Stereocontrolled [3 + 2] Annulations with Arene Chromium Tricarbonyl Complexes: Construction of Spirocyclic Compounds Related to Fredericamycin A
Moser, William H.; Zhang, Jian; Lecher, Carl S.; Frazier, Tracy L.; Pink, Maren; Organic Letters 4 (2002) 1981–1984; doi:10.1021/ol025729m

data_5000304
_publ_section_title
;
 Stereocontrolled [3 + 2] Annulations with Arene Chromium Tricarbonyl
 Complexes: Construction of Spirocyclic Compounds Related to Fredericamycin A
;
_journal_coden_ASTM              ORLEF7
_journal_issue                   12
_journal_name_full               'Organic Letters'
_journal_page_first              1981
_journal_page_last               1984
_journal_paper_doi               10.1021/ol025729m
_journal_volume                  4
_journal_year                    2002
_chemical_formula_moiety         'C17 H22 Cr O5 Si'
_chemical_formula_sum            'C17 H22 Cr O5 Si'
_chemical_formula_weight         386.44
_chemical_melting_point          ?
_chemical_name_common            ?
_chemical_name_systematic        ?
_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                98.7610(10)
_cell_angle_beta                 91.0120(10)
_cell_angle_gamma                104.2370(10)
_cell_formula_units_Z            2
_cell_length_a                   6.4814(2)
_cell_length_b                   10.6477(4)
_cell_length_c                   13.9211(5)
_cell_measurement_reflns_used    7913
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      30.03
_cell_measurement_theta_min      2.29
_cell_volume                     918.83(6)
_computing_cell_refinement       'SAINT (Bruker, 1999)'
_computing_data_collection       'SMART (Bruker, 1999)'
_computing_data_reduction        'SAINT (Bruker, 1999)'
_computing_molecular_graphics    'XP, Bruker'
_computing_publication_material  'XCIF (Bruker, 1999), XTEL (local library)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Alatomare et al., 1993)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 44.52
_diffrn_detector_type            'Bruker SMART 6000'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details
'0.30 degree frames measured for 60 seconds each'
_diffrn_measurement_device       'three-circle goniometer with fixed chi'
_diffrn_measurement_device_type  'Bruker Platform goniometer'
_diffrn_measurement_method       \w-scans
_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  0.0339
_diffrn_reflns_av_sigmaI/netI    0.0404
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15407
_diffrn_reflns_theta_full        30.05
_diffrn_reflns_theta_max         30.05
_diffrn_reflns_theta_min         2.29
_diffrn_standards_decay_%        0.0
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  2175
_diffrn_standards_number         1235
_exptl_absorpt_coefficient_mu    0.710
_exptl_absorpt_correction_T_max  0.9790
_exptl_absorpt_correction_T_min  0.8152
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing (1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             404
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.593
_refine_diff_density_min         -0.340
_refine_diff_density_rms         0.070
_refine_ls_extinction_coef       ?
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         5369
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0353
_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^)+(0.0509P)^2^+0.2076P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0877
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                4381
_reflns_number_total             5369
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol025729m_s1.cif
_cod_data_source_block           02041
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'multi-scans' was replaced
with 'multi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               5000304