A bidirectional synthesis of spiroacetals via Rh(ii)-catalysed C-H insertion.
Lepage, Romain J.; White, Jonathan M.; Coster, Mark J.; Chemical communications (Cambridge, England) 53 (2017) 4219–4221; doi:10.1039/c7cc00459a

data_7119872
_publ_section_title
;
 A bidirectional synthesis of spiroacetals via Rh(ii)-catalysed C-H
 insertion.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4219
_journal_page_last               4221
_journal_paper_doi               10.1039/c7cc00459a
_journal_volume                  53
_journal_year                    2017
_chemical_absolute_configuration ad
_chemical_formula_sum            'C23 H22 Br2 O6'
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_space_group_name_Hall           'P 2ac 2ab'
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_symmetry_space_group_name_Hall  'P 2ac 2ab'
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2016-11-29 deposited with the CCDC.
2017-03-24 downloaded from the CCDC.
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_collection
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_data_reduction
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
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_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_diffrn_ambient_temperature      130.0(1)
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_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            15254
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.889
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_exptl_absorpt_coefficient_mu    5.007
_exptl_absorpt_correction_T_max  1.00000
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_exptl_absorpt_process_details
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CrysAlisPro, Agilent Technologies,
Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
(compiled Feb  1 2013,16:14:44)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
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_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.675
_exptl_crystal_description       Block
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_exptl_crystal_size_max          0.5546
_exptl_crystal_size_mid          0.2710
_exptl_crystal_size_min          0.2193
_refine_diff_density_max         0.352
_refine_diff_density_min         -0.388
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details
;
 Flack x determined using 1909 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.012(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         4594
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0261
_refine_ls_R_factor_gt           0.0259
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+0.8656P]
 where P=(Fo^2^+2Fc^2^)/3
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_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0702
_refine_ls_wR_factor_ref         0.0703
_reflns_Friedel_coverage         0.720
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.981
_reflns_number_gt                4580
_reflns_number_total             4594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7cc00459a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments          'Adding full bibliography for 7119872.cif.'
_cod_original_cell_volume        2197.36(2)
_cod_database_code               7119872
_chemical_oxdiff_usercomment     'mark Coster sample MJC-2-049A'
_shelxl_version_number           2012-9