Regioselective Baeyer–Villiger oxidation of lignin model compounds with tin beta zeolite catalyst and hydrogen peroxide
Jennings, John A.; Parkin, Sean; Munson, Eric; Delaney, Sean P.; Calahan, Julie L.; Isaacs, Mark; Hong, Kunlun; Crocker, Mark; RSC Adv. 7 (2017) 25987–; doi:10.1039/C7RA03830E

data_7228285
_publ_section_title
;
 Regioselective Baeyer--Villiger oxidation of lignin model compounds with
 tin beta zeolite catalyst and hydrogen peroxide
;
_journal_issue                   42
_journal_name_full               'RSC Adv.'
_journal_page_first              25987
_journal_paper_doi               10.1039/C7RA03830E
_journal_volume                  7
_journal_year                    2017
_chemical_formula_moiety         'C16 H16 O5'
_chemical_formula_sum            'C16 H16 O5'
_chemical_formula_weight         288.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2017-03-30 deposited with the CCDC.
2017-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                87.423(4)
_cell_angle_beta                 89.813(5)
_cell_angle_gamma                77.523(5)
_cell_formula_units_Z            4
_cell_length_a                   5.8859(5)
_cell_length_b                   12.7775(10)
_cell_length_c                   19.1219(14)
_cell_measurement_reflns_used    4563
_cell_measurement_temperature    90.0(2)
_cell_measurement_theta_max      68.21
_cell_measurement_theta_min      3.55
_cell_volume                     1402.69(19)
_computing_cell_refinement       '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_data_collection       '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_data_reduction        '<i>APEX2</i> (Bruker-AXS, 2006)'
_computing_molecular_graphics    '<i>XP in SHELXTL</i> (Sheldrick, 2008)'
_computing_publication_material
'<i>SHELX</i> (Sheldrick, 2008) and <i>CIFFIX</i> (Parkin, 2013)'
_computing_structure_refinement  '<i>SHELXL-2016/6</i> (Sheldrick, 2015b)'
_computing_structure_solution    '<i>SHELXT</i> (Sheldrick, 2015a)'
_diffrn_ambient_temperature      90.0(2)
_diffrn_detector_area_resol_mean 5.6
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker X8 Proteum diffractometer'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24835
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.429
_diffrn_reflns_theta_min         2.313
_diffrn_source                   'fine-focus rotating anode'
_exptl_absorpt_coefficient_mu    0.847
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '<i>TWINABS</i> (Sheldrick, 2008b)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       block
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.120
_refine_diff_density_max         0.389
_refine_diff_density_min         -0.347
_refine_diff_density_rms         0.088
_refine_ls_extinction_coef       0.0022(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick, 2015b)'
_refine_ls_goodness_of_fit_ref   1.104
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     385
_refine_ls_number_reflns         24835
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.104
_refine_ls_R_factor_all          0.0835
_refine_ls_R_factor_gt           0.0684
_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^)+(0.1138P)^2^+0.4394P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2084
_refine_ls_wR_factor_ref         0.2283
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18988
_reflns_number_total             24835
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ra03830e2.cif
_cod_data_source_block           x17027
_cod_database_code               7228285
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.849
_shelx_estimated_absorpt_t_max   0.905
_exptl_absorpt_special_details
; 
In addition to absorption, multi-scan techniques also correct other slowly 
varying changes in scale factor over reciprocal space, such as those caused 
by x-ray beam inhomogeneity, goniometer imperfection, crystal decomposition, 
crystal longer than the x-ray beam cross section, absorption by the crystal 
mount etc.  These account, by and large, for much of the difference between 
estimated values of Tmin and Tmax and the _exptl_absorpt_correction_ values. 
;
_shelx_res_checksum              53905