Controlled photochemical reaction of 4-oxo(phenylacetyl)morpholine and 1-(phenylglyoxylyl)piperidine in solid supramolecular systems
Lavy, Tali; Sheynin, Yana; Sparkes, Hazel A.; Howard, Judith A. K.; Kaftory, Menahem; CrystEngComm 10 (2008) 734–; doi:10.1039/b715981a

data_7201790
_publ_section_title
;
 Controlled photochemical reaction of 4-oxo(phenylacetyl)morpholine and
 1-(phenylglyoxylyl)piperidine in solid supramolecular systems
;
_journal_issue                   6
_journal_name_full               CrystEngComm
_journal_page_first              734
_journal_paper_doi               10.1039/b715981a
_journal_volume                  10
_journal_year                    2008
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C30 H20 Cl2 O2, C12 H13 N O3'
_chemical_formula_sum            'C42 H33 Cl2 N O5'
_chemical_formula_weight         702.59
_chemical_name_common
;
2,4-hexadiyne-1,6-diol-1,6-bis(2-chlorophenyl)-1,6-diphenyl,
4-oxo(phenylacetyl)morpholine clathrate
;
_chemical_name_systematic
;
2,4-hexadiyne-1,6-diol-1,6-bis(2-chlorophenyl)-1,6-diphenyl,
4-oxo(phenylacetyl)morpholine clathrate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 111.8526(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.2078(2)
_cell_length_b                   24.8368(7)
_cell_length_c                   9.4738(3)
_cell_measurement_reflns_used    3583
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.08
_cell_measurement_theta_min      1.018
_cell_volume                     1792.51(9)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.930
_diffrn_measured_fraction_theta_max 0.930
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       CCD
_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  0.0856
_diffrn_reflns_av_sigmaI/netI    0.1478
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            12082
_diffrn_reflns_theta_full        27.35
_diffrn_reflns_theta_max         27.35
_diffrn_reflns_theta_min         1.64
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.228
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             732
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.327
_refine_diff_density_min         -0.223
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.92(8)
_refine_ls_extinction_coef       0.027(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.819
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         7122
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      0.818
_refine_ls_R_factor_all          0.1424
_refine_ls_R_factor_gt           0.0584
_refine_ls_shift/su_max          0.028
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0663P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1317
_refine_ls_wR_factor_ref         0.1565
_reflns_number_gt                3098
_reflns_number_total             7122
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715981a.txt
_cod_data_source_block           IVa
_cod_original_sg_symbol_H-M      P21
_cod_database_code               7201790