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_7048344
_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         'C43 H63 Mg N2, B C24 F20'
_chemical_formula_sum            'C67 H63 B F20 Mg N2'
_chemical_formula_weight         1311.31
_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   geom
_audit_creation_date             2018-07-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 93.9920(14)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.3516(3)
_cell_length_b                   17.6435(3)
_cell_length_c                   18.8442(3)
_cell_measurement_reflns_used    11476
_cell_measurement_temperature    99.98(16)
_cell_measurement_theta_max      72.8710
_cell_measurement_theta_min      3.4080
_cell_volume                     6086.69(17)
_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)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      99.98(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.960
_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    -63.00  28.00   1.00    3.00    --  -41.15  57.00 150.00   91
  2  \w    -68.00 -18.00   1.00    3.00    --  -41.15  57.00  60.00   50
  3  \w   -106.00 -15.00   1.00    3.00    --  -41.15 -57.00 -90.00   91
  4  \w     36.00 130.00   1.00   15.00    --  104.96 -61.00 120.00   94
  5  \w     83.00 177.00   1.00   15.00    --  104.96  45.00 -90.00   94
  6  \w     94.00 178.00   1.00   15.00    --  104.96 125.00 120.00   84
  7  \w     22.00 109.00   1.00   15.00    --  104.96 -94.00  60.00   87
;
_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      -0.0737724000
_diffrn_orient_matrix_UB_12      -0.0421419000
_diffrn_orient_matrix_UB_13      -0.0045150000
_diffrn_orient_matrix_UB_21      0.0404259000
_diffrn_orient_matrix_UB_22      -0.0759178000
_diffrn_orient_matrix_UB_23      0.0123909000
_diffrn_orient_matrix_UB_31      -0.0041624000
_diffrn_orient_matrix_UB_32      0.0091528000
_diffrn_orient_matrix_UB_33      0.0808296000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0424
_diffrn_reflns_Laue_measured_fraction_full 0.992
_diffrn_reflns_Laue_measured_fraction_max 0.960
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            21338
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.960
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         72.823
_diffrn_reflns_theta_min         3.435
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.184
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.68541
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)
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    1.431
_exptl_crystal_description       needle
_exptl_crystal_F_000             2704
_exptl_crystal_size_max          0.334
_exptl_crystal_size_mid          0.238
_exptl_crystal_size_min          0.068
_refine_diff_density_max         0.977
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.017
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     836
_refine_ls_number_reflns         11659
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0558
_refine_ls_R_factor_gt           0.0490
_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^)+(0.0751P)^2^+3.0985P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1286
_refine_ls_wR_factor_ref         0.1363
_reflns_Friedel_coverage         0.000
_reflns_number_gt                10120
_reflns_number_total             11659
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03576h2.cif
_cod_data_source_block           hasj180318a
_cod_depositor_comments
'Adding full bibliography for 7048343--7048345.cif.'
_cod_original_cell_volume        6086.70(16)
_cod_database_code               7048344
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B F'
_reflns_odcompleteness_completeness 99.17
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.49
_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:
 C18(H18), C33(H33), C21(H21), C30(H30)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C28(H28), C26(H26), C14(H14), C27(H27), C16(H16), C15(H15), C39(H39),
 C37(H37), C36(H36), C41(H41)
2.c Idealised Me refined as rotating group:
 C10(H10A,H10B,H10C), C9(H9A,H9B,H9C), C1(H1A,H1B,H1C), C3(H3A,H3B,H3C),
 C2(H2A,H2B,H2C), C11(H11A,H11B,H11C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C),
  C31(H31A,H31B,H31C), C42(H42A,H42B,H42C), C32(H32A,H32B,H32C), C43(H43A,H43B,
 H43C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C22(H22A,H22B,H22C), C23(H23A,
 H23B,H23C)
;
_olex2_date_sample_data_collection 2018-03-18
_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 1.662
_oxdiff_exptl_absorpt_empirical_full_min 0.692