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_7049863
_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         'C36 H36 Ca2 F20 N4 Si4'
_chemical_formula_sum            'C36 H36 Ca2 F20 N4 Si4'
_chemical_formula_weight         1097.21
_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             2018-09-25
_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                63.347(3)
_cell_angle_beta                 83.970(2)
_cell_angle_gamma                89.760(2)
_cell_formula_units_Z            4
_cell_length_a                   8.8864(2)
_cell_length_b                   24.4425(6)
_cell_length_c                   24.5767(7)
_cell_measurement_reflns_used    12307
_cell_measurement_temperature    200.0(1)
_cell_measurement_theta_max      73.5760
_cell_measurement_theta_min      3.5990
_cell_volume                     4739.0(2)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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      200.0(1)
_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 0.959
_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  32.00   1.00    4.50    --  -40.61  57.00   0.00   94
  2  \w    -65.00  34.00   1.00    4.50    --  -40.61  38.00 150.00   99
  3  \w   -109.00 -13.00   1.00    4.50    --  -40.61 -57.00-150.00   96
  4  \w     45.00  97.00   1.00    4.50    --   40.61-125.00-180.00   52
  5  \w     42.00  90.00   1.00   18.00    --  107.07-125.00 150.00   48
  6  \w     35.00 100.00   1.00   18.00    --  107.07-125.00  90.00   65
  7  \w     41.00 127.00   1.00   18.00    --  107.07 -77.00-180.00   86
  8  \w     51.00 117.00   1.00   18.00    --  107.07-125.00  30.00   66
  9  \w     37.00 134.00   1.00   18.00    --  107.07 -30.00-120.00   97
 10  \w     93.00 149.00   1.00   18.00    --  107.07  30.00-150.00   56
 11  \w     81.00 168.00   1.00   18.00    --  107.07  45.00 -90.00   87
 12  \w     80.00 106.00   1.00   18.00    --  107.07  77.00-150.00   26
 13  \w    114.00 175.00   1.00   18.00    --  107.07  77.00-150.00   61
 14  \w     43.00 118.00   1.00   18.00    --  107.07-125.00-180.00   75
 15  \w    114.00 173.00   1.00   18.00    --  107.07  77.00 -60.00   59
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1501546000
_diffrn_orient_matrix_UB_12      0.0153061000
_diffrn_orient_matrix_UB_13      -0.0425314000
_diffrn_orient_matrix_UB_21      0.0317079000
_diffrn_orient_matrix_UB_22      0.0550409000
_diffrn_orient_matrix_UB_23      0.0124452000
_diffrn_orient_matrix_UB_31      0.0831208000
_diffrn_orient_matrix_UB_32      -0.0414867000
_diffrn_orient_matrix_UB_33      0.0549704000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0308
_diffrn_reflns_av_unetI/netI     0.0492
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.959
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            30487
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.959
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.904
_diffrn_reflns_theta_min         3.450
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    4.085
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68420
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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    1.538
_exptl_crystal_description       block
_exptl_crystal_F_000             2224
_exptl_crystal_size_max          0.327
_exptl_crystal_size_mid          0.121
_exptl_crystal_size_min          0.077
_refine_diff_density_max         0.293
_refine_diff_density_min         -0.598
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1213
_refine_ls_number_reflns         18418
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0573
_refine_ls_R_factor_gt           0.0434
_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^)+(0.0584P)^2^+0.1794P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1201
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14521
_reflns_number_total             18418
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj180921b
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_database_code               7049863
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N Ca Si F '
_reflns_odcompleteness_completeness 99.53
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C13(H13a,H13b,H13c), C14(H14a,H14b,H14c), C15(H15a,H15b,H15c), C16(H16a,H16b,
 H16c), C17(H17a,H17b,H17c), C18(H18a,H18b,H18c), C19(H19a,H19b,H19c), C20(H20a,
 H20b,H20c), C21(H21a,H21b,H21c), C22(H22a,H22b,H22c), C23(H23a,H23b,H23c),
 C24(H24a,H24b,H24c), C49(H49a,H49b,H49c), C50(H50a,H50b,H50c), C51(H51a,H51b,
 H51c), C52(H52a,H52b,H52c), C53(H53a,H53b,H53c), C54(H54a,H54b,H54c), C55(H55a,
 H55b,H55c), C56(H56a,H56b,H56c), C57(H57a,H57b,H57c), C58(H58a,H58b,H58c),
 C59(H59a,H59b,H59c), C60(H60a,H60b,H60c)
;
_olex2_date_sample_data_collection 2018-09-21
_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 2.246
_oxdiff_exptl_absorpt_empirical_full_min 0.410