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_7201795
_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_formula_moiety         'C30 H22 O2, 2(C12 H13 N O3)'
_chemical_formula_sum            'C54 H48 N2 O8'
_chemical_formula_weight         852.94
_chemical_name_common
;
1,1,6,6-tetrahphenyl-2,4-hexadiyne-1,6-diol, 4-
oxo(phenylacetyl)morpholine clathrate
;
_chemical_name_systematic
;
1,1,6,6-tetrahphenyl-2,4-hexadiyne-1,6-diol,
4-oxo(phenylacetyl)morpholine clathrate
;
_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                 94.7310(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   5.9540(2)
_cell_length_b                   27.5070(7)
_cell_length_c                   13.7050(5)
_cell_measurement_reflns_used    3145
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.028
_cell_measurement_theta_min      1.018
_cell_volume                     2236.91(12)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.99
_diffrn_measured_fraction_theta_max 0.99
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0963
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3584
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.085
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             900
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.142
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.032
_refine_ls_extinction_coef       0.028(3)
_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   0.869
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     291
_refine_ls_number_reflns         3584
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.869
_refine_ls_R_factor_all          0.1456
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0656P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1076
_refine_ls_wR_factor_ref         0.1321
_reflns_number_gt                1599
_reflns_number_total             3584
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b715981a.txt
_cod_data_source_block           IIa
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               7201795