Magnesium-halobenzene bonding: mapping the halogen sigma-hole with a Lewis-acidic complex.
Friedrich, Alexander; Pahl, Jürgen; Eyselein, Jonathan; Langer, Jens; van Eikema Hommes, Nico; Görling, Andreas; Harder, Sjoerd; Chemical science 12 (2020) 2410–2418; doi:10.1039/d0sc06321e

data_1559821
_publ_section_title
;
 Magnesium-halobenzene bonding: mapping the halogen sigma-hole with a
 Lewis-acidic complex.
;
_journal_issue                   7
_journal_name_full               'Chemical science'
_journal_page_first              2410
_journal_page_last               2418
_journal_paper_doi               10.1039/d0sc06321e
_journal_volume                  12
_journal_year                    2020
_chemical_formula_moiety         'C47 H56 F3 Mg N2, B C24 F20'
_chemical_formula_sum            'C71 H56 B F23 Mg N2'
_chemical_formula_weight         1409.29
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-30
_audit_creation_method
;
Olex2 1.3
(compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145)
;
_audit_update_record
;
2020-11-06 deposited with the CCDC.	2020-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                102.494(3)
_cell_angle_beta                 106.268(2)
_cell_angle_gamma                96.734(2)
_cell_formula_units_Z            2
_cell_length_a                   12.2177(3)
_cell_length_b                   15.9583(5)
_cell_length_c                   17.8965(5)
_cell_measurement_reflns_used    10541
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      73.3680
_cell_measurement_theta_min      3.8200
_cell_volume                     3210.89(17)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.956
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -33.00  27.00   1.00    1.00    --  -41.69  57.00 120.00   60
  2  \w    -96.00  -5.00   1.00    1.00    --  -41.69 125.00 -30.00   91
  3  \w    -92.00 -10.00   1.00    1.00    --  -41.69 -19.00-120.00   82
  4  \w   -114.00 -20.00   1.00    1.00    --  -41.69 -38.00-180.00   94
  5  \w     62.00 135.00   1.00    2.00    --  106.00 -77.00 -30.00   73
  6  \w     82.00 150.00   1.00    2.00    --  106.00  30.00  90.00   68
  7  \w     41.00 130.00   1.00    2.00    --  106.00 -45.00 -90.00   89
  8  \w     79.00 119.00   1.00    2.00    --  106.00 -30.00-180.00   40
  9  \w     33.00  69.00   1.00    2.00    --  106.00 -30.00-180.00   36
 10  \w     30.00 109.00   1.00    2.00    --  106.00 -94.00 -90.00   79
 11  \w     34.00 146.00   1.00    2.00    --  106.00 -15.00  60.00  112
 12  \w     36.00 116.00   1.00    2.00    --  106.00 -61.00 120.00   80
 13  \w     25.00 109.00   1.00    2.00    --  106.00 -94.00 120.00   84
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0764678000
_diffrn_orient_matrix_UB_12      -0.0468508000
_diffrn_orient_matrix_UB_13      -0.0440060000
_diffrn_orient_matrix_UB_21      -0.0205536000
_diffrn_orient_matrix_UB_22      -0.0786648000
_diffrn_orient_matrix_UB_23      0.0346401000
_diffrn_orient_matrix_UB_31      -0.1078340000
_diffrn_orient_matrix_UB_32      -0.0419410000
_diffrn_orient_matrix_UB_33      -0.0741234000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0420
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.956
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            20340
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.956
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.650
_diffrn_reflns_theta_min         2.889
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.637
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.458
_exptl_crystal_description       block
_exptl_crystal_F_000             1440
_exptl_crystal_size_max          0.265
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.182
_refine_diff_density_max         0.359
_refine_diff_density_min         -0.291
_refine_diff_density_rms         0.050
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     923
_refine_ls_number_reflns         12406
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0462
_refine_ls_R_factor_gt           0.0403
_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^)+(0.0433P)^2^+1.4233P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1020
_refine_ls_wR_factor_ref         0.1069
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10945
_reflns_number_total             12406
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06321e2.cif
_cod_data_source_block           hasj160111a
_cod_depositor_comments
;Adding full bibliography for 1559817--1559822.cif.

 Adding full bibliography for 1559817--1559822.cif.
;
_cod_original_cell_volume        3210.89(16)
_cod_database_code               1559821
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C71H56BF23MgN2
_reflns_odcompleteness_completeness 99.02
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C17-C15 \\sim C15A-C17A \\sim C15A-C16A \\sim C16-C15
 with sigma of 0.02
 C15-C11 \\sim C15A-C11
 with sigma of 0.02
3. Others
 Sof(C15A)=Sof(H15A)=Sof(C16A)=Sof(H16d)=Sof(H16e)=Sof(H16f)=Sof(C17A)=
 Sof(H17d)=Sof(H17e)=Sof(H17f)=1-FVAR(1)
 Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16a)=Sof(H16b)=Sof(H16c)=Sof(C17)=Sof(H17a)=
 Sof(H17b)=Sof(H17c)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C24(H24), C27(H27), C15(H15), C15A(H15A)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C31(H31),
 C32(H32), C33(H33), C34(H34), C35(H35), C37(H37), C38(H38), C39(H39), C40(H40),
  C41(H41), C43(H43), C44(H44), C45(H45), C46(H46), C47(H47)
4.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C13(H13a,H13b,H13c), C14(H14a,H14b,H14c),
 C25(H25a,H25b,H25c), C26(H26a,H26b,H26c), C28(H28a,H28b,H28c), C29(H29a,H29b,
 H29c), C16(H16a,H16b,H16c), C17(H17a,H17b,H17c), C16A(H16d,H16e,H16f),
 C17A(H17d,H17e,H17f)
;
_shelx_res_checksum              87895
_olex2_date_sample_data_collection 2016-01-11
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.263
_oxdiff_exptl_absorpt_empirical_full_min 0.786