first              15503
_journal_paper_doi               10.1039/C4cc06367H
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C55 H60 B Cl N2 O2 P3 Re'
_chemical_formula_sum            'C55 H60 B Cl N2 O2 P3 Re'
_chemical_formula_weight         1106.42
_chemical_name_systematic
;
?
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 91.786(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.1749(4)
_cell_length_b                   10.0931(4)
_cell_length_c                   33.0892(12)
_cell_measurement_reflns_used    6612
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.52
_cell_measurement_theta_min      2.73
_cell_volume                     2728.9(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.845
_diffrn_measurement_device_type
'Oxford Diffraction Gemini A Ultra diffractometer'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  none
_diffrn_radiation_source         'sealed tube with Enhance optics'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0621
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            17360
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         28.61
_diffrn_reflns_theta_min         2.74
_exptl_absorpt_coefficient_mu    2.403
_exptl_absorpt_correction_T_max  0.795
_exptl_absorpt_correction_T_min  0.432
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.49 (release 20-01-2011 CrysAlis171 .NET)
(compiled Jan 20 2011,15:58:25)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.347
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
;
_refine_diff_density_max         1.495
_refine_diff_density_min         -1.194
_refine_diff_density_rms         0.101
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.014(5)
_refine_ls_extinction_coef       0.00021(18)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         10027
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0392
_refine_ls_R_factor_gt           0.0348
_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^)+(0.0321P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0732
_refine_ls_wR_factor_ref         0.0749
_reflns_number_gt                9293
_reflns_number_total             10027
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c4cc06367h2.cif
_cod_data_source_block           ljh84_6b
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7116059
_computing_special_details
;
TITL ljh84 in P2(1)
CELL 0.71073 8.1749 10.0931 33.0892 90.000 91.786 90.000
ZERR 2.00 0.0004 0.0004 0.0012 0.000 0.004 0.000
LATT -1
SYMM -X, 0.5+Y, -Z
SFAC C H B N O P CL RE
UNIT 110 120 2 4 4 6 2 2

