Heteroscorpionate Rare-Earth Catalysts for the Hydroalkoxylation/Cyclization of Alkynyl Alcohols
Martínez, Javier; Otero, Antonio; Lara-Sánchez, Agustín; Castro-Osma, José Antonio; Fernández-Baeza, Juan; Sánchez-Barba, Luis F.; Rodríguez, Ana M.; Organometallics 35 (2016) 1802–; doi:10.1021/acs.organomet.6b00203

data_4088577
_publ_section_title
;
 Heteroscorpionate Rare-Earth Catalysts for the
 Hydroalkoxylation/Cyclization of Alkynyl Alcohols
;
_journal_issue                   11
_journal_name_full               Organometallics
_journal_page_first              1802
_journal_paper_doi               10.1021/acs.organomet.6b00203
_journal_volume                  35
_journal_year                    2016
_chemical_formula_moiety         'C48 H75 N12 O3 Y, 1.5(C7 H8)'
_chemical_formula_sum            'C58.5 H87 N12 O3 Y'
_chemical_formula_weight         1095.31
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                86.754(3)
_cell_angle_beta                 77.112(4)
_cell_angle_gamma                67.426(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5220(6)
_cell_length_b                   12.3560(8)
_cell_length_c                   23.3170(15)
_cell_measurement_reflns_used    2465
_cell_measurement_temperature    230(2)
_cell_measurement_theta_max      19.619
_cell_measurement_theta_min      2.933
_cell_volume                     2986.4(3)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      230(2)
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1031
_diffrn_reflns_av_unetI/netI     0.1188
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            32077
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.690
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.486
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_description       prism
_exptl_crystal_F_000             1170
_exptl_crystal_size_max          0.190
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.658
_refine_diff_density_min         -0.926
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.927
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10483
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.927
_refine_ls_R_factor_all          0.1251
_refine_ls_R_factor_gt           0.0659
_refine_ls_shift/su_max          0.036
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0998P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1479
_refine_ls_wR_factor_ref         0.1792
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6313
_reflns_number_total             10483
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om6b00203_si_002.cif
_cod_data_source_block           7
_cod_original_formula_sum        'C58.50 H87 N12 O3 Y'
_cod_database_code               4088577
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.904
_shelxl_version_number           2013-4
_shelx_res_checksum              73715
_shelx_hkl_checksum              70275