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_4107380
_publ_section_title
;
 Metal-Mediated Retro Diels-Alder of Dicyclopentadiene Derivatives:
 A Convenient Synthesis of [(Cp-R)M(CO)3] (M = 99mTc, Re) Complexes
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_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            'C12 H8 Cl6 O2'
_chemical_formula_weight         396.88
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                89.5244(15)
_cell_angle_beta                 85.4836(15)
_cell_angle_gamma                77.2782(18)
_cell_formula_units_Z            2
_cell_length_a                   7.9757(2)
_cell_length_b                   8.3191(2)
_cell_length_c                   11.4545(2)
_cell_measurement_reflns_used    26189
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      34.8631
_cell_measurement_theta_min      2.5027
_cell_volume                     739.02(3)
_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
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0283
_diffrn_reflns_av_sigmaI/netI    0.0171
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            45043
_diffrn_reflns_theta_full        33.14
_diffrn_reflns_theta_max         33.14
_diffrn_reflns_theta_min         2.51
_exptl_absorpt_coefficient_mu    1.157
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.79205
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.5 (release 08-05-2007 CrysAlis171 .NET)
(compiled May  8 2007,13:10:02)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            plate
_exptl_crystal_density_diffrn    1.784
_exptl_crystal_description       colorless
_exptl_crystal_F_000             396
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.508
_refine_diff_density_min         -0.454
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         5631
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.131
_refine_ls_R_factor_all          0.0348
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0459P)^2^+0.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0777
_refine_ls_wR_factor_ref         0.0817
_reflns_number_gt                4490
_reflns_number_total             5631
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja077741l-file005.cif
_cod_data_source_block           yl280807
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-09
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_cod_database_code               4107380