Rhodium-catalysed alkoxylation/acetalization of diazo compounds: one-step synthesis of highly functionalised quaternary carbon centres
Jola Pospech; Alastair J. J. Lennox; Matthias Beller; Chem.Commun. 51 (2015) 14505–; doi:10.1039/C5cc03903G

data_7117796
_publ_section_title
;
 Rhodium-catalysed alkoxylation/acetalization of diazo compounds: one-step
 synthesis of highly functionalised quaternary carbon centres
;
_journal_name_full               Chem.Commun.
_journal_page_first              14505
_journal_paper_doi               10.1039/C5cc03903G
_journal_volume                  51
_journal_year                    2015
_chemical_formula_sum            'C20 H22 O7'
_chemical_formula_weight         374.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2015-01-13 deposited with the CCDC.
2015-08-11 downloaded from the CCDC.
;
_cell_angle_alpha                90
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_cell_angle_gamma                90
_cell_formula_units_Z            4
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_cell_measurement_reflns_used    9976
_cell_measurement_temperature    150(2)
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_cell_measurement_theta_min      2.87
_cell_volume                     1808.68(9)
_computing_cell_refinement       'SAINT (Bruker, 2013)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
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_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.3333
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0181
_diffrn_reflns_Laue_measured_fraction_full 1.000
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_diffrn_reflns_number            35963
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
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_diffrn_reflns_theta_min         2.136
_diffrn_source                   'fine-focus sealed tube'
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_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.375
_exptl_crystal_description       plate
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_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         4368
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0445
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0494P)^2^+1.2497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
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_cod_data_source_file            c5cc03903g2.cif
_cod_data_source_block           AX0635
_cod_original_cell_volume        1808.67(9)
_cod_database_code               7117796
_shelxl_version_number           2014-3
_shelx_res_checksum              58162