Hydrogen-bond quenching of photodecarbonylation in the solid state and recovery of reactivity by co-crystallization
Zhang, Jing; Gembicky, Milan; Messerschmidt, Marc; Coppens, Philip; Chemical Communications (Cambridge, United Kingdom)  (2007) 2399–2401; doi:10.1039/b700073a

data_7101968
_publ_section_title
;
 Hydrogen-bond quenching of photodecarbonylation in the solid state and
 recovery of reactivity by co-crystallization
;
_journal_coden_ASTM              CHCOFS
_journal_issue                   23
_journal_name_full
;
 Chemical Communications (Cambridge, United Kingdom)
;
_journal_page_first              2399
_journal_page_last               2401
_journal_paper_doi               10.1039/b700073a
_journal_year                    2007
_chemical_formula_sum            'C31 H40 O5'
_chemical_formula_weight         492.63
_chemical_name_common            HOTMK-biscyclohexanone
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                109.2590(10)
_cell_angle_beta                 92.6450(10)
_cell_angle_gamma                90.7540(10)
_cell_formula_units_Z            2
_cell_length_a                   7.74590(10)
_cell_length_b                   11.0192(2)
_cell_length_c                   16.6519(3)
_cell_measurement_reflns_used    4447
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      26.359
_cell_measurement_theta_min      2.634
_cell_volume                     1339.72(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0312
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            14589
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.30
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.994
_exptl_absorpt_correction_T_min  0.935
_exptl_absorpt_correction_type   'empirical SADABS'
_exptl_absorpt_process_details
'Blessing, R. (1995) Acta Crystallogr., A51, 33-38'
_exptl_crystal_colour            Colorless
_exptl_crystal_density_diffrn    1.221
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             532
_exptl_crystal_size_max          0.09
_exptl_crystal_size_mid          0.085
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.287
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.012
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     485
_refine_ls_number_reflns         5489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0376
_refine_ls_shift/su_max          0.022
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0466P)^2^+0.3199P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0942
_reflns_number_gt                4321
_reflns_number_total             5489
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b700073a.txt
_cod_data_source_block           scale
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101968