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_7048345
_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 H59 Mg N2, B C24 F20'
_chemical_formula_sum            'C65 H59 B F20 Mg N2'
_chemical_formula_weight         1283.26
_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
_atom_sites_solution_primary     direct
_audit_creation_date             2016-07-07
_audit_creation_method
;
Olex2 1.2
(compiled 2016.02.19 svn.r3266 for OlexSys, GUI svn.r5155)
;
_audit_update_record
;
2018-08-31 deposited with the CCDC.
2018-12-06 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.265(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   17.6212(4)
_cell_length_b                   17.7017(5)
_cell_length_c                   19.0530(4)
_cell_measurement_reflns_used    14271
_cell_measurement_temperature    200.00(10)
_cell_measurement_theta_max      73.4430
_cell_measurement_theta_min      3.3940
_cell_volume                     5943.0(2)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
;
_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      200.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2903
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.963
_diffrn_measurement_details
;
  1 omega -114.00  -19.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -38.0000 -150.0000 95

  2 omega  -96.00   -2.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  125.0000  150.0000 94

  3 omega   23.00   97.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -       41.6909 -125.0000  120.0000 74

  4 omega   35.00  130.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000   30.0000 95

  5 omega   35.00  130.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955  -45.0000  150.0000 95

  6 omega   75.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955   77.0000 -180.0000 103

  7 omega   19.00  178.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955    0.0000  120.0000 159

  8 omega -112.00  -15.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -57.0000  120.0000 97

  9 omega -116.00  -10.00   1.0000   10.0000
omega____ theta____ kappa____ phi______ frames
    -      -41.6909  -77.0000    0.0000 106

 10 omega   34.00  101.00   1.0000   40.0000
omega____ theta____ kappa____ phi______ frames
    -      105.9955 -125.0000   30.0000 67
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0762294000
_diffrn_orient_matrix_UB_12      0.0097114000
_diffrn_orient_matrix_UB_13      -0.0381587000
_diffrn_orient_matrix_UB_21      -0.0218964000
_diffrn_orient_matrix_UB_22      -0.0640899000
_diffrn_orient_matrix_UB_23      -0.0510164000
_diffrn_orient_matrix_UB_31      -0.0368292000
_diffrn_orient_matrix_UB_32      0.0579879000
_diffrn_orient_matrix_UB_33      -0.0498100000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0340
_diffrn_reflns_av_unetI/netI     0.0306
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.963
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            33902
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.963
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.165
_diffrn_reflns_theta_min         3.408
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    1.201
_exptl_absorpt_correction_T_max  0.981
_exptl_absorpt_correction_T_min  0.966
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET)
(compiled Aug 13 2014,18:06:01)
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    1.434
_exptl_crystal_description       block
_exptl_crystal_F_000             2640
_exptl_crystal_size_max          0.1684
_exptl_crystal_size_mid          0.1292
_exptl_crystal_size_min          0.0797
_refine_diff_density_max         0.449
_refine_diff_density_min         -0.369
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     816
_refine_ls_number_reflns         11638
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0605
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0740P)^2^+1.4740P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1287
_refine_ls_wR_factor_ref         0.1426
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9191
_reflns_number_total             11638
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt03576h2.cif
_cod_data_source_block           hasj160701b
_cod_depositor_comments
'Adding full bibliography for 7048343--7048345.cif.'
_cod_original_cell_volume        5943.1(2)
_cod_database_code               7048345
_chemical_oxdiff_formula         'C65 H59 N2 Mg1 F20 B1'
_reflns_odcompleteness_completeness 99.47
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_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:
 C21(H21), C18(H18), C30(H30), C33(H33)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C16(H16), C14(H14), C15(H15), C28(H28), C26(H26), C27(H27), C36(H36),
 C37(H37), C41(H41), C38(H38), C39(H39), C40(H40)
2.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C3(H3A,H3B,H3C), C1(H1A,H1B,H1C), C22(H22A,H22B,H22C),
 C2(H2A,H2B,H2C), C10(H10A,H10B,H10C), C23(H23A,H23B,H23C), C31(H31A,H31B,H31C),
  C9(H9A,H9B,H9C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C32(H32A,H32B,
 H32C), C35(H35A,H35B,H35C), C34(H34A,H34B,H34C)
;
_shelx_shelxl_version_number     2014/7
_olex2_date_sample_data_collection 2016-07-01
_olex2_submission_special_instructions 'No special instructions were received'