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_7121796
_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         'C41 H71 Mg N2 O2 P2, B C24 F20'
_chemical_formula_sum            'C65 H71 B F20 Mg N2 O2 P2'
_chemical_formula_weight         1389.29
_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   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-08-03
_audit_creation_method
;
Olex2 1.2
(compiled 2017.07.20 svn.r3457 for OlexSys, GUI svn.r5370)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                94.761(3)
_cell_angle_beta                 92.981(3)
_cell_angle_gamma                96.921(3)
_cell_formula_units_Z            2
_cell_length_a                   12.9094(5)
_cell_length_b                   15.1447(6)
_cell_length_c                   16.9144(7)
_cell_measurement_reflns_used    10869
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      73.4030
_cell_measurement_theta_min      3.7390
_cell_volume                     3265.1(2)
_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      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.954
_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    -63.00  32.00   1.00    1.00    --  -41.15  57.00 150.00   95
  2  \w    -74.00  28.00   1.00    1.00    --  -41.15  77.00 -90.00  102
  3  \w   -115.00 -17.00   1.00    1.00    --  -41.15 -77.00  30.00   98
  4  \w     32.00 128.00   1.00    1.00    --  106.54 -30.00-120.00   96
  5  \w     72.00 139.00   1.00    1.00    --  106.54 -77.00  30.00   67
  6  \w     86.00 178.00   1.00    1.00    --  106.54  30.00  60.00   92
  7  \w    102.00 175.00   1.00    1.00    --  106.54 125.00   0.00   73
  8  \w     40.00 136.00   1.00    1.00    --  106.54 -61.00 -30.00   96
  9  \w     30.00 133.00   1.00    1.00    --  106.54 -30.00  60.00  103
 10  \w     34.00 122.00   1.00    1.00    --  106.54-125.00-120.00   88
 11  \w     26.00 109.00   1.00    1.00    --  106.54 -94.00 -60.00   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_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0327408000
_diffrn_orient_matrix_UB_12      0.0711614000
_diffrn_orient_matrix_UB_13      -0.0529637000
_diffrn_orient_matrix_UB_21      -0.1002890000
_diffrn_orient_matrix_UB_22      0.0042642000
_diffrn_orient_matrix_UB_23      0.0449697000
_diffrn_orient_matrix_UB_31      0.0581221000
_diffrn_orient_matrix_UB_32      0.0741870000
_diffrn_orient_matrix_UB_33      0.0596542000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0287
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            20397
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.681
_diffrn_reflns_theta_min         2.951
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.606
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.485
_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    1.413
_exptl_crystal_description       block
_exptl_crystal_F_000             1436
_exptl_crystal_size_max          0.281
_exptl_crystal_size_mid          0.218
_exptl_crystal_size_min          0.198
_refine_diff_density_max         0.639
_refine_diff_density_min         -0.403
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.016
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     894
_refine_ls_number_reflns         12574
_refine_ls_number_restraints     29
_refine_ls_restrained_S_all      1.020
_refine_ls_R_factor_all          0.0503
_refine_ls_R_factor_gt           0.0439
_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^)+(0.0622P)^2^+1.5141P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1146
_refine_ls_wR_factor_ref         0.1208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10908
_reflns_number_total             12574
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj170524a
_cod_depositor_comments
'Adding full bibliography for 7121792--7121797.cif.'
_cod_database_code               7121796
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F P'
_reflns_odcompleteness_completeness 99.21
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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. Restrained distances
 P2-C38A \\sim P2-C38
 with sigma of 0.02
 C39A-C38A \\sim C39-C38
 with sigma of 0.02
3. Rigid body (RIGU) restrains
 C38A, P2, C38, C39A, C39, C36
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C41A)=Sof(H41D)=Sof(H41E)=Sof(H41F)=Sof(C40A)=Sof(H40C)=Sof(H40D)=1-FVAR(1)
 Sof(C40)=Sof(H40A)=Sof(H40B)=Sof(C41)=Sof(H41A)=Sof(H41B)=Sof(H41C)=FVAR(1)
 Sof(C38A)=Sof(H38C)=Sof(H38D)=Sof(C39A)=Sof(H39D)=Sof(H39E)=Sof(H39F)=1-FVAR(2)
 Sof(C38)=Sof(H38A)=Sof(H38B)=Sof(C39)=Sof(H39A)=Sof(H39B)=Sof(H39C)=FVAR(2)
5.a Ternary CH refined with riding coordinates:
 C15(H15), C12(H12), C24(H24), C27(H27)
5.b Secondary CH2 refined with riding coordinates:
 C30(H30A,H30B), C34(H34A,H34B), C32(H32A,H32B), C36(H36A,H36B), C40(H40A,
 H40B), C38(H38A,H38B), C40A(H40C,H40D), C38A(H38C,H38D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C10(H10), C9(H9), C20(H20), C22(H22), C21(H21)
5.d Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C35(H35A,H35B,H35C), C16(H16A,H16B,H16C),
 C25(H25A,H25B,H25C), C31(H31A,H31B,H31C), C17(H17A,H17B,H17C), C26(H26A,H26B,
 H26C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C), C33(H33A,H33B,H33C), C28(H28A,
 H28B,H28C), C29(H29A,H29B,H29C), C41(H41A,H41B,H41C), C37(H37A,H37B,H37C),
 C39(H39A,H39B,H39C), C41A(H41D,H41E,H41F), C39A(H39D,H39E,H39F)
;
_olex2_date_sample_data_collection 2017-05-24
_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 1.309
_oxdiff_exptl_absorpt_empirical_full_min 0.806