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_7124484
_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         'B C24 F20, C29 H43 N2'
_chemical_formula_sum            'C53 H43 B F20 N2'
_chemical_formula_weight         1098.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_date             2018-04-13
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Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
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_audit_update_record
;
2018-06-07 deposited with the CCDC.
2018-06-12 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.9705(13)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.73722(14)
_cell_length_b                   32.4655(4)
_cell_length_c                   14.61307(20)
_cell_measurement_reflns_used    9426
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3000
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_cell_volume                     5000.87(11)
_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
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CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
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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)'
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_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_environment      air
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_diffrn_detector                 'CCD plate'
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_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_details
;
  1 omega  -50.00   30.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   38.0000  -30.0000 80

  2 omega  -73.00   28.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.8784   77.0000   30.0000 101

  3 omega   51.00  121.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000  -30.0000 70

  4 omega   83.00  109.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   90.0000 26

  5 omega   35.00   98.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  120.0000 63

  6 omega   86.00  177.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   45.0000   30.0000 91

  7 omega  103.00  176.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  125.0000 -180.0000 73

  8 omega   32.00   87.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -30.0000  -90.0000 55

  9 omega   25.00   57.00   1.0000    6.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -94.0000   90.0000 32
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
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_diffrn_orient_matrix_UB_11      -0.0195166000
_diffrn_orient_matrix_UB_12      0.0464698000
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_diffrn_orient_matrix_UB_21      -0.0639900000
_diffrn_orient_matrix_UB_22      -0.0093213000
_diffrn_orient_matrix_UB_23      0.0834776000
_diffrn_orient_matrix_UB_31      0.1300243000
_diffrn_orient_matrix_UB_32      0.0023806000
_diffrn_orient_matrix_UB_33      0.0661188000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0409
_diffrn_reflns_av_unetI/netI     0.0524
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -38
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            17824
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.117
_diffrn_reflns_theta_min         3.368
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.211
_exptl_absorpt_correction_T_max  0.989
_exptl_absorpt_correction_T_min  0.960
_exptl_absorpt_correction_type   gaussian
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;
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    1.459
_exptl_crystal_description       block
_exptl_crystal_F_000             2240
_exptl_crystal_size_max          0.3596
_exptl_crystal_size_mid          0.1036
_exptl_crystal_size_min          0.0656
_refine_diff_density_max         0.358
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_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         9060
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.049
_refine_ls_R_factor_all          0.0504
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_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^)+(0.0640P)^2^+0.7110P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1179
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7872
_reflns_number_total             9060
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj151027a
_cod_original_cell_volume        5000.86(12)
_cod_database_code               7124484
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F Cl O'
_reflns_odcompleteness_completeness 99.06
_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:
 C15(H15), C27(H27), C24(H24), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C9(H9), C20(H20), C22(H22), C21(H21)
2.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C17(H17A,H17B,H17C), C16(H16A,H16B,H16C),
 C26(H26A,H26B,H26C), C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C13(H13A,H13B,
 H13C), C25(H25A,H25B,H25C), C14(H14A,H14B,H14C)
;
_olex2_date_sample_data_collection 2015-10-27
_olex2_submission_special_instructions 'No special instructions were received'