A combined experimental and computational study on the reaction of fluoroarenes with Mg-Mg, Mg-Zn, Mg-Al and Al-Zn bonds.
Bakewell, Clare; Ward, Bryan J.; White, Andrew J. P.; Crimmin, Mark R.; Chemical science 9 (2018) 2348–2356; doi:10.1039/c7sc05059c

data_1548758
_publ_section_title
;
 A combined experimental and computational study on the reaction of
 fluoroarenes with Mg-Mg, Mg-Zn, Mg-Al and Al-Zn bonds.
;
_journal_issue                   8
_journal_name_full               'Chemical science'
_journal_page_first              2348
_journal_page_last               2356
_journal_paper_doi               10.1039/c7sc05059c
_journal_volume                  9
_journal_year                    2018
_chemical_formula_moiety         'C40 H45 F4 N3 Zn, 0.5(C7 H8), 0.5(C6 H14)'
_chemical_formula_sum            'C46.5 H56 F4 N3 Zn'
_chemical_formula_weight         798.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-09-20 deposited with the CCDC.
2018-01-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.230(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.6052(4)
_cell_length_b                   24.2499(5)
_cell_length_c                   23.5838(5)
_cell_measurement_reflns_used    5078
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.5900
_cell_measurement_theta_min      2.7800
_cell_volume                     8722.1(3)
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2014)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 16.0382
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.804
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0171
_diffrn_reflns_av_unetI/netI     0.0348
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.804
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            15428
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.804
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.371
_diffrn_reflns_theta_min         2.438
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.614
_exptl_absorpt_correction_T_max  0.909
_exptl_absorpt_correction_T_min  0.848
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Colourless
_exptl_crystal_density_diffrn    1.216
_exptl_crystal_description       blocks
_exptl_crystal_F_000             3376
_exptl_crystal_size_max          0.54
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.23
_refine_diff_density_max         0.576
_refine_diff_density_min         -0.259
_refine_diff_density_rms         0.056
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     525
_refine_ls_number_reflns         8797
_refine_ls_number_restraints     96
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0685P)^2^+9.6589P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1208
_refine_ls_wR_factor_ref         0.1384
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6650
_reflns_number_total             8797
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05059c3.cif
_cod_data_source_block           3a
_cod_depositor_comments
'Adding full bibliography for 1548752--1548762.cif.'
_cod_original_formula_sum        'C46.50 H56 F4 N3 Zn'
_cod_database_code               1548758
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              24711