A Metal-Templated 4 + 2 Cycloaddition Reaction of an Alkyne and a Diyne To Form a 1,2-Aryne
Tsui, Jordan A.; Sterenberg, Brian T.; Organometallics 28 (2009) 4906–; doi:10.1021/om900578d

data_4070038
_publ_section_title
;
 A Metal-Templated 4 + 2 Cycloaddition Reaction of an Alkyne and a Diyne
 To Form a 1,2-Aryne
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              4906
_journal_paper_doi               10.1021/om900578d
_journal_volume                  28
_journal_year                    2009
_chemical_formula_moiety         'C62 H48 O4 P4 Pt1 W1, C4 H10 O'
_chemical_formula_sum            'C64 H52 Cl2 O5 P4 Pt W'
_chemical_formula_weight         1474.78
_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                 117.7430(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.8800(19)
_cell_length_b                   15.9958(15)
_cell_length_c                   21.821(2)
_cell_measurement_reflns_used    5545
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.01
_cell_measurement_theta_min      2.24
_cell_volume                     6450.2(10)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0528
_diffrn_reflns_av_sigmaI/netI    0.0507
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            44326
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    4.175
_exptl_absorpt_correction_T_max  0.5925
_exptl_absorpt_correction_T_min  0.2668
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.519
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2888
_exptl_crystal_size_max          0.43
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.735
_refine_diff_density_min         -1.170
_refine_diff_density_rms         0.231
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     709
_refine_ls_number_reflns         13116
_refine_ls_number_restraints     20
_refine_ls_restrained_S_all      1.085
_refine_ls_R_factor_all          0.0878
_refine_ls_R_factor_gt           0.0479
_refine_ls_shift/su_max          3.822
_refine_ls_shift/su_mean         0.050
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0913P)^2^+10.2970P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1382
_refine_ls_wR_factor_ref         0.1654
_reflns_number_gt                8716
_reflns_number_total             13116
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om900578d_si_002.cif
_cod_data_source_block           jt-06
_cod_original_cell_volume        6450.1(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4070038