New Route to Dehydroannulenes by Coupling Linear Polyynes Using Ruthenium Carbonyl
Richard D. Adams; Bo Qu; Mark D. Smith; Inorganic Chemistry 40 (2001) 2932–2934; doi:10.1021/ic001132w

data_4319737
_publ_section_title
;
 New Route to Dehydroannulenes by Coupling Linear Polyynes Using Ruthenium
 Carbonyl
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2932
_journal_page_last               2934
_journal_paper_doi               10.1021/ic001132w
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C69 H36 Cl2 Fe4 O12 Ru4'
_chemical_formula_weight         1755.56
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 107.262(4)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.222(4)
_cell_length_b                   10.121(2)
_cell_length_c                   31.938(7)
_cell_measurement_reflns_used    4365
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.43
_cell_volume                     6551(2)
_computing_cell_refinement       'SAINT+ NT V5.0 (Bruker, 1998)'
_computing_data_collection       'SMART NT V5.0 (Bruker, 1998)'
_computing_data_reduction        'SAINT+ NT V5.0'
_computing_molecular_graphics    'SHELXTL V5.1 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL V5.1'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART APEX 1K'
_diffrn_measurement_method       '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  0.1338
_diffrn_reflns_av_sigmaI/netI    0.1639
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            28526
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.41
_diffrn_standards_decay_%        -0.02
_exptl_absorpt_coefficient_mu    1.898
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.780
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             3440
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.445
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     779
_refine_ls_number_reflns         9419
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.1210
_refine_ls_R_factor_gt           0.0521
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(5.03(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0230P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1294
_reflns_number_gt                3859
_reflns_number_total             9419
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001132w.cif
_cod_data_source_block           bo02b1t
_cod_database_code               4319737