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_1548755
_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         'C34 H33 F4 Mg N3, 0.25(C6 H14)'
_chemical_formula_sum            'C35.5 H36.5 F4 Mg N3'
_chemical_formula_weight         605.48
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -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                83.738(4)
_cell_angle_beta                 85.661(4)
_cell_angle_gamma                88.935(4)
_cell_formula_units_Z            4
_cell_length_a                   11.8799(7)
_cell_length_b                   16.0457(8)
_cell_length_c                   17.2413(8)
_cell_measurement_reflns_used    4018
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      72.8160
_cell_measurement_theta_min      3.5530
_cell_volume                     3257.4(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 10.4115
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.945
_diffrn_measurement_device_type  'Agilent Xcalibur PX Ultra A'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0397
_diffrn_reflns_av_unetI/netI     0.0743
_diffrn_reflns_Laue_measured_fraction_full 0.984
_diffrn_reflns_Laue_measured_fraction_max 0.945
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            18961
_diffrn_reflns_point_group_measured_fraction_full 0.984
_diffrn_reflns_point_group_measured_fraction_max 0.945
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.836
_diffrn_reflns_theta_min         3.580
_diffrn_source                   'Enhance Ultra (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.957
_exptl_absorpt_correction_T_min  0.886
_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            'Pale yellow'
_exptl_crystal_density_diffrn    1.235
_exptl_crystal_description       shards
_exptl_crystal_F_000             1274
_exptl_crystal_size_max          0.220
_exptl_crystal_size_mid          0.131
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     822
_refine_ls_number_reflns         12455
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0996
_refine_ls_R_factor_gt           0.0640
_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^)+(0.0947P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1646
_refine_ls_wR_factor_ref         0.2005
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7949
_reflns_number_total             12455
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7sc05059c3.cif
_cod_data_source_block           2a-hexane
_cod_depositor_comments
'Adding full bibliography for 1548752--1548762.cif.'
_cod_original_formula_sum        'C35.50 H36.50 F4 Mg N3'
_cod_database_code               1548755
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              60543