Synthesis of cyclopentadienyl alkyl ethers via Pd-catalyzed cyclotrimerization of diarylacetylenes
Cai, Ranran; Huang, Mengmeng; Cui, Xiuling; Zhang, Jianye; Du, Chenxia; Wu, Yusheng; Wu, Yangjie; RSC Advances 3 (2013) 13140–; doi:10.1039/c3ra41326h

data_7239031
_publ_section_title
;
 Synthesis of cyclopentadienyl alkyl ethers via Pd-catalyzed
 cyclotrimerization of diarylacetylenes
;
_journal_issue                   32
_journal_name_full               'RSC Advances'
_journal_page_first              13140
_journal_paper_doi               10.1039/c3ra41326h
_journal_volume                  3
_journal_year                    2013
_chemical_formula_moiety         'C28 H20 O'
_chemical_formula_sum            'C28 H20 O'
_chemical_formula_weight         372.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2011-12-30
_audit_creation_method
;
Olex2 1.1
(compiled 2011.11.01 svn.r2039, GUI svn.r3906)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 117.408(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.7493(14)
_cell_length_b                   8.1753(3)
_cell_length_c                   21.7304(12)
_cell_measurement_reflns_used    1789
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      26.3153
_cell_measurement_theta_min      2.9913
_cell_volume                     4061.0(4)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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      291.15
_diffrn_detector_area_resol_mean 16.2312
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
1 omega -16.00 25.00 1.0000 19.0000
omega____ theta____ kappa____ phi______ frames
- -17.2104 -99.0000 0.0000 41

2 omega -39.00 13.00 1.0000 19.0000
omega____ theta____ kappa____ phi______ frames
- -17.2104 57.0000 -30.0000 52

3 omega -53.00 90.00 1.0000 19.0000
omega____ theta____ kappa____ phi______ frames
- 19.9448 0.0000 -60.0000 143
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0143077000
_diffrn_orient_matrix_UB_12      0.0758844000
_diffrn_orient_matrix_UB_13      -0.0029181000
_diffrn_orient_matrix_UB_21      -0.0243685000
_diffrn_orient_matrix_UB_22      -0.0280050000
_diffrn_orient_matrix_UB_23      -0.0305283000
_diffrn_orient_matrix_UB_31      -0.0128216000
_diffrn_orient_matrix_UB_32      -0.0313582000
_diffrn_orient_matrix_UB_33      0.0202928000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0315
_diffrn_reflns_av_unetI/netI     0.0399
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -4
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            8377
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.00
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.94670
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_refine_diff_density_max         0.169
_refine_diff_density_min         -0.193
_refine_diff_density_rms         0.033
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     262
_refine_ls_number_reflns         4148
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0480
_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^)+(0.0477P)^2^+0.6729P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1043
_refine_ls_wR_factor_ref         0.1209
_reflns_number_gt                2821
_reflns_number_total             4148
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41326h.txt
_cod_data_source_block           201112183
_cod_database_code               7239031
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.78
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32