REM red slab
SIZE 0.42 0.20 0.10
TEMP -123

L.S. 12
ACTA 52
BOND $H
FMAP 2
PLAN 10

SADI C15 C16 C15A C16
SADI C8 C15 C8 C15A
SIMU C15 C15A C16
DELU C15 C15A C16

WGHT 0.032100
EXTI 0.000214
FVAR 3.12427 0.90020
RE 8 0.538804 0.689279 0.370363 11.00000 0.01722 0.01801 =
0.01747 0.00051 0.00076 -0.00151
P1 6 0.640562 0.910333 0.377038 11.00000 0.02019 0.01995 =
0.02026 -0.00157 0.00248 -0.00133
P2 6 0.331401 0.805793 0.331289 11.00000 0.01974 0.02147 =
0.01668 0.00164 0.00091 0.00090
P3 6 0.331691 0.522608 0.366160 11.00000 0.02081 0.02009 =
0.01923 0.00140 0.00082 -0.00215
CL 7 0.377011 0.760650 0.430265 11.00000 0.03094 0.03234 =
0.02069 -0.00005 0.00384 -0.00281
N1 4 0.314373 0.773961 0.079724 11.00000 0.04224 0.06992 =
0.02345 0.00055 0.00227 -0.00019
N2 4 0.045972 0.667337 0.096048 11.00000 0.04132 0.05216 =
0.03180 -0.01222 -0.00169 -0.00320
B 3 0.165125 0.696802 0.060013 11.00000 0.05061 0.08228 =
0.02590 -0.01620 0.00154 0.01510
C1 1 0.442697 0.824401 0.061119 11.00000 0.05669 0.07617 =
0.02996 0.00834 0.01034 0.00454
O1 5 0.749252 0.589669 0.302932 11.00000 0.02976 0.03646 =
0.03475 -0.00797 0.00776 -0.00186
C2 1 0.556263 0.880473 0.088991 11.00000 0.04990 0.06879 =
0.03296 0.00451 0.01215 -0.00313
O2 5 0.790176 0.547217 0.426518 11.00000 0.02597 0.04832 =
0.05360 0.01934 -0.01181 0.00020
C3 1 0.494944 0.857635 0.126937 11.00000 0.04637 0.05715 =
0.03606 0.00523 -0.00164 0.00009
C4 1 0.344531 0.792778 0.121252 11.00000 0.04553 0.06023 =
0.01963 0.00693 0.00142 0.00366
C5 1 0.227655 0.751565 0.149003 11.00000 0.04272 0.04757 =
0.01942 0.00051 -0.00052 0.00618
C6 1 0.081787 0.692692 0.137030 11.00000 0.04443 0.04657 =
0.02447 -0.00257 0.00012 0.00421
C7 1 -0.052354 0.647458 0.160181 11.00000 0.03635 0.05265 =
0.03793 -0.00982 0.00527 0.00638
C8 1 -0.165513 0.597139 0.132838 11.00000 0.04268 0.06545 =
0.04877 -0.01069 0.01124 0.00188
C9 1 -0.103421 0.609553 0.094468 11.00000 0.04556 0.08197 =
0.04877 -0.02295 -0.00699 -0.00370
C10 1 0.458040 0.827965 0.015585 11.00000 0.07960 0.12331 =
0.03221 0.00047 0.01566 -0.00859
AFIX 33
H10A 2 0.364542 0.782036 0.002706 11.00000 -1.50000
H10B 2 0.559710 0.783919 0.008222 11.00000 -1.50000
H10C 2 0.459785 0.920244 0.006395 11.00000 -1.50000
AFIX 0
C11 1 0.675794 1.101433 0.075171 11.00000 0.11329 0.08693 =
0.10431 0.01994 0.02375 -0.03238
AFIX 33
H11A 2 0.774559 1.145433 0.065821 11.00000 -1.50000
H11B 2 0.648735 1.136114 0.101807 11.00000 -1.50000
H11C 2 0.584613 1.118379 0.055936 11.00000 -1.50000
AFIX 0
C12 1 0.706346 0.951403 0.078230 11.00000 0.06929 0.09567 =
0.05639 0.01271 0.01399 -0.02459
AFIX 23
H12A 2 0.744321 0.917991 0.052001 11.00000 -1.20000
H12B 2 0.793492 0.933982 0.098996 11.00000 -1.20000
AFIX 0
C13 1 0.580517 0.903825 0.165666 11.00000 0.05778 0.06807 =
0.04091 -0.00098 0.00373 -0.01663
AFIX 33
H13A 2 0.685924 0.943875 0.159376 11.00000 -1.50000
H13B 2 0.598812 0.827962 0.183731 11.00000 -1.50000
H13C 2 0.512196 0.969532 0.178954 11.00000 -1.50000
AFIX 0
C14 1 -0.072017 0.651359 0.204817 11.00000 0.04433 0.05909 =
0.04057 0.00173 0.01112 -0.00319
AFIX 33
H14A 2 -0.177179 0.611552 0.211448 11.00000 -1.50000
H14B 2 -0.068907 0.743543 0.214110 11.00000 -1.50000
H14C 2 0.017113 0.601547 0.218226 11.00000 -1.50000
AFIX 0
PART 1
C15 1 -0.318005 0.393370 0.156633 21.00000 0.10749 0.09118 =
0.19322 -0.03846 0.08089 -0.04406
AFIX 33
H15A 2 -0.427259 0.362206 0.163469 21.00000 -1.50000
H15B 2 -0.244746 0.387814 0.180585 21.00000 -1.50000
H15C 2 -0.275221 0.337927 0.135064 21.00000 -1.50000
