Rhodium(I)-Catalyzed [2 + 2 + 2] Cycloaddition Reactions of Triacetylenic 15-Membered Aza Macrocycles: A Comparative Structural Study
Brun, Sandra; Torrent, Anna; Pla-Quintana, Anna; Roglans, Anna; Fontrodona, Xavier; Benet-Buchholz, Jordi; Parella, Teodor; Organometallics 31 (2012) 318–; doi:10.1021/om200927f

data_4067928
_publ_section_title
;
 Rhodium(I)-Catalyzed [2 + 2 + 2] Cycloaddition Reactions of Triacetylenic
 15-Membered Aza Macrocycles: A Comparative Structural Study
;
_journal_issue                   1
_journal_name_full               Organometallics
_journal_page_first              318
_journal_paper_doi               10.1021/om200927f
_journal_volume                  31
_journal_year                    2012
_chemical_formula_moiety         'C37 H41 N3 O6 S3, C4 H8 O'
_chemical_formula_sum            'C41 H49 N3 O7 S3'
_chemical_formula_weight         792.01
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 96.319(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   29.726(8)
_cell_length_b                   11.085(3)
_cell_length_c                   24.760(7)
_cell_measurement_reflns_used    5138
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      20.19
_cell_measurement_theta_min      2.76
_cell_volume                     8109(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  ccd
_diffrn_measurement_method       'phi and omega scans'
_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  0.1287
_diffrn_reflns_av_sigmaI/netI    0.1060
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -39
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            62782
_diffrn_reflns_theta_full        28.32
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.96
_exptl_absorpt_coefficient_mu    0.235
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.808388
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS v2.10 BRUKER 2001'
_exptl_crystal_colour            colorles
_exptl_crystal_density_diffrn    1.297
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             3360
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.378
_refine_diff_density_min         -0.326
_refine_diff_density_rms         0.049
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         10019
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.010
_refine_ls_R_factor_all          0.1836
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0935P)^2^+1.3190P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.2172
_reflns_number_gt                4152
_reflns_number_total             10019
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200927f_si_003.cif
_cod_data_source_block           sb104_2c
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4067928