Lewis Acid/Rhodium-Catalyzed Formal [3 + 3]-Cycloaddition of Enoldiazoacetates with Donor-Acceptor Cyclopropanes.
Cheng, Qing-Qing; Qian, Yu; Zavalij, Peter Y.; Doyle, Michael P.; Organic letters 17 (2015) 3568–3571; doi:10.1021/acs.orglett.5b01674

data_1520728
_publ_section_title
;
 Lewis Acid/Rhodium-Catalyzed Formal [3 + 3]-Cycloaddition of
 Enoldiazoacetates with Donor-Acceptor Cyclopropanes.
;
_journal_issue                   14
_journal_name_full               'Organic letters'
_journal_page_first              3568
_journal_page_last               3571
_journal_paper_doi               10.1021/acs.orglett.5b01674
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C25 H34 N2 O9 Si'
_chemical_formula_sum            'C25 H34 N2 O9 Si'
_chemical_formula_weight         534.63
_chemical_name_common            QY614
_chemical_name_systematic
;
Doyle-Quian QY614
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL-97 & ZCIF'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   10.3059(7)
_cell_length_b                   20.6482(13)
_cell_length_c                   25.5756(17)
_cell_measurement_reflns_used    26365
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.0
_cell_measurement_theta_min      2.3
_cell_volume                     5442.4(6)
_computing_cell_refinement       Apex2
_computing_data_collection       'Apex2 (Bruker, 2010)'
_computing_data_reduction        Apex2
_computing_molecular_graphics    'XSHEL (Bruker, 2004)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD area detector'
_diffrn_detector_area_resol_mean 8.333
_diffrn_detector_type            'Bruker Smart Apex II'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'three-circle diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_measurement_specimen_support 'MiTeGen loop'
_diffrn_orient_matrix_type       standard
_diffrn_orient_matrix_UB_11      0.0961084
_diffrn_orient_matrix_UB_12      0.0066537
_diffrn_orient_matrix_UB_13      -0.0002222
_diffrn_orient_matrix_UB_21      -0.0005304
_diffrn_orient_matrix_UB_22      -0.0000168
_diffrn_orient_matrix_UB_23      -0.0390993
_diffrn_orient_matrix_UB_31      -0.0133438
_diffrn_orient_matrix_UB_32      0.0479716
_diffrn_orient_matrix_UB_33      0.0000232
_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  0.0251
_diffrn_reflns_av_sigmaI/netI    0.0131
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            73823
_diffrn_reflns_theta_full        30.00
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_min         1.97
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    0.140
_exptl_absorpt_correction_T_max  0.950
_exptl_absorpt_correction_T_min  0.915
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.305
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2272
_exptl_crystal_size_max          0.47
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.394
_refine_diff_density_min         -0.290
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     470
_refine_ls_number_reflns         7938
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.000
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.01P)^2^+3.155P], P=(max(Fo^2^,0)+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0666
_reflns_number_gt                6916
_reflns_number_total             7938
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol5b01674_si_002.cif
_cod_data_source_block           2302
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

'_refine_ls_hydrogen_treatment' value 'refAll' changed to 'refall'
according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 

 Adding full bibliography for 1520728.cif.
;
_cod_original_sg_symbol_H-M      Pbca
_cod_database_code               1520728