Isolation and structure of an 18-membered macrocycle containing two diselenide linkages and its precursor
Raju, Saravanan; Butcher, Ray J.; Singh, Harkesh B.; Acta Crystallographica Section C 75 (2019) –; doi:10.1107/S2053229619002341

data_2021523
_publ_section_title
;
 Isolation and structure of an 18-membered macrocycle containing two
 diselenide linkages and its precursor
;
_journal_coeditor_code           FN3298
_journal_issue                   3
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first
;
;
_journal_paper_doi               10.1107/S2053229619002341
_journal_volume                  75
_journal_year                    2019
_chemical_formula_iupac          'C36 H34 N4 O6 Se4'
_chemical_formula_moiety         'C36 H34 N4 O6 Se4'
_chemical_formula_sum            'C36 H34 N4 O6 Se4'
_chemical_formula_weight         934.51
_chemical_name_systematic
'10,27-Di-<i>tert</i>-butyl 11,28-dioxo-2,3,19,20-tetraselena-10,12,27,29-tetraazapentacyclo[28.4.0.0^4,9^.0^13,18^.0^21,26^]tetratriaconta-1(30),4(9),5,7,13,15,17,21,23,25,31,33-dodecaene-10,27-dicarboxylate'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                101.000(2)
_cell_angle_beta                 108.394(2)
_cell_angle_gamma                105.264(2)
_cell_formula_units_Z            1
_cell_length_a                   9.4865(3)
_cell_length_b                   9.7410(2)
_cell_length_c                   11.2789(3)
_cell_measurement_reflns_used    15479
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31.2870
_cell_measurement_theta_min      2.3910
_cell_volume                     910.42(5)
_computing_cell_refinement
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_collection
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_data_reduction
;
CrysAlis PRO (Rigaku OD, 2015)
;
_computing_molecular_graphics
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_publication_material
;
OLEX2 (Dolomanov <i>et al.</i>, 2009)
;
_computing_structure_refinement
;
SHELXL2018 (Sheldrick, 2015b)
;
_computing_structure_solution
;
SHELXT2014 (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.917
_diffrn_measurement_device_type  'Rigaku CCD dual source'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0368
_diffrn_reflns_av_unetI/netI     0.0300
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            23930
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.185
_diffrn_reflns_theta_min         2.413
_diffrn_source                   'fine-focus sealed X-ray tube'
_exptl_absorpt_coefficient_mu    4.080
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82321
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlis PRO; Rigaku OD, 2015)
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.704
_exptl_crystal_description       needle
_exptl_crystal_F_000             462
_exptl_crystal_size_max          0.172
_exptl_crystal_size_mid          0.156
_exptl_crystal_size_min          0.109
_refine_diff_density_max         0.686
_refine_diff_density_min         -0.468
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.051
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     294
_refine_ls_number_reflns         5406
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_R_factor_all          0.0332
_refine_ls_R_factor_gt           0.0258
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0337P)^2^+0.3223P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0620
_refine_ls_wR_factor_ref         0.0651
_reflns_number_gt                4766
_reflns_number_total             5406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            fn3298sup1.cif
_cod_data_source_block           4
_cod_original_cell_volume        910.42(4)
_cod_database_code               2021523
_shelx_hkl_checksum              57702
_shelx_res_checksum              30740
_cod_database_fobs_code 2021523