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_7208337
_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_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_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             2011-11-01
_audit_creation_method
;
Olex2 1.1
(compiled 2011.09.07 svn.r1971, GUI svn.r3853)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 102.026(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.9199(2)
_cell_length_b                   14.3119(4)
_cell_length_c                   13.7279(4)
_cell_measurement_reflns_used    4435
_cell_measurement_temperature    110.00(10)
_cell_measurement_theta_max      31.6527
_cell_measurement_theta_min      2.8398
_cell_volume                     2290.53(10)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
;
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
XL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
;
XS, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_diffrn_ambient_temperature      110.00(10)
_diffrn_detector_area_resol_mean 16.1450
_diffrn_measured_fraction_theta_full 0.9958
_diffrn_measured_fraction_theta_max 0.886
_diffrn_measurement_details
;
1 omega -89.00 5.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -24.0022 -77.0000 -180.0000 94

2 omega -48.00 45.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- -24.0022 77.0000 -60.0000 93

3 omega 15.00 56.00 1.0000 120.0000
omega____ theta____ kappa____ phi______ frames
- 25.5647 -77.0000 -30.0000 41
;
_diffrn_measurement_device_type  'SuperNova, Single source at offset), Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0244170000
_diffrn_orient_matrix_UB_12      0.0408279000
_diffrn_orient_matrix_UB_13      -0.0249116000
_diffrn_orient_matrix_UB_21      -0.0150747000
_diffrn_orient_matrix_UB_22      0.0157533000
_diffrn_orient_matrix_UB_23      0.0446067000
_diffrn_orient_matrix_UB_31      0.0535271000
_diffrn_orient_matrix_UB_32      0.0231074000
_diffrn_orient_matrix_UB_33      0.0136667000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_unetI/netI     0.0498
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            12391
_diffrn_reflns_theta_full        29.51
_diffrn_reflns_theta_max         31.74
_diffrn_reflns_theta_min         2.85
_diffrn_source                   'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.231
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.977
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.15 (release 03-08-2011 CrysAlis171 .NET)
(compiled Aug 3 2011,13:03:54)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.306
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             944
_exptl_crystal_recrystallization_method 'CD2Cl2, acetone'
_exptl_crystal_size_max          0.2505
_exptl_crystal_size_mid          0.1012
_exptl_crystal_size_min          0.076
_refine_diff_density_max         0.448
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     297
_refine_ls_number_reflns         6896
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0462
_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^)+(0.0322P)^2^+1.5380P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0991
_refine_ls_wR_factor_ref         0.1077
_reflns_number_gt                5498
_reflns_number_total             6896
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2ce25480h.txt
_cod_data_source_block           ijsf1114
_cod_original_cell_volume        2290.54(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7208337
_reflns_odcompleteness_completeness 99.58
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     29.51