AFIX 0
PART 2
C15A 1 -0.322130 0.439600 0.177530 -21.00000 0.11536 0.09956 =
0.12736 -0.00024 0.03257 -0.00361
AFIX 33
H15D 2 -0.432804 0.407776 0.182680 -21.00000 -1.50000
H15E 2 -0.277597 0.485007 0.201630 -21.00000 -1.50000
H15F 2 -0.251906 0.364240 0.171138 -21.00000 -1.50000
AFIX 0
PART 0
C16 1 -0.328375 0.534136 0.142551 11.00000 0.05229 0.10065 =
0.07291 -0.03047 0.01147 -0.02541
PART 1
AFIX 23
H16A 2 -0.380019 0.587583 0.163758 21.00000 -1.20000
H16B 2 -0.400971 0.537896 0.118066 21.00000 -1.20000
AFIX 23
PART 2
H16C 2 -0.407316 0.605457 0.148415 -21.00000 -1.20000
H16D 2 -0.370545 0.486253 0.118281 -21.00000 -1.20000
AFIX 0
PART 0
C17 1 -0.186487 0.562974 0.055318 11.00000 0.06593 0.12976 =
0.05446 -0.02625 -0.00621 -0.02647
AFIX 33
H17A 2 -0.293721 0.525228 0.061080 11.00000 -1.50000
H17B 2 -0.118634 0.495359 0.042761 11.00000 -1.50000
H17C 2 -0.200718 0.638273 0.036843 11.00000 -1.50000
AFIX 0
C18 1 0.263863 0.770858 0.192855 11.00000 0.03470 0.04258 =
0.02167 0.00276 0.00345 0.00203
C19 1 0.213511 0.884543 0.212794 11.00000 0.05469 0.04724 =
0.02468 0.00378 -0.00428 0.01693
AFIX 43
H19 2 0.161904 0.954097 0.197844 11.00000 -1.20000
AFIX 0
C20 1 0.237700 0.897049 0.253788 11.00000 0.04583 0.03047 =
0.02443 0.00158 -0.00054 0.01452
AFIX 43
H20 2 0.197831 0.973251 0.267159 11.00000 -1.20000
AFIX 0
C21 1 0.320266 0.799062 0.276109 11.00000 0.02523 0.02713 =
0.01649 0.00286 0.00057 -0.00494
C22 1 0.376700 0.686663 0.256031 11.00000 0.02470 0.02566 =
0.02142 0.00648 0.00322 0.00042
AFIX 43
H22 2 0.434883 0.619514 0.270562 11.00000 -1.20000
AFIX 0
C23 1 0.346868 0.674378 0.214807 11.00000 0.03054 0.02982 =
0.02393 -0.00107 0.00567 -0.00269
AFIX 43
H23 2 0.384427 0.597673 0.201282 11.00000 -1.20000
AFIX 0
C24 1 0.669213 0.628903 0.327375 11.00000 0.02004 0.01574 =
0.03281 -0.00234 -0.00683 -0.00370
C25 1 0.696519 0.601114 0.406358 11.00000 0.02151 0.01837 =
0.03140 -0.00161 0.00225 -0.00395
C26 1 0.327456 0.422389 0.320539 11.00000 0.02767 0.02014 =
0.02065 0.00311 0.00618 -0.00439
C27 1 0.200848 0.426516 0.291184 11.00000 0.03356 0.02540 =
0.03196 0.00283 0.00315 -0.01045
AFIX 43
H27 2 0.107205 0.479884 0.295419 11.00000 -1.20000
AFIX 0
C28 1 0.211110 0.353203 0.255929 11.00000 0.05853 0.04303 =
0.02679 0.00005 -0.00852 -0.02166
AFIX 43
H28 2 0.124884 0.357722 0.236055 11.00000 -1.20000
AFIX 0
C29 1 0.344319 0.274162 0.249381 11.00000 0.08042 0.03546 =
0.02781 -0.00311 0.00618 -0.01758
AFIX 43
H29 2 0.349623 0.223700 0.225221 11.00000 -1.20000
AFIX 0
C30 1 0.468855 0.268322 0.277632 11.00000 0.06967 0.02585 =
0.04249 -0.00259 0.02391 -0.00532
AFIX 43
H30 2 0.560652 0.212775 0.273505 11.00000 -1.20000
AFIX 0
C31 1 0.460476 0.345573 0.313157 11.00000 0.04247 0.02347 =
0.02862 0.00000 0.00555 -0.01097
AFIX 43
H31 2 0.549484 0.343926 0.332307 11.00000 -1.20000
AFIX 0
C32 1 0.306105 0.399151 0.404994 11.00000 0.02137 0.01851 =
0.01521 -0.00062 0.00460 0.00295
C33 1 0.188092 0.299836 0.399873 11.00000 0.03582 0.03537 =
0.02583 0.00546 -0.00118 -0.01144
AFIX 43
H33 2 0.121571 0.297202 0.375828 11.00000 -1.20000
AFIX 0
C34 1 0.167190 0.204007 0.429998 11.00000 0.03692 0.03508 =
0.03051 0.00512 0.00827 -0.01531
AFIX 43
H34 2 0.086714 0.136702 0.426569 11.00000 -1.20000
AFIX 0
C35 1 0.264747 0.208923 0.464509 11.00000 0.03568 0.02432 =
0.02767 0.00797 0.01053 0.00559
AFIX 43
H35 2 0.251015 0.144329 0.485009 11.00000 -1.20000
AFIX 0
C36 1 0.380824 0.304645 0.469908 11.00000 0.03001 0.03130 =
0.02224 0.00356 -0.00111 0.00401
AFIX 43
