Revisiting the Aufbau Reaction with Acetylene: Further Insights from Experiment and Theory
Karpiniec, Samuel S.; McGuinness, David S.; Gardiner, Michael G.; Yates, Brian F.; Patel, Jim; Organometallics 30 (2011) 1569–; doi:10.1021/om101114c

data_4064066
_publ_section_title
;
 Revisiting the Aufbau Reaction with Acetylene: Further Insights from
 Experiment and Theory
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1569
_journal_paper_doi               10.1021/om101114c
_journal_volume                  30
_journal_year                    2011
_chemical_formula_moiety         'C56 H60 Al4 O8'
_chemical_formula_sum            'C56 H60 Al4 O8'
_chemical_formula_weight         968.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_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_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                 92.923(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.819(3)
_cell_length_b                   15.4020(9)
_cell_length_c                   13.3430(9)
_cell_measurement_reflns_used    21346
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.24
_cell_measurement_theta_min      2.62
_cell_volume                     2631.0(7)
_computing_cell_refinement       XDS
_computing_data_collection       BLU-ICE
_computing_data_reduction        XDS
_computing_molecular_graphics
;
'X-SEED (Barbour, 2008) and ORTEPIII (Farrugia, 2008)' 
;
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 'ADSC Q210'
_diffrn_measured_fraction_theta_full 0.958
_diffrn_measured_fraction_theta_max 0.958
_diffrn_measurement_device_type  '3-BM1 Australian Synchrotron'
_diffrn_measurement_method       Rotation
_diffrn_radiation_monochromator  Si<111>
_diffrn_radiation_source         'Synchrotron BM'
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.77500
_diffrn_reflns_av_R_equivalents  0.0937
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27949
_diffrn_reflns_theta_full        26.59
_diffrn_reflns_theta_max         26.59
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    0.141
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1024
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.423
_refine_diff_density_min         -0.338
_refine_diff_density_rms         0.055
_refine_ls_extinction_coef       0.106(12)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4075
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0814
_refine_ls_R_factor_gt           0.0733
_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^)+(0.1065P)^2^+2.0574P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1966
_refine_ls_wR_factor_ref         0.2063
_reflns_number_gt                3500
_reflns_number_total             4075
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om101114c_si_002.cif
_cod_data_source_block           d:\as4m2a\revised
_cod_original_cell_volume        2631.0(6)
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4064066