First Stepwise Dötz Reaction: Isolation and Characterization of a Chelated Metallatriene Intermediate. Influence of Its Pattern of Substitution in Product Partition
José Barluenga; Fernando Aznar; Ignacio Gutiérrez; Alfredo Martín; Santiago García-Granda; M. Amparo Llorca-Baragaño; Journal of the American Chemical Society 122 (2000) 1314–1324; doi:10.1021/ja991865j

data_4115920
_publ_contact_author
;
      Santiago Garc\'ia-Granda
      Departamento de Qu\'imica F\'isica y Anal\'itica
      Facultad de Qu\'imica
      Universidad de Oviedo
      Avda. Juli\'an Claver\'ia, 8
      33071 Oviedo
      Spain
;
_publ_contact_author_email       sgg@sauron.quimica.uniovi.es
_publ_contact_author_fax         '0034 98 5103125'
_publ_contact_author_phone       '0034 98 5103477'
_publ_section_title
;
 First Stepwise D\"otz Reaction: Isolation and Characterization of a
 Chelated Metallatriene Intermediate. Influence of Its Pattern of
 Substitution in Product Partition
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              1314
_journal_page_last               1324
_journal_paper_doi               10.1021/ja991865j
_journal_volume                  122
_journal_year                    2000
_chemical_compound_source        synthesis
_chemical_formula_moiety         'C20 H17 Cr N O10'
_chemical_formula_sum            'C20 H17 Cr N O10'
_chemical_formula_weight         483.35
_chemical_name_systematic
; 
 Pentacarbonyl[3-dimethylamino-5-(2-furyl)-1,2-dimethoxycarbonyl-2,4-
 pentadien-1-yliden]chromium (0) 
;
_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                103.80(2)
_cell_angle_beta                 100.23(2)
_cell_angle_gamma                105.080(13)
_cell_formula_units_Z            2
_cell_length_a                   9.1582(18)
_cell_length_b                   10.905(2)
_cell_length_c                   14.564(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      17
_cell_measurement_theta_min      15
_cell_volume                     1318.6(6)
_computing_cell_refinement       'CRYSDA (Beurskens et al., 1992)'
_computing_data_collection
;
 CAD-4 Diffractometer Control Software (Enraf-Nonius, 1984)
;
_computing_data_reduction        'REFLEX (local program)'
_computing_molecular_graphics    'EUCLID (Version, 1982)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-90 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Enraf-Nonius CAD-4 diffractometer'
_diffrn_measurement_method       '\w-2\ q scan technique'
_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  0.0185
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_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            4940
_diffrn_reflns_theta_full        24.98
_diffrn_reflns_theta_max         25
_diffrn_reflns_theta_min         1.49
_diffrn_standards_decay_%        5.28
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.590
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      1.217
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             568
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.543
_refine_diff_density_min         -0.520
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.287
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     329
_refine_ls_number_reflns         4622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.287
_refine_ls_R_factor_all          0.0998
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.1102
_refine_ls_wR_factor_ref         0.1226
_reflns_number_gt                2899
_reflns_number_total             4622
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja991865j.cif
_cod_data_source_block           amf211
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0508P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4115920