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_7239032
_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         'C41 H35 O'
_chemical_formula_sum            'C41 H38 O'
_chemical_formula_weight         546.71
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             2012-05-08
_audit_creation_method
;
Olex2 1.2-ac2
(compiled 2012.03.06 svn.r2239, GUI svn.r4109)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 127.958(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.9360(9)
_cell_length_b                   7.9365(3)
_cell_length_c                   25.6157(14)
_cell_measurement_reflns_used    3781
_cell_measurement_temperature    291(2)
_cell_measurement_theta_max      66.9666
_cell_measurement_theta_min      3.4498
_cell_volume                     3195.6(3)
_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 -59.00 -33.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 178.0000 0.0000 26

2 omega 28.00 57.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 57.0000 -150.0000 29

3 omega -92.00 -41.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -57.0000 -120.0000 51

4 omega -26.00 28.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 30.0000 90.0000 54

5 omega -31.00 -6.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 30.0000 -180.0000 25

6 omega -100.00 -33.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 178.0000 -150.0000 67

7 omega -62.00 26.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 57.0000 -150.0000 88

8 omega -7.00 30.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 37.0000 120.0000 37

9 omega 123.00 175.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 101.0000 72.0000 52

10 omega 122.00 178.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 111.0000 30.0000 56

11 omega 39.00 69.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 -30.0000 30.0000 30

12 omega 40.00 91.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 -30.0000 60.0000 51

13 omega 87.00 114.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 30.0000 90.0000 27

14 omega 123.00 171.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 30.0000 90.0000 48

15 omega 60.00 171.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 15.0000 -120.0000 111

16 omega 42.00 78.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 -30.0000 -60.0000 36

17 omega 48.00 74.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 -37.0000 -151.0000 26

18 omega 51.00 132.00 1.0000 40.0000
omega____ theta____ kappa____ phi______ frames
- 111.7251 -61.0000 120.0000 81

19 omega -4.00 42.00 1.0000 2.0000
omega____ theta____ kappa____ phi______ frames
- 0.0000 -99.0000 -90.0000 46

20 omega -111.00 -45.00 1.0000 6.0000
omega____ theta____ kappa____ phi______ frames
- -42.5000 -57.0000 60.0000 66
;
_diffrn_measurement_device_type  'Xcalibur, Eos, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0183087000
_diffrn_orient_matrix_UB_12      -0.0264491000
_diffrn_orient_matrix_UB_13      0.0682778000
_diffrn_orient_matrix_UB_21      -0.0694232000
_diffrn_orient_matrix_UB_22      0.0872391000
_diffrn_orient_matrix_UB_23      -0.0245896000
_diffrn_orient_matrix_UB_31      -0.0328204000
_diffrn_orient_matrix_UB_32      -0.1714621000
_diffrn_orient_matrix_UB_33      -0.0232193000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.5418
_diffrn_reflns_av_R_equivalents  0.0366
_diffrn_reflns_av_unetI/netI     0.0423
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -6
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            11885
_diffrn_reflns_theta_full        67.11
_diffrn_reflns_theta_max         67.11
_diffrn_reflns_theta_min         3.45
_diffrn_source                   'Enhance (Cu) X-ray Source'
_diffrn_source_current           n/a
_diffrn_source_voltage           n/a
_exptl_absorpt_coefficient_mu    0.503
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.78072
_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    1.136
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.33
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         0.592
_refine_diff_density_min         -0.313
_refine_diff_density_rms         0.040
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     408
_refine_ls_number_reflns         5710
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0764
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1212P)^2^+0.7618P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2249
_refine_ls_wR_factor_ref         0.2499
_reflns_number_gt                4134
_reflns_number_total             5710
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c3ra41326h.txt
_cod_data_source_block           20120553
_cod_database_code               7239032
_chemical_oxdiff_formula         'C11 H10 S O2'
_reflns_odcompleteness_completeness 99.94
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97