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_7121797
_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 H51 B F20 Mg N2'
_chemical_formula_sum            'C59 H51 B F20 Mg N2'
_chemical_formula_weight         1203.14
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.557(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.3528(6)
_cell_length_b                   20.1560(9)
_cell_length_c                   19.2715(8)
_cell_measurement_reflns_used    11255
_cell_measurement_temperature    99.99(10)
_cell_measurement_theta_max      29.2180
_cell_measurement_theta_min      3.7040
_cell_volume                     5480.8(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)'
_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      N~2~
_diffrn_ambient_temperature      99.99(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.856
_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    -62.00  37.00   1.00   90.00    --   12.17 -38.00-120.00   99
  2  \w     34.00  99.00   1.00   90.00    --   12.17-178.00  90.00   65
  3  \w    -88.00 -19.00   1.00   90.00    --  -11.70 -77.00-180.00   69
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0417817000
_diffrn_orient_matrix_UB_12      -0.0130184000
_diffrn_orient_matrix_UB_13      -0.0094563000
_diffrn_orient_matrix_UB_21      -0.0277560000
_diffrn_orient_matrix_UB_22      -0.0158462000
_diffrn_orient_matrix_UB_23      -0.0296376000
_diffrn_orient_matrix_UB_31      0.0039100000
_diffrn_orient_matrix_UB_32      0.0285973000
_diffrn_orient_matrix_UB_33      -0.0207824000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_unetI/netI     0.0372
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.856
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            33685
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.856
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.841
_diffrn_reflns_theta_min         2.978
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.142
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.683
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.458
_exptl_crystal_description       plate
_exptl_crystal_F_000             2464
_exptl_crystal_size_max          0.347
_exptl_crystal_size_mid          0.187
_exptl_crystal_size_min          0.073
_refine_diff_density_max         0.307
_refine_diff_density_min         -0.297
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     760
_refine_ls_number_reflns         13472
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0600
_refine_ls_R_factor_gt           0.0413
_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^)+(0.0380P)^2^+2.4640P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1001
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10339
_reflns_number_total             13472
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj170216b
_cod_depositor_comments
'Adding full bibliography for 7121792--7121797.cif.'
_cod_database_code               7121797
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F O Cl'
_reflns_odcompleteness_completeness 99.59
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C12(H12), C15(H15)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C20(H20), C22(H22), C21(H21), C10(H10), C9(H9)
2.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C26(H26A,H26B,H26C), C25(H25A,H25B,H25C),
 C29(H29A,H29B,H29C), C28(H28A,H28B,H28C), C17(H17A,H17B,H17C), C35(H35A,H35B,
 H35C), C14(H14A,H14B,H14C), C16(H16A,H16B,H16C), C13(H13A,H13B,H13C), C30(H30A,
 H30B,H30C)
;
_olex2_date_sample_data_collection 2017-02-16
_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 1.262
_oxdiff_exptl_absorpt_empirical_full_min 0.779