Monitoring structural transformations in crystals. 13. On photocyclization in 2,3,4,5,6-pentamethylbenzophenone, 1,3-diphenylbutan-1-one and 2,4,6-triisopropyl-4'-methoxybenzophenone
Bakowicz, Julia; Turowska-Tyrk, Ilona; Acta Crystallographica Section C 66 (2010) o29–o32; doi:10.1107/S0108270109052858

data_2017477
_publ_section_title
;
 Monitoring structural transformations in crystals. 13. On
 photocyclization in 2,3,4,5,6-pentamethylbenzophenone,
 1,3-diphenylbutan-1-one and 2,4,6-triisopropyl-4'-methoxybenzophenone
;
_journal_coeditor_code           GZ3170
_journal_issue                   1
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              o29
_journal_page_last               o32
_journal_paper_doi               10.1107/S0108270109052858
_journal_volume                  66
_journal_year                    2010
_chemical_formula_iupac          '0.90C23 H30 O2, 0.10C23 H30 O2'
_chemical_formula_moiety         '0.90(C23 H30 O2), 0.10(C23 H30 O2)'
_chemical_formula_sum            'C23 H30 O2'
_chemical_formula_weight         338.47
_chemical_name_systematic
;
2,4,6-triisopropyl-4'-methoxybenzophenone--
3,5-diisopropyl-7-(4-methoxyphenyl)-8,8-dimethylbicyclo[4.2.0]octa-1,3,5-
trien-7-ol (9/1)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.021(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.2288(10)
_cell_length_b                   12.0541(14)
_cell_length_c                   18.821(2)
_cell_measurement_reflns_used    1000
_cell_measurement_temperature    299(2)
_cell_measurement_theta_max      17.91
_cell_measurement_theta_min      3.65
_cell_volume                     2093.7(4)
_computing_cell_refinement       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2003)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2003)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      299(2)
_diffrn_measured_fraction_theta_full 0.969
_diffrn_measured_fraction_theta_max 0.969
_diffrn_measurement_device_type  'Kuma KM-4 CCD diffractometer'
_diffrn_measurement_method       '\w 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  0.0401
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            9964
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         4.02
_exptl_absorpt_coefficient_mu    0.067
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.074
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             736
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.264
_refine_diff_density_min         -0.154
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     328
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.645
_refine_ls_R_factor_all          0.1463
_refine_ls_R_factor_gt           0.0657
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1192P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1756
_refine_ls_wR_factor_ref         0.2316
_reflns_number_gt                1609
_reflns_number_total             3564
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            gz3170.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2017477
_cod_database_fobs_code          2017477