H36 2 0.447190 0.306358 0.493987 11.00000 -1.20000
AFIX 0
C37 1 0.401947 0.398982 0.440434 11.00000 0.02800 0.02367 =
0.02707 0.00369 0.00351 -0.00346
AFIX 43
H37 2 0.483530 0.465140 0.444407 11.00000 -1.20000
AFIX 0
C38 1 0.752867 0.987253 0.335718 11.00000 0.02089 0.02745 =
0.02575 0.00578 -0.00170 -0.00447
C39 1 0.740964 0.934271 0.296958 11.00000 0.02967 0.02644 =
0.02431 0.00360 0.00471 -0.00551
AFIX 43
H39 2 0.684936 0.852875 0.292472 11.00000 -1.20000
AFIX 0
C40 1 0.810121 0.999218 0.264863 11.00000 0.03663 0.03250 =
0.02789 0.00317 0.00664 -0.00207
AFIX 43
H40 2 0.799364 0.963072 0.238404 11.00000 -1.20000
AFIX 0
C41 1 0.893588 1.114751 0.270986 11.00000 0.04319 0.06184 =
0.03413 0.02268 0.00131 -0.01758
AFIX 43
H41 2 0.941616 1.158725 0.248912 11.00000 -1.20000
AFIX 0
C42 1 0.908028 1.167667 0.309494 11.00000 0.06543 0.05974 =
0.03869 0.01441 -0.01265 -0.04425
AFIX 43
H42 2 0.966642 1.247917 0.313894 11.00000 -1.20000
AFIX 0
C43 1 0.837109 1.103840 0.341738 11.00000 0.04633 0.03725 =
0.02757 0.00278 -0.00911 -0.01666
AFIX 43
H43 2 0.846849 1.140922 0.368091 11.00000 -1.20000
AFIX 0
C44 1 0.754607 0.957583 0.423083 11.00000 0.02405 0.02008 =
0.01812 0.00057 0.00228 -0.00513
C45 1 0.707586 1.061686 0.447197 11.00000 0.02501 0.03282 =
0.03729 -0.01296 0.00534 -0.00581
AFIX 43
H45 2 0.617820 1.116065 0.438903 11.00000 -1.20000
AFIX 0
C46 1 0.791249 1.087013 0.483530 11.00000 0.03721 0.04619 =
0.03307 -0.01239 0.00610 -0.01280
AFIX 43
H46 2 0.756255 1.156748 0.500498 11.00000 -1.20000
AFIX 0
C47 1 0.924946 1.011212 0.495032 11.00000 0.03197 0.04512 =
0.01995 -0.00220 -0.00174 -0.01752
AFIX 43
H47 2 0.982677 1.028777 0.519815 11.00000 -1.20000
AFIX 0
C48 1 0.974268 0.909974 0.470405 11.00000 0.02936 0.03459 =
0.02963 0.00862 -0.00392 -0.00695
AFIX 43
H48 2 1.067458 0.858383 0.477985 11.00000 -1.20000
AFIX 0
C49 1 0.889310 0.883227 0.434917 11.00000 0.01945 0.02270 =
0.02459 -0.00108 0.00569 -0.00551
AFIX 43
H49 2 0.923773 0.812485 0.418264 11.00000 -1.20000
AFIX 0
C50 1 0.458312 1.018932 0.377066 11.00000 0.02468 0.01805 =
0.02981 -0.00267 -0.00071 0.00024
AFIX 23
H50A 2 0.401249 1.008009 0.402808 11.00000 -1.20000
H50B 2 0.492702 1.112646 0.374897 11.00000 -1.20000
AFIX 0
C51 1 0.341742 0.984094 0.341598 11.00000 0.03683 0.02132 =
0.03042 -0.00234 -0.00545 0.00813
AFIX 23
H51A 2 0.377991 1.030467 0.317079 11.00000 -1.20000
H51B 2 0.230765 1.016594 0.347518 11.00000 -1.20000
AFIX 0
C52 1 0.127568 0.744055 0.345010 11.00000 0.02414 0.04157 =
0.03379 0.00864 0.00311 0.00020
AFIX 23
H52A 2 0.076850 0.809252 0.363135 11.00000 -1.20000
H52B 2 0.057309 0.737573 0.320174 11.00000 -1.20000
AFIX 0
C53 1 0.132032 0.609177 0.365932 11.00000 0.01614 0.04192 =
0.02662 -0.00143 0.00737 -0.00764
AFIX 23
H53A 2 0.049021 0.551352 0.352492 11.00000 -1.20000
H53B 2 0.099792 0.621363 0.394284 11.00000 -1.20000
AFIX 0
C54 1 0.072881 0.790333 0.026226 11.00000 0.07361 0.12545 =
0.03138 0.00444 -0.00853 0.00802
AFIX 33
H54A 2 0.033692 0.871194 0.039159 11.00000 -1.50000
H54B 2 -0.020212 0.742196 0.013972 11.00000 -1.50000
H54C 2 0.149708 0.813841 0.005234 11.00000 -1.50000
AFIX 0
C55 1 0.232037 0.558216 0.042778 11.00000 0.07003 0.08430 =
0.04949 -0.01832 0.01579 -0.00756
AFIX 33
H55A 2 0.276116 0.504402 0.065236 11.00000 -1.50000
H55B 2 0.318585 0.575560 0.023634 11.00000 -1.50000
H55C 2 0.142076 0.510465 0.028989 11.00000 -1.50000

HKLF 4

REM ljh84 in P2(1)
REM R1 = 0.0348 for 9293 Fo > 4sig(Fo) and 0.0392 for all 10027 data
REM 597 parameters refined using 23 restraints

END

;