Structural and reactivity insights in Mg–Zn hybrid chemistry: Zn–I exchange and Pd-catalysed cross-coupling applications of aromatic substrates
Bluemke, Tobias D.; Clegg, William; García-Alvarez, Pablo; Kennedy, Alan R.; Koszinowski, Konrad; McCall, Matthew D.; Russo, Luca; Hevia, Eva; Chemical Science 5 (2014) 3552–; doi:10.1039/C4SC01263A

data_1516679
_publ_section_title
;
 Structural and reactivity insights in Mg--Zn hybrid chemistry: Zn--I
 exchange and Pd-catalysed cross-coupling applications of aromatic
 substrates
;
_journal_issue                   9
_journal_name_full               'Chemical Science'
_journal_page_first              3552
_journal_paper_doi               10.1039/C4SC01263A
_journal_volume                  5
_journal_year                    2014
_chemical_formula_moiety         'C24 H48 Mg O6 2+,2 C21 H21 O3 Zn -,C4 H8 O'
_chemical_formula_sum            'C70 H98 Mg O13 Zn2'
_chemical_formula_weight         1302.53
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_symmetry_space_group_name_Hall  'P 4nw 2abw'
_symmetry_space_group_name_H-M   'P 43 21 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.1808(3)
_cell_length_b                   12.1808(3)
_cell_length_c                   44.474(2)
_cell_measurement_reflns_used    3175
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.49
_cell_measurement_theta_min      3.21
_cell_volume                     6598.7(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
;
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL and local programs'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 10.3968
_diffrn_measured_fraction_theta_full 0.796
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction Gemini A Ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0504
_diffrn_reflns_av_unetI/netI     0.0825
_diffrn_reflns_Laue_measured_fraction_full 0.796
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            11087
_diffrn_reflns_point_group_measured_fraction_full 0.789
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         23.245
_diffrn_reflns_theta_min         3.217
_diffrn_source                   'sealed tube with Enhance optics'
_exptl_absorpt_coefficient_mu    0.799
_exptl_absorpt_correction_T_max  0.784
_exptl_absorpt_correction_T_min  0.710
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.52 (release 06-11-2009 CrysAlis171 .NET)
(compiled Nov  6 2009,16:24:50)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.311
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.32
_refine_diff_density_max         0.573
_refine_diff_density_min         -0.252
_refine_diff_density_rms         0.069
_refine_ls_abs_structure_details
;
 Flack x determined using 978 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.032(10)
_refine_ls_extinction_coef       0.0013(8)
_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   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         4726
_refine_ls_number_restraints     1396
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1206P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1729
_refine_ls_wR_factor_ref         0.1841
_reflns_Friedel_coverage         0.679
_reflns_Friedel_fraction_full    0.780
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                3052
_reflns_number_total             4726
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4sc01263a2.cif
_cod_data_source_block           rem538
_cod_depositor_comments
'Adding full bibliography for 1516679--1516680.cif.'
_cod_database_code               1516679
_shelx_estimated_absorpt_t_min   0.710
_shelx_estimated_absorpt_t_max   0.784