Photochemical-mediated solid-state [2+2]-cycloaddition reactions of an unsymmetrical dibenzylidene acetone (monothiophos-dba)
Jarvis, A. G.; Sparkes, H. A.; Tallentire, S. E.; Hatcher, L. E.; Warren, M. R.; Raithby, P. R.; Allan, D. R.; Whitwood, A. C.; Cockett, M. C. R.; Duckett, S. B.; Clark, J. L.; Fairlamb, I. J. S.; CrystEngComm 14 (2012) 5564–; doi:10.1039/c2ce25480h

data_7208336
_publ_section_title
;
 Photochemical-mediated solid-state [2+2]-cycloaddition reactions of an
 unsymmetrical dibenzylidene acetone (monothiophos-dba)
;
_journal_issue                   17
_journal_name_full               CrystEngComm
_journal_page_first              5564
_journal_paper_doi               10.1039/c2ce25480h
_journal_volume                  14
_journal_year                    2012
_chemical_formula_moiety         'C58 H46 O2 P2 S2'
_chemical_formula_sum            'C58 H46 O2 P2 S2'
_chemical_formula_weight         901.0
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date
;
'Thu Jan 29 14:58:21 2009'
;
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.3283(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.39010(10)
_cell_length_b                   17.15340(10)
_cell_length_c                   14.8607(2)
_cell_measurement_reflns_used    11626
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      70.4366
_cell_measurement_theta_min      3.9815
_cell_volume                     2338.45(4)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 8.2707
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_details
;
1 omega 35.00 88.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 13.7937 45.0000 150.0000 0.0000 0.0000 53

2 omega -10.00 48.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 13.7937 -77.0000 60.0000 0.0000 0.0000 58

3 omega 35.00 88.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 13.7937 45.0000 270.0000 0.0000 0.0000 53

4 omega -38.00 20.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -13.7937 -77.0000 240.0000 0.0000 0.0000 58

5 omega -72.00 -14.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 77.0000 210.0000 0.0000 0.0000 58

6 omega -178.00 -90.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 0.0000 210.0000 0.0000 0.0000 88

7 omega -72.00 -19.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 45.0000 210.0000 0.0000 0.0000 53

8 omega -121.00 -68.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 45.0000 150.0000 0.0000 0.0000 53

9 omega -72.00 -14.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 77.0000 330.0000 0.0000 0.0000 58

10 omega 21.00 80.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 100.0000 -77.0000 240.0000 0.0000 0.0000 59

11 omega 75.00 128.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 100.0000 -45.0000 210.0000 0.0000 0.0000 53

12 omega 74.00 128.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- 100.0000 82.0000 107.0000 0.0000 0.0000 54

13 omega -178.00 -6.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 0.0000 180.0000 0.0000 0.0000 172

14 omega -178.00 -6.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 0.0000 0.0000 0.0000 0.0000 172

15 omega -178.00 -6.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 0.0000 330.0000 0.0000 0.0000 172

16 omega -178.00 -49.00 1.0000 23.1000
omega____ theta____ kappa____ phi______ omega'___ theta'___ frames
- -93.0000 0.0000 150.0000 0.0000 0.0000 129

;
_diffrn_measurement_device_type  'CCD are detector'
_diffrn_measurement_method       'Phi & Omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Cu) X-ray Source'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_sigmaI/netI    0.0484
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21056
_diffrn_reflns_theta_full        70.46
_diffrn_reflns_theta_max         70.46
_diffrn_reflns_theta_min         3.99
_exptl_absorpt_coefficient_mu    2.014
_exptl_absorpt_correction_T_max  0.920
_exptl_absorpt_correction_T_min  0.191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET)
(compiled Apr 21 2008,18:23:10)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.280
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       shard
_exptl_crystal_F_000             944
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.231
_refine_diff_density_rms         0.041
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     392
_refine_ls_number_reflns         4254
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0395
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0488P)^2^+1.3514P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0981
_refine_ls_wR_factor_ref         0.1022
_reflns_number_gt                3679
_reflns_number_total             4254
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25480h.txt
_cod_data_source_block           ijf0902
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7208336