Glaser–Eglinton–Hay sp–sp coupling and macrocyclization: construction of a new class of polyether macrocycles having a 1,3-diyne unit
Naveen, Naveen; Babu, Srinivasarao Arulananda; Kaur, Gurpreet; Aslam, Nayyar Ahmad; Karanam, Maheswararao; RSC Adv. 4 (2014) 18904–; doi:10.1039/C4RA02174F

data_7235614
_publ_section_title
;
 Glaser--Eglinton--Hay sp--sp coupling and macrocyclization: construction
 of a new class of polyether macrocycles having a 1,3-diyne unit
;
_journal_issue                   36
_journal_name_full               'RSC Adv.'
_journal_page_first              18904
_journal_paper_doi               10.1039/C4RA02174F
_journal_volume                  4
_journal_year                    2014
_chemical_formula_moiety         'C24 H20 O4'
_chemical_formula_sum            'C24 H20 O4'
_chemical_formula_weight         372.42
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_primary     direct
_audit_creation_date             2014-02-20
_audit_creation_method
;
  Olex2 1.2
  (compiled Apr 23 2013 17:59:47, GUI svn.r4466)
;
_cell_angle_alpha                90
_cell_angle_beta                 93.902(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   4.856(3)
_cell_length_b                   53.09(4)
_cell_length_c                   7.510(5)
_cell_measurement_temperature    298(2)
_cell_volume                     1932(2)
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
        J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
        SHELXL, G.M. Sheldrick, Acta Cryst.
        (2008). A64, 112-122
;
_computing_structure_solution
;
        SHELXS, G.M. Sheldrick, Acta Cryst.
        (2008). A64, 112-122
;
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 0.9861
_diffrn_measured_fraction_theta_max 0.9861
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0816
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -2
_diffrn_reflns_limit_k_max       63
_diffrn_reflns_limit_k_min       -61
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            10743
_diffrn_reflns_theta_full        25.0259
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         0.77
_exptl_absorpt_coefficient_mu    0.087
_exptl_absorpt_correction_T_max  0.7355
_exptl_absorpt_correction_T_min  0.5730
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
        SADABS-2008/1 (Bruker,2008) was used for absorption correction.
        wR2(int) was 0.1098 before and 0.0781 after correction.
        The Ratio of minimum to maximum transmission is 0.7079.
        The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.2805
_exptl_crystal_F_000             784.0
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.4804
_refine_diff_density_min         -0.3494
_refine_diff_density_rms         0.0933
_refine_ls_goodness_of_fit_ref   1.1283
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.1283
_refine_ls_R_factor_all          0.1366
_refine_ls_R_factor_gt           0.0797
_refine_ls_shift/su_max          0.0159
_refine_ls_shift/su_mean         0.0034
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2365
_reflns_number_gt                1842
_reflns_number_total             3345
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            c4ra02174f2.cif
_cod_data_source_block           nm1135a1_0m
_cod_database_code               7235614