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_7049864
_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 F20 Mg2 N4 Si4'
_chemical_formula_sum            'C36 H36 F20 Mg2 N4 Si4'
_chemical_formula_weight         1065.67
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_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                 111.787(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.7023(3)
_cell_length_b                   15.6263(3)
_cell_length_c                   13.0643(3)
_cell_measurement_reflns_used    4181
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.3990
_cell_measurement_theta_min      4.5950
_cell_volume                     2218.34(10)
_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    -67.00  29.00   1.00    1.00    --  -41.33  57.00  60.00   96
  2  \w     46.00  97.00   1.00    1.00    --   41.33-125.00-120.00   51
  3  \w     24.00 105.00   1.00    1.50    --  106.54 -94.00-120.00   81
  4  \w     40.00 135.00   1.00    1.50    --  106.54 -30.00-180.00   95
  5  \w     85.00 152.00   1.00    1.50    --  106.54  45.00-150.00   67
  6  \w     33.00 149.00   1.00    1.50    --  106.54 -15.00   0.00  116
  7  \w   -116.00 -30.00   1.00    1.00    --  -41.33 -38.00 120.00   86
;
_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      -0.1352672000
_diffrn_orient_matrix_UB_12      0.0091636000
_diffrn_orient_matrix_UB_13      -0.0114308000
_diffrn_orient_matrix_UB_21      0.0288126000
_diffrn_orient_matrix_UB_22      -0.0483889000
_diffrn_orient_matrix_UB_23      0.1093664000
_diffrn_orient_matrix_UB_31      0.0310583000
_diffrn_orient_matrix_UB_32      0.0855055000
_diffrn_orient_matrix_UB_33      0.0632798000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0225
_diffrn_reflns_av_unetI/netI     0.0326
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7362
_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         68.095
_diffrn_reflns_theta_min         4.339
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    2.616
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.602
_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    1.595
_exptl_crystal_description       block
_exptl_crystal_F_000             1080
_exptl_crystal_size_max          0.242
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.147
_refine_diff_density_max         0.323
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.062
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     304
_refine_ls_number_reflns         4040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.0416
_refine_ls_R_factor_gt           0.0366
_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^)+(0.0611P)^2^+0.6963P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1001
_refine_ls_wR_factor_ref         0.1052
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3588
_reflns_number_total             4040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9dt01272a2.cif
_cod_data_source_block           hasj170503a
_cod_depositor_comments
'Adding full bibliography for 7049859--7049867.cif.'
_cod_database_code               7049864
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg Si F'
_reflns_odcompleteness_completeness 99.41
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_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), C17(H17A,H17B,H17C), C18(H18A,H18B,
 H18C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_olex2_date_sample_data_collection 2017-05-03
_olex2_submission_original_sample_id hasj170503a
_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 1.539
_oxdiff_exptl_absorpt_empirical_full_min 0.714