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_1559822
_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 I Mg N2, B C24 F20'
_chemical_formula_sum            'C65 H58 B F20 I Mg N2'
_chemical_formula_weight         1409.15
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-10-15
_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                 102.692(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.7237(5)
_cell_length_b                   18.0226(4)
_cell_length_c                   18.7649(5)
_cell_measurement_reflns_used    16766
_cell_measurement_temperature    100.02(16)
_cell_measurement_theta_max      29.2140
_cell_measurement_theta_min      2.9980
_cell_volume                     6177.5(3)
_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 2014/7 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.02(16)
_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 0.864
_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    -16.00  85.00   1.00   75.00    --   12.17  57.00 150.00  101
  2  \w    -16.00  85.00   1.00   75.00    --   12.17  57.00-120.00  101
  3  \w    -15.00  41.00   1.00   75.00    --   12.17 -99.00 120.00   56
;
_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      -0.0322704000
_diffrn_orient_matrix_UB_12      -0.0011093000
_diffrn_orient_matrix_UB_13      -0.0280645000
_diffrn_orient_matrix_UB_21      0.0215979000
_diffrn_orient_matrix_UB_22      -0.0007009000
_diffrn_orient_matrix_UB_23      -0.0266621000
_diffrn_orient_matrix_UB_31      0.0005455000
_diffrn_orient_matrix_UB_32      -0.0393460000
_diffrn_orient_matrix_UB_33      0.0012693000
_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  0.0296
_diffrn_reflns_av_unetI/netI     0.0393
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.864
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42831
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.864
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.728
_diffrn_reflns_theta_min         2.260
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.632
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.883
_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    1.515
_exptl_crystal_description       cube
_exptl_crystal_F_000             2848
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.123
_exptl_crystal_size_min          0.067
_refine_diff_density_max         0.588
_refine_diff_density_min         -0.889
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     825
_refine_ls_number_reflns         15163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0388
_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^)+(0.0359P)^2^+5.4222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0844
_refine_ls_wR_factor_ref         0.0927
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11957
_reflns_number_total             15163
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0sc06321e2.cif
_cod_data_source_block           hasj191021a
_cod_depositor_comments
;Adding full bibliography for 1559817--1559822.cif.

 Adding full bibliography for 1559817--1559822.cif.
;
_cod_database_code               1559822
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         C65H58BF20IMgN2
_shelx_estimated_absorpt_t_max   0.959
_shelx_estimated_absorpt_t_min   0.897
_reflns_odcompleteness_completeness 99.89
_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:
 C18(H18), C30(H30), C33(H33), C21(H21)
2.b Aromatic/amide H refined with riding coordinates:
 C14(H14), C26(H26), C27(H27), C38(H38), C28(H28), C4(H4), C36(H36), C41(H41),
 C15(H15), C39(H39), C16(H16), C40(H40)
2.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C22(H22A,H22B,H22C), C19(H19A,H19B,H19C), C7(H7A,H7B,
 H7C), C11(H11A,H11B,H11C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C9(H9A,
 H9B,H9C), C32(H32A,H32B,H32C), C34(H34A,H34B,H34C), C1(H1A,H1B,H1C), C35(H35A,
 H35B,H35C), C23(H23A,H23B,H23C), C8(H8A,H8B,H8C)
;
_olex2_date_sample_data_collection 2019-10-21
_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 1.179
_oxdiff_exptl_absorpt_empirical_full_min 0.865