Active Iron(II) Catalysts toward gem-Specific Dimerization of Terminal Alkynes
Liang, Qiuming; Sheng, Kai; Salmon, Andrew; Zhou, Vivian Yue; Song, Datong; ACS Catalysis 9 (2018) 810–; doi:10.1021/acscatal.8b03552

data_4515500
_publ_section_title
;
 Active Iron(II) Catalysts toward gem-Specific Dimerization of Terminal
 Alkynes
;
_journal_issue                   2
_journal_name_full               'ACS Catalysis'
_journal_page_first              810
_journal_paper_doi               10.1021/acscatal.8b03552
_journal_volume                  9
_journal_year                    2018
_chemical_formula_sum            'C20 H16 O4'
_chemical_formula_weight         320.33
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'I -2ya'
_space_group_name_H-M_alt        'I 1 a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 94.848(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   6.1010(5)
_cell_length_b                   7.1857(6)
_cell_length_c                   36.046(4)
_cell_measurement_reflns_used    7255
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.574
_cell_measurement_theta_min      2.268
_cell_volume                     1574.6(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker Kappa Apex II'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0667
_diffrn_reflns_av_unetI/netI     0.1236
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            7255
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         2.268
_exptl_absorpt_coefficient_mu    0.094
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6384
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.351
_exptl_crystal_description       plate
_exptl_crystal_F_000             672
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.436
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.066
_refine_ls_abs_structure_details
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     220
_refine_ls_number_reflns         3564
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0668
_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^)+(0.0672P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1589
_reflns_Friedel_coverage         0.998
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.992
_reflns_number_gt                2057
_reflns_number_total             3564
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cs8b03552_si_010.cif
_cod_data_source_block           enyne
_cod_original_sg_symbol_H-M      'I a'
_cod_database_code               4515500
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              44695
_shelx_hkl_checksum              80472