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_7121795
_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 Ca F20 N2, C6 H6'
_chemical_formula_sum            'C65 H53 B Ca F20 N2'
_chemical_formula_weight         1292.98
_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             2018-04-19
_audit_creation_method
;
Olex2 1.2
(compiled 2018.04.03 svn.r3497 for OlexSys, GUI svn.r5486)
;
_audit_update_record
;
2018-05-22 deposited with the CCDC.
2018-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 94.3470(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   15.4894(2)
_cell_length_b                   16.6388(2)
_cell_length_c                   22.8557(3)
_cell_measurement_reflns_used    11340
_cell_measurement_temperature    100.00(19)
_cell_measurement_theta_max      73.1030
_cell_measurement_theta_min      3.8500
_cell_volume                     5873.54(13)
_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(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.964
_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    -64.00  31.00   1.00    1.00    --  -41.69  38.00-150.00   95
  2  \w   -114.00 -21.00   1.00    1.00    --  -41.69 -38.00-150.00   93
  3  \w     24.00 108.00   1.00    5.00    --  105.04 -94.00 -60.00   84
  4  \w     83.00 109.00   1.00    5.00    --  105.04 -94.00-180.00   26
  5  \w     35.00 120.00   1.00    5.00    --  105.04 -61.00 -30.00   85
  6  \w     31.00 135.00   1.00    5.00    --  105.04 -15.00  30.00  104
  7  \w    122.00 168.00   1.00    5.00    --  105.04  77.00  30.00   46
  8  \w     26.00  61.00   1.00    5.00    --  105.04 -94.00-180.00   35
;
_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      -0.0886567000
_diffrn_orient_matrix_UB_12      -0.0257371000
_diffrn_orient_matrix_UB_13      -0.0290900000
_diffrn_orient_matrix_UB_21      -0.0217568000
_diffrn_orient_matrix_UB_22      -0.0407706000
_diffrn_orient_matrix_UB_23      0.0576763000
_diffrn_orient_matrix_UB_31      -0.0402417000
_diffrn_orient_matrix_UB_32      0.0789401000
_diffrn_orient_matrix_UB_33      0.0201079000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0503
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.964
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            20692
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.964
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.141
_diffrn_reflns_theta_min         3.289
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.875
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.606
_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    1.462
_exptl_crystal_description       block
_exptl_crystal_F_000             2648
_exptl_crystal_size_max          0.278
_exptl_crystal_size_mid          0.209
_exptl_crystal_size_min          0.088
_refine_diff_density_max         0.602
_refine_diff_density_min         -0.383
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     812
_refine_ls_number_reflns         11345
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.035
_refine_ls_R_factor_all          0.0493
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+1.4160P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1239
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10121
_reflns_number_total             11345
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8cc04083d2.cif
_cod_data_source_block           hasj180418a
_cod_depositor_comments
'Adding full bibliography for 7121792--7121797.cif.'
_cod_database_code               7121795
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Ca B F'
_reflns_odcompleteness_completeness 99.12
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C27(H27), C15(H15), C24(H24), C12(H12)
2.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C32(H32), C33(H33), C34(H34), C63(H63), C21(H21), C30(H30), C31(H31),
 C22(H22), C35(H35), C20(H20), C61(H61), C62(H62), C64(H64), C65(H65), C60(H60),
  C8(H8), C10(H10), C9(H9)
2.c Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C1(H1A,H1B,H1C), C29(H29A,H29B,H29C), C16(H16A,H16B,H16C),
 C28(H28A,H28B,H28C), C25(H25A,H25B,H25C), C13(H13A,H13B,H13C), C17(H17A,H17B,
 H17C), C14(H14A,H14B,H14C), C26(H26A,H26B,H26C)
;
_olex2_date_sample_data_collection 2018-04-18
_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
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.210
_oxdiff_exptl_absorpt_empirical_full_min 0.833