Bulky cationic β-diketiminate magnesium complexes.
Friedrich, Alexander; Pahl, Jürgen; Elsen, Holger; Harder, Sjoerd; Dalton transactions (Cambridge, England : 2003) 48 (2019) 5560–5568; doi:10.1039/c8dt03576h

data_7048343
_publ_section_title
;
 Bulky cationic \b-diketiminate magnesium complexes.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5560
_journal_page_last               5568
_journal_paper_doi               10.1039/c8dt03576h
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C41 H58 Cl Mg N2, B C24 F20'
_chemical_formula_sum            'C65 H58 B Cl F20 Mg N2'
_chemical_formula_weight         1317.70
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2018-05-30
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.18 svn.r3508 for OlexSys, GUI svn.r5497)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.2360(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5500(2)
_cell_length_b                   17.9339(2)
_cell_length_c                   18.7239(2)
_cell_measurement_reflns_used    20945
_cell_measurement_temperature    100
_cell_measurement_theta_max      72.8410
_cell_measurement_theta_min      3.4230
_cell_volume                     6063.48(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    '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 0.998
_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  30.00   94
  2  \w    -69.00  32.00   1.00    1.00    --  -41.15  57.00   0.00  101
  3  \w     32.00 131.00   1.00    4.00    --  104.96 -45.00 -30.00   99
  4  \w     76.00 177.00   1.00    4.00    --  104.96  61.00 -90.00  101
  5  \w     22.00 109.00   1.00    4.00    --  104.96 -94.00   0.00   87
  6  \w     29.00 138.00   1.00    4.00    --  104.96 -77.00 150.00  109
  7  \w     94.00 178.00   1.00    4.00    --  104.96 125.00  90.00   84
  8  \w   -117.00  -9.00   1.00    1.00    --  -41.15 -77.00-120.00  108
  9  \w   -117.00  -9.00   1.00    1.00    --  -41.15 -77.00  30.00  108
 10  \w     52.00 126.00   1.00    4.00    --  104.96  15.00  90.00   74
;
_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      -0.0392050000
_diffrn_orient_matrix_UB_12      0.0762154000
_diffrn_orient_matrix_UB_13      -0.0047655000
_diffrn_orient_matrix_UB_21      0.0668167000
_diffrn_orient_matrix_UB_22      0.0324275000
_diffrn_orient_matrix_UB_23      0.0558694000
_diffrn_orient_matrix_UB_31      0.0358575000
_diffrn_orient_matrix_UB_32      0.0228271000
_diffrn_orient_matrix_UB_33      -0.0631758000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0301
_diffrn_reflns_av_unetI/netI     0.0269
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            33397
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.108
_diffrn_reflns_theta_min         3.457
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.588
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.403
_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    1.443
_exptl_crystal_description       block
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.568
_exptl_crystal_size_mid          0.33
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.589
_refine_diff_density_min         -0.363
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     829
_refine_ls_number_reflns         11056
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0456
_refine_ls_R_factor_gt           0.0427
_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^)+(0.0700P)^2^+2.9420P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1155
_refine_ls_wR_factor_ref         0.1188
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10192
_reflns_number_total             11056
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03576h2.cif
_cod_data_source_block           hasj180405a
_cod_depositor_comments
'Adding full bibliography for 7048343--7048345.cif.'
_cod_database_code               7048343
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg Cl O B F '
_shelx_estimated_absorpt_t_max   0.670
_shelx_estimated_absorpt_t_min   0.466
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C27(H27), C24(H24), C39(H39), C36(H36)
2.b Aromatic/amide H refined with riding coordinates:
 C22(H22), C6(H6), C21(H21), C2(H2), C20(H20), C5(H5), C3(H3), C4(H4),
 C32(H32), C34(H34), C33(H33)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C25(H25A,H25B,H25C), C40(H40A,H40B,H40C), C41(H41A,H41B,
 H41C), C17(H17A,H17B,H17C), C37(H37A,H37B,H37C), C16(H16A,H16B,H16C), C26(H26A,
 H26B,H26C), C29(H29A,H29B,H29C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C),
 C15(H15A,H15B,H15C), C28(H28A,H28B,H28C), C38(H38A,H38B,H38C)
;
_olex2_date_sample_data_collection 2018-04-05
_olex2_submission_original_sample_id hasj180405a
_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 1.325
_oxdiff_exptl_absorpt_empirical_full_min 0.808