Metal-Mediated Retro Diels-Alder of Dicyclopentadiene Derivatives: A Convenient Synthesis of [(Cp-R)M(CO)3] (M = 99mTc, Re) Complexes
Liu, Yu; Spingler, Bernhard; Schmutz, Paul; Alberto, Roger; Journal of the American Chemical Society 130 (2008) 1554–1555; doi:10.1021/ja077741l

data_4107378
_publ_section_title
;
 Metal-Mediated Retro Diels-Alder of Dicyclopentadiene Derivatives:
 A Convenient Synthesis of [(Cp-R)M(CO)3] (M = 99mTc, Re) Complexes
;
_journal_coden_ASTM              JACSAT
_journal_issue                   5
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1554
_journal_page_last               1555
_journal_paper_doi               10.1021/ja077741l
_journal_volume                  130
_journal_year                    2008
_chemical_formula_sum            'C9 H5 O5 Re'
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_cell_length_c                   9.5610(18)
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_cell_measurement_temperature    183(2)
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_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Xcalibur Ruby'
_diffrn_measurement_method       '/o oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           MoK\a
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_exptl_absorpt_correction_T_min  0.46263
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.8 (release 12-01-2007 CrysAlis171 .NET)
(compiled Jan 12 2007,17:49:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
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_exptl_crystal_description       plate
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_refine_ls_extinction_coef       0.0022(4)
_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   1.071
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_refine_ls_number_parameters     138
_refine_ls_number_reflns         2487
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0191
_refine_ls_R_factor_gt           0.0164
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0228P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0382
_refine_ls_wR_factor_ref         0.0388
_reflns_number_gt                2260
_reflns_number_total             2487
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077741l-file003.cif
_cod_data_source_block           yl310107
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-09
;
_cod_original_cell_volume        489.81(15)
_cod_database_code               4107378