Solid state [2 + 2] photocycloaddition for constructing dimers of N,N′-diacyl-1,4-dihydropyrazines based on thiourea-induced assembly
Fan, Qiangwen; Duan, Xiaowei; Yan, Hong; CrystEngComm 20 (2018) 1151–; doi:10.1039/C7CE01996C

data_7230039
_publ_section_title
;
 Solid state [2 + 2] photocycloaddition for constructing dimers of
 N,N&#x2032;-diacyl-1,4-dihydropyrazines based on thiourea-induced
 assembly
;
_journal_issue                   8
_journal_name_full               CrystEngComm
_journal_page_first              1151
_journal_paper_doi               10.1039/C7CE01996C
_journal_volume                  20
_journal_year                    2018
_chemical_formula_sum            'C11 H18 N4 O2 S'
_chemical_formula_weight         270.35
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2018-01-12 deposited with the CCDC.
2018-01-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.88(3)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.286(3)
_cell_length_b                   10.958(2)
_cell_length_c                   16.735(3)
_cell_measurement_reflns_used    5236
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.8824
_cell_measurement_theta_min      2.2219
_cell_volume                     2801.7(9)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  confocal
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0571
_diffrn_reflns_av_unetI/netI     0.0573
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28188
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.928
_diffrn_reflns_theta_min         1.333
_exptl_absorpt_coefficient_mu    0.232
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.282
_exptl_crystal_description       Orthorhombic
_exptl_crystal_F_000             1152
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7453
_exptl_transmission_factor_min   0.5950
_refine_diff_density_max         0.251
_refine_diff_density_min         -0.213
_refine_diff_density_rms         0.049
_refine_ls_extinction_coef       0.0137(15)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   0.989
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     358
_refine_ls_number_reflns         6684
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      0.989
_refine_ls_R_factor_all          0.0922
_refine_ls_R_factor_gt           0.0546
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0752P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1285
_refine_ls_wR_factor_ref         0.1482
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4224
_reflns_number_total             6684
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01996c1.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7230035--7230039.cif.'
_cod_original_cell_volume        2801.6(10)
_cod_database_code               7230039
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.955
_shelx_estimated_absorpt_t_max   0.973
_shelx_res_checksum              16928