Highly Lewis acidic cationic alkaline earth metal complexes.
Pahl, Jürgen; Brand, Steffen; Elsen, Holger; Harder, Sjoerd; Chemical communications (Cambridge, England) 54 (2018) 8685–8688; doi:10.1039/c8cc04083d

data_7121794
_publ_section_title
;
 Highly Lewis acidic cationic alkaline earth metal complexes.
;
_journal_issue                   63
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              8685
_journal_page_last               8688
_journal_paper_doi               10.1039/c8cc04083d
_journal_volume                  54
_journal_year                    2018
_chemical_formula_moiety         'C59 H47 B F20 Mg N2, C6 H6'
_chemical_formula_sum            'C65 H53 B F20 Mg N2'
_chemical_formula_weight         1277.21
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2015-10-23
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                100.801(2)
_cell_angle_beta                 101.644(2)
_cell_angle_gamma                110.656(3)
_cell_formula_units_Z            2
_cell_length_a                   12.6783(4)
_cell_length_b                   13.1414(4)
_cell_length_c                   19.5127(5)
_cell_measurement_reflns_used    10909
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3990
_cell_measurement_theta_min      3.7280
_cell_volume                     2858.36(17)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      100
_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 0.989
_diffrn_measurement_details
;
  1 omega  -50.00   31.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -150.0000 81

  2 omega  -48.00   -8.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909   38.0000 -180.0000 40

  3 omega  -95.00   -7.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000  -90.0000 88

  4 omega -113.00  -23.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000   30.0000 90

  5 omega   89.00  173.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000  -30.0000 84

  6 omega  108.00  134.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000  120.0000 26

  7 omega   36.00  121.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   30.0000 85

  8 omega   41.00  105.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -61.0000  120.0000 64

  9 omega   31.00   90.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000   60.0000 59

 10 omega   25.00  109.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   90.0000 84

 11 omega   87.00  177.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   30.0000 -120.0000 90

 12 omega   71.00  137.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -77.0000 -180.0000 66

 13 omega   33.00   87.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000 -150.0000 54

 14 omega   95.00  178.00   1.0000    3.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000  150.0000 83
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      -0.0604482000
_diffrn_orient_matrix_UB_12      -0.1257423000
_diffrn_orient_matrix_UB_13      -0.0030104000
_diffrn_orient_matrix_UB_21      0.1098088000
_diffrn_orient_matrix_UB_22      -0.0180503000
_diffrn_orient_matrix_UB_23      -0.0109029000
_diffrn_orient_matrix_UB_31      0.0521304000
_diffrn_orient_matrix_UB_32      0.0302749000
_diffrn_orient_matrix_UB_33      0.0832601000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0235
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            17441
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.116
_diffrn_reflns_theta_min         3.747
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.248
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.284
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.484
_exptl_crystal_description       block
_exptl_crystal_F_000             1308
_exptl_crystal_size_max          0.2777
_exptl_crystal_size_mid          0.1663
_exptl_crystal_size_min          0.0823
_refine_diff_density_max         0.778
_refine_diff_density_min         -0.288
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         10342
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0401
_refine_ls_R_factor_gt           0.0365
_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^)+(0.0480P)^2^+1.0980P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0931
_refine_ls_wR_factor_ref         0.0963
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9384
_reflns_number_total             10342
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj150313b
_cod_depositor_comments
'Adding full bibliography for 7121792--7121797.cif.'
_cod_original_cell_volume        2858.37(14)
_cod_database_code               7121794
_chemical_oxdiff_formula         'C H N B F Mg Cl'
_reflns_odcompleteness_completeness 98.96
_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.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C60(H60),
 C61(H61), C62(H62), C63(H63), C64(H64), C65(H65)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2015-03-13
_olex2_submission_special_instructions 'No special instructions were received'