Lewis acidic alkaline earth metal complexes with a perfluorinated diphenylamide ligand.
Fischer, Christian A.; Rösch, Andreas; Elsen, Holger; Ballmann, Gerd; Wiesinger, Michael; Langer, Jens; Färber, Christian; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 48 (2019) 6757–6766; doi:10.1039/c9dt01272a

data_7049867
_publ_section_title
;
 Lewis acidic alkaline earth metal complexes with a perfluorinated
 diphenylamide ligand.
;
_journal_issue                   20
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              6757
_journal_page_last               6766
_journal_paper_doi               10.1039/c9dt01272a
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         '0.25(C144 H144 F80 N16 Si16 Sr8), 2(C6 H6)'
_chemical_formula_sum            'C48 H48 F20 N4 Si4 Sr2'
_chemical_formula_weight         1348.50
_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             2018-12-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                99.6880(10)
_cell_angle_beta                 99.7680(10)
_cell_angle_gamma                102.2650(10)
_cell_formula_units_Z            4
_cell_length_a                   12.5188(2)
_cell_length_b                   20.5028(3)
_cell_length_c                   23.2272(2)
_cell_measurement_reflns_used    43497
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.7100
_cell_measurement_theta_min      3.7630
_cell_volume                     5610.49(14)
_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
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
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)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.0
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details
;
  1 omega  -69.00   32.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471   57.0000  -90.0000 101

  2 omega  -66.00   33.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471   38.0000  150.0000 99

  3 omega -115.00  -17.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  -38.0000  -30.0000 98

  4 omega   23.00   97.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1471 -125.0000  -60.0000 74

  5 omega   94.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  125.0000 -180.0000 84

  6 omega   29.00  133.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  -30.0000  -30.0000 104

  7 omega   29.00  133.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  -30.0000  150.0000 104

  8 omega   77.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   30.0000  -30.0000 101

  9 omega   29.00  138.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  -77.0000 -180.0000 109

 10 omega   94.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  125.0000  -90.0000 84

 11 omega   77.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   30.0000  150.0000 101

 12 omega   32.00  121.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610 -125.0000  -30.0000 89

 13 omega   33.00  134.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  -61.0000  -60.0000 101

 14 omega   22.00  109.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610  -94.0000  120.0000 87

 15 omega -114.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  -57.0000   90.0000 101

 16 omega  -96.00   -2.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  125.0000  -60.0000 94

 17 omega -114.00  -13.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  -57.0000 -180.0000 101

 18 omega -117.00   -9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  -77.0000  -60.0000 108

 19 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000  -30.0000 101

 20 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000   90.0000 101

 21 omega   77.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   30.0000 -120.0000 101

 22 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000    0.0000 101

 23 omega   77.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   30.0000   60.0000 101

 24 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000 -120.0000 101

 25 omega   79.00  178.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   45.0000 -180.0000 99

 26 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000  -90.0000 101

 27 omega -117.00   -9.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.1471  -77.0000   30.0000 108

 28 omega    9.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1471   77.0000  -60.0000 108

 29 omega    9.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1471   77.0000  120.0000 108

 30 omega    9.00  117.00   1.0000    1.0000
omega____ theta____ kappa____ phi______ frames
    -       41.1471   77.0000 -150.0000 108

 31 omega   76.00  177.00   1.0000    4.0000
omega____ theta____ kappa____ phi______ frames
    -      104.9610   61.0000   60.0000 101
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0422
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            104506
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.951
_diffrn_reflns_theta_min         3.300
_exptl_absorpt_coefficient_mu    4.269
_exptl_absorpt_correction_T_max  0.962
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
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    1.596
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.2785
_exptl_crystal_size_mid          0.2206
_exptl_crystal_size_min          0.1705
_refine_diff_density_max         1.345
_refine_diff_density_min         -0.570
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1460
_refine_ls_number_reflns         21992
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0504
_refine_ls_R_factor_gt           0.0439
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+4.6880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1203
_refine_ls_wR_factor_ref         0.1268
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18858
_reflns_number_total             21992
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj180302a
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_original_cell_volume        5610.49(13)
_cod_database_code               7049867
_shelx_shelxl_version_number     2016/6
_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. Uiso/Uaniso restraints and constraints
C98 \\sim C99 \\sim C100 \\sim C101 \\sim C102 \\sim C97 \\sim C91 \\sim C92
\\sim C93 \\sim C94 \\sim C96 \\sim C95: within 2A with sigma of 0.04 and sigma
for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 C92, C93, C94, C95, C96, C91
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 C98, C99, C100, C101, C102, C97
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(C98)=Sof(H98)=Sof(C99)=Sof(H99)=Sof(C100)=Sof(H100)=Sof(C101)=Sof(H101)=
 Sof(C102)=Sof(H102)=Sof(C97)=Sof(H97)=1-FVAR(1)
 Sof(C92)=Sof(H92)=Sof(C93)=Sof(H93)=Sof(C94)=Sof(H94)=Sof(C95)=Sof(H95)=
 Sof(C96)=Sof(H96)=Sof(C91)=Sof(H91)=FVAR(1)
5.a Aromatic/amide H refined with riding coordinates:
 C85(H85), C86(H86), C88(H88), C89(H89), C87(H87), C76(H76), C77(H77),
 C90(H90), C79(H79), C78(H78), C82(H82), C80(H80), C81(H81), C84(H84), C83(H83),
  C73(H73), C75(H75), C74(H74), C92(H92), C93(H93), C94(H94), C95(H95),
 C96(H96), C91(H91), C98(H98), C99(H99), C100(H100), C101(H101), C102(H102),
 C97(H97)
5.b Fitted hexagon refined as free rotating group:
 C92(C93,C94,C95,C96,C91), C98(C99,C100,C101,C102,C97)
5.c Idealised Me refined as rotating group:
 C31(H31A,H31B,H31C), C71(H71A,H71B,H71C), C27(H27A,H27B,H27C), C69(H69A,H69B,
 H69C), C34(H34A,H34B,H34C), C64(H64A,H64B,H64C), C62(H62A,H62B,H62C), C33(H33A,
 H33B,H33C), C66(H66A,H66B,H66C), C29(H29A,H29B,H29C), C70(H70A,H70B,H70C),
 C68(H68A,H68B,H68C), C30(H30A,H30B,H30C), C36(H36A,H36B,H36C), C72(H72A,H72B,
 H72C), C25(H25A,H25B,H25C), C65(H65A,H65B,H65C), C32(H32A,H32B,H32C), C35(H35A,
 H35B,H35C), C28(H28A,H28B,H28C), C63(H63A,H63B,H63C), C67(H67A,H67B,H67C),
 C26(H26A,H26B,H26C), C61(H61A,H61B,H61C)
;
_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
;