Bora-amidinate as a cooperative ligand in group 2 metal catalysis
Freitag, Benjamin; Fischer, Christian A.; Penafiel, Johanne; Ballmann, Gerd; Elsen, Holger; Färber, Christian; Piesik, Dirk F.; Harder, Sjoerd; Dalton Trans.  (2017) –; doi:10.1039/C7DT02136D

data_7043833
_publ_section_title
;
 Bora-amidinate as a cooperative ligand in group 2 metal catalysis
;
_journal_name_full               'Dalton Trans.'
_journal_paper_doi               10.1039/C7DT02136D
_journal_year                    2017
_chemical_formula_moiety         'C36 H59 B Mg N2 O3'
_chemical_formula_sum            'C36 H59 B Mg N2 O3'
_chemical_formula_weight         602.97
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2017-03-08
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_audit_update_record
;
2017-05-22 deposited with the CCDC.
2017-07-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5266(2)
_cell_length_b                   17.9167(3)
_cell_length_c                   18.7856(4)
_cell_measurement_reflns_used    11721
_cell_measurement_temperature    100
_cell_measurement_theta_max      73.4500
_cell_measurement_theta_min      3.3830
_cell_volume                     3543.00(12)
_computing_cell_refinement       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43 (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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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    -64.00  31.00   1.00    2.00    --  -41.69  38.00  90.00   95
  2  \w     17.00 112.00   1.00    2.00    --   41.69  49.00 165.00   95
  3  \w     23.00  97.00   1.00    2.00    --   41.69-125.00-120.00   74
  4  \w     82.00 177.00   1.00    8.00    --  106.00  45.00 150.00   95
  5  \w     25.00 109.00   1.00    8.00    --  106.00 -94.00-150.00   84
  6  \w     75.00 178.00   1.00    8.00    --  106.00  77.00-120.00  103
  7  \w   -112.00 -62.00   1.00    2.00    --  -41.69-143.00 150.00   50
  8  \w   -116.00 -10.00   1.00    2.00    --  -41.69 -77.00   0.00  106
  9  \w     15.00  54.00   1.00    2.00    --   41.69  57.00 -90.00   39
 10  \w    120.00 171.00   1.00    8.00    --  106.00 125.00 -90.00   51
 11  \w     78.00 144.00   1.00    8.00    --  106.00  61.00 -60.00   66
;
_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      -0.0038888000
_diffrn_orient_matrix_UB_12      0.0857505000
_diffrn_orient_matrix_UB_13      -0.0048056000
_diffrn_orient_matrix_UB_21      0.0884170000
_diffrn_orient_matrix_UB_22      -0.0026276000
_diffrn_orient_matrix_UB_23      -0.0653216000
_diffrn_orient_matrix_UB_31      -0.1166597000
_diffrn_orient_matrix_UB_32      -0.0047446000
_diffrn_orient_matrix_UB_33      -0.0493717000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0486
_diffrn_reflns_av_unetI/netI     0.0457
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17026
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.115
_diffrn_reflns_theta_min         3.409
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.698
_exptl_absorpt_correction_T_max  0.992
_exptl_absorpt_correction_T_min  0.981
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43 (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    1.130
_exptl_crystal_description       block
_exptl_crystal_F_000             1320
_exptl_crystal_size_max          0.425
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.164
_refine_diff_density_max         0.422
_refine_diff_density_min         -0.307
_refine_diff_density_rms         0.046
_refine_ls_abs_structure_details
;
 Flack x determined using 2431 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.04(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         6422
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0490
_refine_ls_R_factor_gt           0.0466
_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^)+(0.0710P)^2^+0.9060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1245
_reflns_Friedel_coverage         0.770
_reflns_Friedel_fraction_full    0.987
_reflns_Friedel_fraction_max     0.984
_reflns_number_gt                6102
_reflns_number_total             6422
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c7dt02136d2.cif
_cod_data_source_block           hasj161205b
_cod_database_code               7043833
_shelx_shelxl_version_number     2014/7
_chemical_oxdiff_formula         'C H N Mg B O'
_reflns_odcompleteness_completeness 99.92
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.96
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C7(H7), C19(H19), C22(H22), C10(H10)
2.b Secondary CH2 refined with riding coordinates:
 C34(H34A,H34B), C29(H29A,H29B), C28(H28A,H28B), C35(H35A,H35B), C25(H25A,
 H25B), C36(H36A,H36B), C27(H27A,H27B), C26(H26A,H26B), C33(H33A,H33B),
 C32(H32A,H32B), C30(H30A,H30B), C31(H31A,H31B)
2.c Aromatic/amide H refined with riding coordinates:
 C5(H5), C3(H3), C17(H17), C15(H15), C4(H4), C16(H16)
2.d Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C11(H11A,H11B,H11C), C20(H20A,H20B,
 H20C), C21(H21A,H21B,H21C), C9(H9A,H9B,H9C), C24(H24A,H24B,H24C), C23(H23A,
 H23B,H23C)
;
_olex2_date_sample_data_collection 2016-12-05
_olex2_submission_original_sample_id hasj161205b
_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 4.058
_oxdiff_exptl_absorpt_empirical_full_min 0.292