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_7049865
_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 H20 F20 Mg N2 O2'
_chemical_formula_sum            'C32 H20 F20 Mg N2 O2'
_chemical_formula_weight         868.81
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_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                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.9330(3)
_cell_length_b                   10.43410(10)
_cell_length_c                   11.29390(10)
_cell_measurement_reflns_used    27171
_cell_measurement_temperature    99.98(19)
_cell_measurement_theta_max      72.7890
_cell_measurement_theta_min      4.4750
_cell_volume                     3409.51(6)
_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      99.98(19)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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    -96.00  -2.00   1.00    1.00    --  -41.15 125.00-150.00   94
  2  \w    -96.00  -2.00   1.00    1.00    --  -41.15 125.00 -30.00   94
  3  \w   -114.00 -65.00   1.00    1.00    --  -41.15-137.00-156.00   49
  4  \w   -115.00 -17.00   1.00    1.00    --  -41.15 -38.00 120.00   98
  5  \w   -115.00 -17.00   1.00    1.00    --  -41.15 -38.00  60.00   98
  6  \w      1.00  82.00   1.00    1.00    --   41.15 -99.00-150.00   81
  7  \w     76.00 177.00   1.00    3.00    --  104.96  61.00-180.00  101
  8  \w     94.00 178.00   1.00    3.00    --  104.96 125.00   0.00   84
  9  \w     79.00 178.00   1.00    3.00    --  104.96  45.00 150.00   99
 10  \w     72.00 178.00   1.00    3.00    --  104.96  77.00  90.00  106
 11  \w     32.00 131.00   1.00    3.00    --  104.96 -45.00 -90.00   99
 12  \w     72.00 178.00   1.00    3.00    --  104.96  77.00 150.00  106
 13  \w     76.00 177.00   1.00    3.00    --  104.96  61.00 150.00  101
 14  \w     32.00 121.00   1.00    3.00    --  104.96-125.00-150.00   89
 15  \w     76.00 177.00   1.00    3.00    --  104.96  61.00  60.00  101
 16  \w     76.00 149.00   1.00    3.00    --  104.96  61.00 120.00   73
 17  \w     72.00  99.00   1.00    3.00    --  104.96  77.00 120.00   27
 18  \w     76.00 103.00   1.00    3.00    --  104.96  61.00  90.00   27
 19  \w     79.00 115.00   1.00    3.00    --  104.96  45.00-180.00   36
 20  \w    134.00 161.00   1.00    3.00    --  104.96 125.00-180.00   27
 21  \w     95.00 157.00   1.00    3.00    --  104.96 125.00 -30.00   62
 22  \w     80.00 156.00   1.00    3.00    --  104.96  45.00 120.00   76
 23  \w     70.00 177.00   1.00    3.00    --  104.96  15.00 -30.00  107
;
_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      0.0250912000
_diffrn_orient_matrix_UB_12      -0.0994873000
_diffrn_orient_matrix_UB_13      0.0775131000
_diffrn_orient_matrix_UB_21      -0.0183055000
_diffrn_orient_matrix_UB_22      0.0669153000
_diffrn_orient_matrix_UB_23      0.1122779000
_diffrn_orient_matrix_UB_31      -0.0432382000
_diffrn_orient_matrix_UB_32      -0.0861617000
_diffrn_orient_matrix_UB_33      -0.0026381000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0392
_diffrn_reflns_av_unetI/netI     0.0246
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            38139
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.940
_diffrn_reflns_theta_min         3.055
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.808
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.599
_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    1.693
_exptl_crystal_description       plank
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.149
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.270
_refine_diff_density_rms         0.052
_refine_ls_abs_structure_details
;
 Flack x determined using 2922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.001(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     518
_refine_ls_number_reflns         6590
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0309
_refine_ls_R_factor_gt           0.0305
_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^)+(0.0616P)^2^+0.1634P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0789
_refine_ls_wR_factor_ref         0.0794
_reflns_Friedel_coverage         0.849
_reflns_Friedel_fraction_full    0.963
_reflns_Friedel_fraction_max     0.942
_reflns_number_gt                6500
_reflns_number_total             6590
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj180313a
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_database_code               7049865
_shelx_shelxl_version_number     2016/6
_chemical_oxdiff_formula         'C H N F O Mg'
_reflns_odcompleteness_completeness 99.97
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C31(H31A,H31B), C27(H27A,H27B), C25(H25A,H25B), C29(H29A,H29B)
2.b Idealised Me refined as rotating group:
 C32(H32A,H32B,H32C), C30(H30A,H30B,H30C), C28(H28A,H28B,H28C), C26(H26A,H26B,
 H26C)
;
_olex2_date_sample_data_collection 2018-03-13
_olex2_submission_original_sample_id hasj180313a
_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 1.453
_oxdiff_exptl_absorpt_empirical_full_min 0.766