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_4121939
_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            'C13 H12 N O6 Re'
_chemical_formula_weight         464.43
_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                98.310(12)
_cell_angle_beta                 99.288(12)
_cell_angle_gamma                103.772(12)
_cell_formula_units_Z            4
_cell_length_a                   9.9948(11)
_cell_length_b                   11.9574(12)
_cell_length_c                   12.8209(13)
_cell_measurement_reflns_used    7998
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.4
_cell_measurement_theta_min      3.05
_cell_volume                     1441.7(3)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-RED (Stoe, 1999)'
_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_measured_fraction_theta_full 0.926
_diffrn_measured_fraction_theta_max 0.926
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0465
_diffrn_reflns_av_sigmaI/netI    0.0361
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            20348
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         2.95
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  6
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    8.454
_exptl_absorpt_correction_T_max  0.5213
_exptl_absorpt_correction_T_min  0.0915
_exptl_absorpt_correction_type   numerical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.140
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             880
_exptl_crystal_size_max          0.51
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.437
_refine_diff_density_min         -1.691
_refine_diff_density_rms         0.182
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.991
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     380
_refine_ls_number_reflns         6444
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.998
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0362
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1025
_refine_ls_wR_factor_ref         0.1067
_reflns_number_gt                5140
_reflns_number_total             6444
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             4107379
_cod_data_source_file            ja077741l-file004.cif
_cod_data_source_block           yl071206
_cod_depositor_comments
;
 Updated bibliographic information.

 Antanas Vaitkus,
 2019-10-09

 Marked entry as a duplicate of entry 4107379.

 Antanas Vaitkus,
 2019-10-09
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4121939