Carboxylation of terminal alkynes with CO2catalyzed by bis(amidate) rare-earth metal amides
Cheng, Hao; Zhao, Bei; Yao, Yingming; Lu, Chengrong; Green Chem. 17 (2015) 1675–; doi:10.1039/C4GC02200A

data_7219094
_publ_section_title
;
 Carboxylation of terminal alkynes with CO2catalyzed by bis(amidate)
 rare-earth metal amides
;
_journal_issue                   3
_journal_name_full               'Green Chem.'
_journal_page_first              1675
_journal_paper_doi               10.1039/C4GC02200A
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C76 H124 N6 O6 Si4 La2, 3(C4 H8 O)'
_chemical_formula_sum            'C88 H148 La2 N6 O9 Si4'
_chemical_formula_weight         1824.30
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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
_audit_update_record
;
2014-07-31 deposited with the CCDC.
2014-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                108.936(2)
_cell_angle_beta                 106.425(2)
_cell_angle_gamma                98.499(2)
_cell_formula_units_Z            1
_cell_length_a                   13.963(2)
_cell_length_b                   14.045(2)
_cell_length_c                   15.374(3)
_cell_measurement_reflns_used    9545
_cell_measurement_temperature    223(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      3.1
_cell_volume                     2638.4(7)
_computing_cell_refinement       CrystalClear
_computing_data_collection       CrystalClear
_computing_data_reduction        CrystalStructure
_computing_publication_material  'CrystalStructure 3.7.0'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_detector_area_resol_mean 14.63
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71075
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0601
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24227
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    0.893
_exptl_absorpt_correction_T_max  0.693
_exptl_absorpt_correction_T_min  0.482
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.148
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.80
_exptl_crystal_size_mid          0.60
_exptl_crystal_size_min          0.40
_refine_diff_density_max         0.738
_refine_diff_density_min         -1.148
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     493
_refine_ls_number_reflns         11850
_refine_ls_number_restraints     70
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0675
_refine_ls_R_factor_gt           0.0564
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0851P)^2^+2.1440P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1586
_refine_ls_wR_factor_ref         0.1682
_reflns_number_gt                10069
_reflns_number_total             11850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c4gc02200a2.cif
_cod_data_source_block           shelxl
_cod_depositor_comments
'Adding full bibliography for 7219093--7219095.cif.'
_cod_original_cell_volume        2638.5(7)
_cod_database_code               7219094