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_7049861
_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         'C32 H16 F20 Mg N2 O2'
_chemical_formula_sum            'C32 H16 F20 Mg N2 O2'
_chemical_formula_weight         864.78
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2017-06-22
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.28 svn.r3405 for OlexSys, GUI svn.r5337)
;
_audit_update_record
;
2019-03-25 deposited with the CCDC.    2019-04-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 100.799(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2647(4)
_cell_length_b                   20.2362(8)
_cell_length_c                   17.7948(7)
_cell_measurement_reflns_used    3425
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4790
_cell_measurement_theta_min      5.0260
_cell_volume                     3277.1(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
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.995
_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    -66.00  33.00   1.00    1.00    --  -41.15  38.00 -90.00   99
  2  \w     27.00  73.00   1.00    1.00    --   41.15 -99.00-150.00   46
  3  \w     46.00  97.00   1.00    1.00    --  106.54 -77.00-120.00   51
  4  \w     23.00  90.00   1.00    1.00    --   41.15-125.00  30.00   67
  5  \w     30.00 132.00   1.00    1.00    --  106.54 -77.00  30.00  102
  6  \w    102.00 173.00   1.00    1.00    --  106.54  45.00-150.00   71
  7  \w     76.00 160.00   1.00    1.00    --  106.54  77.00 -90.00   84
  8  \w     78.00 163.00   1.00    1.00    --  106.54  77.00 150.00   85
;
_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      -0.0741269000
_diffrn_orient_matrix_UB_12      0.0002814000
_diffrn_orient_matrix_UB_13      -0.0850477000
_diffrn_orient_matrix_UB_21      -0.0439143000
_diffrn_orient_matrix_UB_22      -0.0728993000
_diffrn_orient_matrix_UB_23      0.0062939000
_diffrn_orient_matrix_UB_31      -0.1456301000
_diffrn_orient_matrix_UB_32      0.0219364000
_diffrn_orient_matrix_UB_33      0.0223055000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0165
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            5622
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.096
_diffrn_reflns_theta_min         4.370
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.881
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.272
_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    1.753
_exptl_crystal_description       block
_exptl_crystal_F_000             1720
_exptl_crystal_size_max          0.446
_exptl_crystal_size_mid          0.39
_exptl_crystal_size_min          0.372
_refine_diff_density_max         0.481
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     258
_refine_ls_number_reflns         2982
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.0440
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0590P)^2^+5.3710P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1090
_refine_ls_wR_factor_ref         0.1112
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2792
_reflns_number_total             2982
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj170517a
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_database_code               7049861
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg Si O F'
_reflns_odcompleteness_completeness 99.51
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C14(H14A,H14B), C16(H16A,H16B), C13(H13A,H13B), C15(H15A,H15B)
;
_olex2_date_sample_data_collection 2017-05-17
_olex2_submission_original_sample_id hasj170517a
_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 1.315
_oxdiff_exptl_absorpt_empirical_full_min 0.711