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_1559817
_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         'C59 H46 B F21 Mg N2'
_chemical_formula_sum            'C59 H46 B F21 Mg N2'
_chemical_formula_weight         1217.10
_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     direct
_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                86.186(3)
_cell_angle_beta                 77.900(3)
_cell_angle_gamma                80.916(3)
_cell_formula_units_Z            2
_cell_length_a                   11.5844(5)
_cell_length_b                   12.7186(5)
_cell_length_c                   19.1320(7)
_cell_measurement_reflns_used    9845
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      29.0780
_cell_measurement_theta_min      2.7080
_cell_volume                     2720.03(19)
_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 (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 0.999
_diffrn_measured_fraction_theta_max 0.848
_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    -40.00  61.00   1.00   90.00    --  -11.70  57.00 120.00  101
  2  \w    -88.00  21.00   1.00   90.00    --  -11.70 -77.00   0.00  109
  3  \w    -20.00  88.00   1.00   90.00    --   12.17  77.00-120.00  108
  4  \w    -62.00  28.00   1.00   90.00    --   12.17 -38.00 -90.00   90
;
_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      -0.0288024000
_diffrn_orient_matrix_UB_12      0.0510261000
_diffrn_orient_matrix_UB_13      0.0118136000
_diffrn_orient_matrix_UB_21      0.0540604000
_diffrn_orient_matrix_UB_22      0.0110085000
_diffrn_orient_matrix_UB_23      0.0077443000
_diffrn_orient_matrix_UB_31      0.0160130000
_diffrn_orient_matrix_UB_32      0.0216479000
_diffrn_orient_matrix_UB_33      -0.0352114000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0326
_diffrn_reflns_av_unetI/netI     0.0514
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.848
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            29754
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.848
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.790
_diffrn_reflns_theta_min         1.985
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.147
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.723
_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    1.486
_exptl_crystal_description       block
_exptl_crystal_F_000             1240
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.137
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.430
_refine_diff_density_min         -0.328
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         13187
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.057
_refine_ls_R_factor_all          0.0828
_refine_ls_R_factor_gt           0.0535
_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^)+(0.0489P)^2^+1.5887P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1172
_refine_ls_wR_factor_ref         0.1324
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9393
_reflns_number_total             13187
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06321e2.cif
_cod_data_source_block           hasj1702012a
_cod_depositor_comments
;Adding full bibliography for 1559817--1559822.cif.

 Adding full bibliography for 1559817--1559822.cif.
;
_cod_original_cell_volume        2720.05(18)
_cod_database_code               1559817
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         C59H46BF21MgN2
_reflns_odcompleteness_completeness 99.91
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_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:
 C24(H24), C15(H15), C27(H27), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C20(H20), C35(H35), C10(H10), C22(H22), C21(H21), C31(H31), C32(H32),
 C34(H34), C33(H33), C9(H9), C8(H8)
2.c Idealised Me refined as rotating group:
 C1(H1a,H1b,H1c), C5(H5a,H5b,H5c), C16(H16a,H16b,H16c), C25(H25a,H25b,H25c),
 C28(H28a,H28b,H28c), C17(H17a,H17b,H17c), C29(H29a,H29b,H29c), C14(H14a,H14b,
 H14c), C13(H13a,H13b,H13c), C26(H26a,H26b,H26c)
;
_shelx_res_checksum              97781
_olex2_date_sample_data_collection 2017-02-12
_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 1.379
_oxdiff_exptl_absorpt_empirical_full_min 0.762