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_7230035
_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            'C53 H80 N22 O12 S5'
_chemical_formula_weight         1377.69
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 93.64(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   40.012(8)
_cell_length_b                   16.186(3)
_cell_length_c                   10.282(2)
_cell_measurement_reflns_used    8512
_cell_measurement_temperature    113(2)
_cell_measurement_theta_max      27.8744
_cell_measurement_theta_min      1.9809
_cell_volume                     6646(2)
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_diffrn_ambient_temperature      113(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'rigaku saturn'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0441
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            33058
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.886
_diffrn_reflns_theta_min         1.981
_exptl_absorpt_coefficient_mu    0.249
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   crystalclear
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_description       block
_exptl_crystal_F_000             2912
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.180
_exptl_crystal_size_min          0.120
_exptl_transmission_factor_max   0.7452
_exptl_transmission_factor_min   0.5951
_refine_diff_density_max         0.304
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     452
_refine_ls_number_reflns         7928
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0635
_refine_ls_R_factor_gt           0.0486
_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^)+(0.0663P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6308
_reflns_number_total             7928
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7ce01996c1.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7230035--7230039.cif.'
_cod_database_code               7230035
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_min   0.952
_shelx_estimated_absorpt_t_max   0.971
_shelx_res_checksum              21000