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_7049862
_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 Ca F20 N2 O2'
_chemical_formula_sum            'C32 H16 Ca F20 N2 O2'
_chemical_formula_weight         880.55
_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     direct
_audit_creation_date             2018-12-04
_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                 98.013(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2667(2)
_cell_length_b                   20.4436(4)
_cell_length_c                   17.8288(4)
_cell_measurement_reflns_used    5786
_cell_measurement_temperature    100.01(10)
_cell_measurement_theta_max      73.3880
_cell_measurement_theta_min      4.9770
_cell_volume                     3344.59(12)
_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    'SIR2004 (Burla et al.,  2007)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  30.00   1.00    1.00    --  -40.90  57.00  30.00   92
  2  \w     16.00 115.00   1.00    1.00    --   40.90  38.00 150.00   99
  3  \w     89.00 172.00   1.00    3.50    --  106.54  45.00  30.00   83
  4  \w    100.00 178.00   1.00    3.50    --  106.54 125.00 -30.00   78
  5  \w     88.00 130.00   1.00    3.50    --  106.54 -45.00 -60.00   42
  6  \w     71.00 121.00   1.00    3.50    --  106.54-125.00 -30.00   50
  7  \w     60.00 117.00   1.00    3.50    --  106.54 -77.00 -60.00   57
  8  \w     42.00  71.00   1.00    3.50    --  106.54 -45.00 -60.00   29
  9  \w     35.00 124.00   1.00    3.50    --  106.54 -45.00-150.00   89
 10  \w     34.00  60.00   1.00    3.50    --  106.54-125.00 -30.00   26
 11  \w     36.00 134.00   1.00    3.50    --  106.54 -61.00  60.00   98
 12  \w     72.00 121.00   1.00    3.50    --  106.54-125.00 120.00   49
 13  \w     39.00  81.00   1.00    1.00    --   40.90 -99.00 150.00   42
 14  \w     58.00 178.00   1.00    3.50    --  106.54  15.00 150.00  120
 15  \w   -110.00 -16.00   1.00    1.00    --  -40.90 -57.00-120.00   94
;
_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      -0.0438830000
_diffrn_orient_matrix_UB_12      0.0189739000
_diffrn_orient_matrix_UB_13      0.0774023000
_diffrn_orient_matrix_UB_21      -0.1501250000
_diffrn_orient_matrix_UB_22      0.0227512000
_diffrn_orient_matrix_UB_23      -0.0395204000
_diffrn_orient_matrix_UB_31      -0.0611662000
_diffrn_orient_matrix_UB_32      -0.0692143000
_diffrn_orient_matrix_UB_33      0.0082740000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0204
_diffrn_reflns_av_unetI/netI     0.0193
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            9982
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         4.325
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.002
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.427
_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    1.749
_exptl_crystal_description       block
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.353
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.484
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     277
_refine_ls_number_reflns         3066
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0317
_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^)+(0.0425P)^2^+3.3497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0830
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2932
_reflns_number_total             3066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj170427a
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_database_code               7049862
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Ca F O '
_reflns_odcompleteness_completeness 99.78
_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, All C(H,H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C13 \\sim C16A \\sim O1 \\sim C15 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
C13A \\sim C16 \\sim O1 \\sim C15 \\sim C14: within 2A with sigma of 0.04 and
sigma for terminal atoms of 0.08
3. Rigid body (RIGU) restrains
 O1, C13, C14, C15, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
 O1, C13A, C14, C15, C16A
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(H15C)=Sof(H15D)=Sof(H14C)=Sof(H14D)=Sof(C13A)=Sof(H13C)=Sof(H13D)=
 Sof(C16)=Sof(H16C)=Sof(H16D)=1-FVAR(1)
 Sof(H15A)=Sof(H15B)=Sof(H14A)=Sof(H14B)=Sof(C13)=Sof(H13A)=Sof(H13B)=
 Sof(C16A)=Sof(H16A)=Sof(H16B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C15(H15A,H15B), C15(H15C,H15D), C14(H14A,H14B), C14(H14C,H14D), C13(H13A,
 H13B), C16A(H16A,H16B), C13A(H13C,H13D), C16(H16C,H16D)
;
_olex2_date_sample_data_collection 2017-04-27
_olex2_submission_original_sample_id hasj170427a
_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 1.671
_oxdiff_exptl_absorpt_empirical_full_min 0.673