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_1559818
_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         'C41 H58 Br Mg N2, B C24 F20'
_chemical_formula_sum            'C65 H58 B Br F20 Mg N2'
_chemical_formula_weight         1362.16
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_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                90
_cell_angle_beta                 102.9937(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6127(3)
_cell_length_b                   17.9643(2)
_cell_length_c                   18.7424(3)
_cell_measurement_reflns_used    14433
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      73.2500
_cell_measurement_theta_min      3.4400
_cell_volume                     6106.32(16)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.957
_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    -59.00  31.00   1.00    1.00    --  -41.69  38.00 -30.00   90
  2  \w    -59.00  30.00   1.00    1.00    --  -41.69  38.00-150.00   89
  3  \w     39.00 129.00   1.00    5.00    --  105.04 -30.00 -30.00   90
  4  \w    146.00 172.00   1.00    5.00    --  105.04  15.00  60.00   26
  5  \w     74.00 177.00   1.00    5.00    --  105.04  77.00 120.00  103
  6  \w     66.00 143.00   1.00    5.00    --  105.04  15.00  60.00   77
  7  \w     34.00 129.00   1.00    5.00    --  105.04 -45.00 120.00   95
;
_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      0.0207596000
_diffrn_orient_matrix_UB_12      0.0619902000
_diffrn_orient_matrix_UB_13      0.0577645000
_diffrn_orient_matrix_UB_21      0.0794281000
_diffrn_orient_matrix_UB_22      0.0000916000
_diffrn_orient_matrix_UB_23      -0.0115206000
_diffrn_orient_matrix_UB_31      -0.0220183000
_diffrn_orient_matrix_UB_32      0.0591124000
_diffrn_orient_matrix_UB_33      -0.0604596000
_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  0.0176
_diffrn_reflns_av_unetI/netI     0.0229
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.957
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            21763
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.957
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.194
_diffrn_reflns_theta_min         3.451
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.942
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.624
_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    1.482
_exptl_crystal_description       block
_exptl_crystal_F_000             2776
_exptl_crystal_size_max          0.339
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.16
_refine_diff_density_max         0.465
_refine_diff_density_min         -0.611
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         11715
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0321
_refine_ls_R_factor_gt           0.0298
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.0214P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0735
_refine_ls_wR_factor_ref         0.0751
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10944
_reflns_number_total             11715
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06321e2.cif
_cod_data_source_block           hasj180510a
_cod_depositor_comments
;Adding full bibliography for 1559817--1559822.cif.

 Adding full bibliography for 1559817--1559822.cif.
;
_cod_original_cell_volume        6106.31(15)
_cod_database_code               1559818
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C65H58BBrF20MgN2
_reflns_odcompleteness_completeness 99.01
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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.a Ternary CH refined with riding coordinates:
 C18(H18), C21(H21), C30(H30), C33(H33)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C14(H14), C15(H15), C16(H16), C26(H26), C27(H27), C28(H28), C37(H37),
 C38(H38), C39(H39), C40(H40), C41(H41)
2.c Idealised Me refined as rotating group:
 C2(H2a,H2b,H2c), C3(H3a,H3b,H3c), C4(H4a,H4b,H4c), C9(H9a,H9b,H9c), C10(H10a,
 H10b,H10c), C11(H11a,H11b,H11c), C19(H19a,H19b,H19c), C20(H20a,H20b,H20c),
 C22(H22a,H22b,H22c), C23(H23a,H23b,H23c), C31(H31a,H31b,H31c), C32(H32a,H32b,
 H32c), C34(H34a,H34b,H34c), C35(H35a,H35b,H35c)
;
_shelx_res_checksum              68372
_olex2_date_sample_data_collection 2018-05-10
_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 1.249
_oxdiff_exptl_absorpt_empirical_full_min 0.895