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_1540545
_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 Cl Mg N6'
_chemical_formula_weight         522.24
_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                 90.136(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.726(5)
_cell_length_b                   17.928(9)
_cell_length_c                   17.689(9)
_cell_measurement_reflns_used    9890
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      30.47
_cell_measurement_theta_min      2.38
_cell_volume                     3084(3)
_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 0.968
_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  0.0626
_diffrn_reflns_av_unetI/netI     0.0690
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.968
_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            50136
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.539
_diffrn_reflns_theta_min         1.136
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.7461
_exptl_absorpt_correction_T_min  0.6259
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.125
_exptl_crystal_description       plate
_exptl_crystal_F_000             1124
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.057
_refine_ls_abs_structure_details
; 
 Flack x determined using 6363 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     674
_refine_ls_number_reflns         18702
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0541
_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^)+(0.0804P)^2^+0.5193P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1405
_refine_ls_wR_factor_ref         0.1531
_reflns_Friedel_coverage         0.931
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.955
_reflns_number_gt                15837
_reflns_number_total             18702
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5sc03504j2.cif
_cod_data_source_block           tpmgcls10d
_cod_depositor_comments
'Adding full bibliography for 1540545--1540548.cif.'
_cod_database_code               1540545
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.949
_shelx_estimated_absorpt_t_max   0.993
_shelx_res_checksum              17567