Ring expansion of cyclic 1,2-diols to form medium sized rings via ruthenium catalyzed transfer hydrogenative [4+2] cycloaddition
Zachary A. Kasun; Laina M. Geary; Michael J. Krische; Chem.Commun. 50 (2014) 7545–; doi:10.1039/C4CC03983A

data_7114649
_publ_section_title
;
 Ring expansion of cyclic 1,2-diols to form medium sized rings via
 ruthenium catalyzed transfer hydrogenative [4+2] cycloaddition
;
_journal_name_full               Chem.Commun.
_journal_page_first              7545
_journal_paper_doi               10.1039/C4CC03983A
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C14 H18 O4'
_chemical_formula_sum            'C14 H18 O4'
_chemical_formula_weight         250.28
_space_group_crystal_system      triclinic
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_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
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_cell_angle_beta                 106.543(16)
_cell_angle_gamma                91.530(11)
_cell_formula_units_Z            4
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_cell_length_b                   10.119(3)
_cell_length_c                   14.590(4)
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_cell_measurement_theta_min      2.0
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_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
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_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
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_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      100(2)
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_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Rgiaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_unetI/netI     0.0545
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_diffrn_reflns_Laue_measured_fraction_max 0.996
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_diffrn_reflns_limit_l_min       -18
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_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.497
_diffrn_reflns_theta_min         1.456
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.103
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.770
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
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_refine_diff_density_min         -0.308
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
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_refine_ls_matrix_type           full
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_refine_ls_number_reflns         5385
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0610
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0641P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
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_reflns_number_gt                4127
_reflns_number_total             5385
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc03983a2.cif
_cod_data_source_block           shelx_1
_cod_original_cell_volume        1177.6(7)
_cod_database_code               7114649
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_shelx_estimated_absorpt_t_max   0.990
_shelxl_version_number           2013-4
_shelx_res_checksum              84144
_shelx_hkl_checksum              65650