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_7121793
_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 H61 F Mg N2 O P, B C24 F20'
_chemical_formula_sum            'C65 H61 B F21 Mg N2 O P'
_chemical_formula_weight         1351.24
_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             2017-08-16
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5375)
;
_audit_update_record
;
2018-02-06 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                92.793(3)
_cell_angle_beta                 107.979(3)
_cell_angle_gamma                99.369(2)
_cell_formula_units_Z            2
_cell_length_a                   12.6579(4)
_cell_length_b                   15.3343(5)
_cell_length_c                   17.5503(6)
_cell_measurement_reflns_used    16742
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.5670
_cell_measurement_theta_min      3.7050
_cell_volume                     3179.12(19)
_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      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.968
_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   -115.00 -17.00   1.00    1.00    --  -41.15 -38.00  90.00   98
  2  \w    -96.00  -2.00   1.00    1.00    --  -41.15 125.00 -30.00   94
  3  \w   -117.00  -9.00   1.00    1.00    --  -41.15 -77.00-150.00  108
  4  \w      1.00  82.00   1.00    1.00    --   41.15 -99.00 -30.00   81
  5  \w     77.00 178.00   1.00    5.00    --  106.54  61.00 120.00  101
  6  \w     24.00 109.00   1.00    5.00    --  106.54 -94.00-180.00   85
  7  \w     34.00 136.00   1.00    5.00    --  106.54 -61.00  30.00  102
  8  \w     81.00 178.00   1.00    5.00    --  106.54  45.00  90.00   97
  9  \w     81.00 178.00   1.00    5.00    --  106.54  45.00-180.00   97
 10  \w     24.00 109.00   1.00    5.00    --  106.54 -94.00 -90.00   85
 11  \w     33.00 122.00   1.00    5.00    --  106.54-125.00  60.00   89
 12  \w     94.00 178.00   1.00    5.00    --  106.54 125.00  90.00   84
 13  \w     24.00 109.00   1.00    5.00    --  106.54 -94.00  90.00   85
 14  \w     30.00 131.00   1.00    5.00    --  106.54 -30.00 150.00  101
;
_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      -0.0305345000
_diffrn_orient_matrix_UB_12      -0.0090022000
_diffrn_orient_matrix_UB_13      0.0780625000
_diffrn_orient_matrix_UB_21      -0.1265897000
_diffrn_orient_matrix_UB_22      -0.0150614000
_diffrn_orient_matrix_UB_23      -0.0492715000
_diffrn_orient_matrix_UB_31      -0.0031226000
_diffrn_orient_matrix_UB_32      -0.1008793000
_diffrn_orient_matrix_UB_33      -0.0095433000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0219
_diffrn_reflns_av_unetI/netI     0.0288
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.968
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26083
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.968
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.649
_diffrn_reflns_theta_min         3.737
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.417
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.366
_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    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             1388
_exptl_crystal_size_max          0.381
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.102
_refine_diff_density_max         0.564
_refine_diff_density_min         -0.436
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.025
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     842
_refine_ls_number_reflns         12436
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0376
_refine_ls_R_factor_gt           0.0343
_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^)+(0.0460P)^2^+1.0940P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0879
_refine_ls_wR_factor_ref         0.0906
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11353
_reflns_number_total             12436
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj170731a
_cod_depositor_comments
'Adding full bibliography for 7121792--7121797.cif.'
_cod_database_code               7121793
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F O P'
_reflns_odcompleteness_completeness 99.61
_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.a Ternary CH refined with riding coordinates:
 C15(H15), C27(H27), C12(H12), C24(H24)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C30(H30A,H30B), C32(H32A,H32B)
2.c Aromatic/amide H refined with riding coordinates:
 C10(H10), C3(H3), C8(H8), C9(H9), C37(H37), C41(H41), C40(H40), C38(H38),
 C39(H39), C22(H22), C20(H20), C21(H21)
2.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C16(H16A,H16B,H16C), C33(H33A,H33B,H33C), C35(H35A,H35B,
 H35C), C17(H17A,H17B,H17C), C5(H5A,H5B,H5C), C31(H31A,H31B,H31C), C28(H28A,
 H28B,H28C), C14(H14A,H14B,H14C), C13(H13A,H13B,H13C), C29(H29A,H29B,H29C),
 C26(H26A,H26B,H26C), C25(H25A,H25B,H25C)
;
_olex2_date_sample_data_collection 2017-07-31
_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 1.424
_oxdiff_exptl_absorpt_empirical_full_min 0.753