Highly Efficient Synthesis ofcis-[3]Cumulenic Diols via Zirconocene-Mediated Coupling of 1,3-Butadiynes with Aldehydes
Fu, Xiaoping; Yu, Shasha; Fan, Guoqin; Liu, Yuanhong; Li, Yuxue; Organometallics 31 (2012) 531–; doi:10.1021/om201125z

data_4068126
_publ_section_title
;
 Highly Efficient Synthesis ofcis-[3]Cumulenic Diols via
 Zirconocene-Mediated Coupling of 1,3-Butadiynes with Aldehydes
;
_journal_issue                   2
_journal_name_full               Organometallics
_journal_page_first              531
_journal_paper_doi               10.1021/om201125z
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C32 H48 Cl2 O3 Si2'
_chemical_formula_weight         607.78
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                65.406(2)
_cell_angle_beta                 67.296(2)
_cell_angle_gamma                82.180(2)
_cell_formula_units_Z            2
_cell_length_a                   12.7728(12)
_cell_length_b                   12.8949(12)
_cell_length_c                   13.2000(12)
_cell_measurement_reflns_used    1298
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      39.132
_cell_measurement_theta_min      4.975
_cell_volume                     1822.9(3)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and 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  0.0402
_diffrn_reflns_av_sigmaI/netI    0.1094
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            9716
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.73
_exptl_absorpt_coefficient_mu    0.271
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68479
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.107
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.285
_exptl_crystal_size_mid          0.266
_exptl_crystal_size_min          0.197
_refine_diff_density_max         0.256
_refine_diff_density_min         -0.172
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.932
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     366
_refine_ls_number_reflns         6697
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.1374
_refine_ls_R_factor_gt           0.0615
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 [0.00000+1.00000exp(2.00(sin\q/\l)^2^)]/ 
   [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0703P)^2^+0.0000sin\q/\l] 
 where P = 0.33333Fo^2^ + 0.66667Fc^2^ 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1437
_refine_ls_wR_factor_ref         0.1743
_reflns_number_gt                2646
_reflns_number_total             6697
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om201125z_si_002.cif
_cod_data_source_block           cd201485_(compound_syn-5b,ethanol_adduct)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4068126