Rare-Earth-Metal-Catalyzed Addition of Terminal Monoalkynes and Dialkynes with Aryl-Substituted Symmetrical or Unsymmetrical Carbodiimides
Zhang, Fangjun; Zhang, Jie; Zhang, Yin; Hong, Jianquan; Zhou, Xigeng; Organometallics 33 (2014) 6186–; doi:10.1021/om5008665

data_4084507
_publ_section_title
;
 Rare-Earth-Metal-Catalyzed Addition of Terminal Monoalkynes and Dialkynes
 with Aryl-Substituted Symmetrical or Unsymmetrical Carbodiimides
;
_journal_issue                   21
_journal_name_full               Organometallics
_journal_page_first              6186
_journal_paper_doi               10.1021/om5008665
_journal_volume                  33
_journal_year                    2014
_chemical_formula_sum            'C27 H26 Cl2 N2'
_chemical_formula_weight         449.40
_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                104.480(5)
_cell_angle_beta                 107.959(5)
_cell_angle_gamma                105.150(5)
_cell_formula_units_Z            2
_cell_length_a                   8.610(4)
_cell_length_b                   12.078(5)
_cell_length_c                   13.503(6)
_cell_measurement_reflns_used    1931
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      22.18
_cell_measurement_theta_min      2.67
_cell_volume                     1202.9(9)
_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 0.969
_diffrn_measured_fraction_theta_max 0.969
_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  0.0559
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_diffrn_reflns_limit_h_max       10
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_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            5352
_diffrn_reflns_theta_full        25.60
_diffrn_reflns_theta_max         25.60
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    0.286
_exptl_absorpt_correction_T_max  0.9775
_exptl_absorpt_correction_T_min  0.9319
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.417
_refine_diff_density_min         -0.447
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.019(5)
_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   1.002
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     281
_refine_ls_number_reflns         4391
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.002
_refine_ls_R_factor_all          0.1091
_refine_ls_R_factor_gt           0.0767
_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^)+(0.1248P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2058
_refine_ls_wR_factor_ref         0.2198
_reflns_number_gt                2431
_reflns_number_total             4391
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5008665_si_002.cif
_cod_data_source_block           a40403a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/home/saulius/struct/COD-crude-data--automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2827 2014-09-09 07:05:25Z andrius 

 Adding full bibliography for 4084505--4084509.cif.
;
_cod_original_cell_volume        1202.9(8)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4084507