Synthesis, structure and reactivity of a terminal magnesium fluoride compound, [TpBut,Me]MgF: hydrogen bonding, halogen bonding and C–F bond formation
Rauch, Michael; Ruccolo, Serge; Mester, John Paul; Rong, Yi; Parkin, Gerard; Chem. Sci. 7 (2016) 142–; doi:10.1039/C5SC03504J

data_1540548
_publ_section_title
;
 Synthesis, structure and reactivity of a terminal magnesium fluoride
 compound, [TpBut,Me]MgF: hydrogen bonding, halogen bonding and C--F bond
 formation
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              142
_journal_paper_doi               10.1039/C5SC03504J
_journal_volume                  7
_journal_year                    2016
_chemical_formula_sum            'C27 H43 B Br Mg N6'
_chemical_formula_weight         566.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-09-15 deposited with the CCDC.
2015-10-22 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.132(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.724(4)
_cell_length_b                   18.118(7)
_cell_length_c                   17.751(6)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.38
_cell_volume                     3127(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0714
_diffrn_reflns_av_unetI/netI     0.0870
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            50225
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.946
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.679
_diffrn_reflns_theta_min         1.124
_exptl_absorpt_coefficient_mu    1.359
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.5753
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.204
_exptl_crystal_description       plate
_exptl_crystal_F_000             1196
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.425
_refine_diff_density_min         -0.879
_refine_diff_density_rms         0.099
_refine_ls_abs_structure_details
; 
 Flack x determined using 5309 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.009(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     644
_refine_ls_number_reflns         19088
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0880
_refine_ls_R_factor_gt           0.0653
_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^)+(0.0868P)^2^+2.6730P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1710
_refine_ls_wR_factor_ref         0.1845
_reflns_Friedel_coverage         0.928
_reflns_Friedel_fraction_full    0.997
_reflns_Friedel_fraction_max     0.937
_reflns_number_gt                14749
_reflns_number_total             19088
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03504j2.cif
_cod_data_source_block           tpmgbrs10
_cod_depositor_comments
'Adding full bibliography for 1540545--1540548.cif.'
_cod_database_code               1540548
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.640
_shelx_estimated_absorpt_t_max   0.948
_shelx_res_checksum              5260