Simple ZnEt2 as catalyst in carbodiimide hydroalkynylation: structural and mechanistic studies
Martínez, Antonio; Moreno-Blázquez, Sonia; Rodriguez-Dieguez, Antonio; Ramos, Alberto; Fernandez-Galan, Rafael; Antiñolo, Antonio; CARRILLO-HERMOSILLA, FERNANDO; Dalton Trans.  (2017) –; doi:10.1039/C7DT02700A

data_7044119
_publ_section_title
;
 Simple ZnEt2 as catalyst in carbodiimide hydroalkynylation: structural
 and mechanistic studies
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02700A
_journal_year                    2017
_chemical_formula_moiety         'C24 H29 N3 O'
_chemical_formula_sum            'C24 H29 N3 O'
_chemical_formula_weight         375.50
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_audit_update_record
;
2017-06-06 deposited with the CCDC.
2017-09-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.000(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.241(2)
_cell_length_b                   9.865(2)
_cell_length_c                   19.417(4)
_cell_measurement_reflns_used    1021
_cell_measurement_temperature    290(2)
_cell_measurement_theta_max      19.284
_cell_measurement_theta_min      2.317
_cell_volume                     2148.0(7)
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_diffrn_ambient_temperature      290(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0687
_diffrn_reflns_av_unetI/netI     0.0696
_diffrn_reflns_Laue_measured_fraction_full 0.973
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13445
_diffrn_reflns_point_group_measured_fraction_full 0.973
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.681
_exptl_absorpt_coefficient_mu    0.072
_exptl_absorpt_correction_T_max  0.746
_exptl_absorpt_correction_T_min  0.6764
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.161
_exptl_crystal_description       prism
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.380
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.178
_refine_diff_density_min         -0.176
_refine_diff_density_rms         0.038
_refine_ls_extinction_coef       0.0057(13)
_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   0.948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3777
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.948
_refine_ls_R_factor_all          0.1163
_refine_ls_R_factor_gt           0.0520
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0743P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1234
_refine_ls_wR_factor_ref         0.1517
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1989
_reflns_number_total             3777
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02700a2.cif
_cod_data_source_block           shelx_CCDC1
_cod_original_cell_volume        2147.9(8)
_cod_database_code               7044119
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.988
_shelxl_version_number           2013-4
_shelx_res_checksum              63572