Reactivity of a magnesium diboranate with organic nitriles.
Shere, Henry; Hill, Michael S.; Pécharman, Anne-Frédérique; Mahon, Mary F.; Dalton transactions (Cambridge, England : 2003) 50 (2021) 1283–1292; doi:10.1039/d0dt04016a

data_7706054
_publ_section_title
;
 Reactivity of a magnesium diboranate with organic nitriles.
;
_journal_issue                   4
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1283
_journal_page_last               1292
_journal_paper_doi               10.1039/d0dt04016a
_journal_volume                  50
_journal_year                    2021
_chemical_formula_moiety         'C43 H67 B Mg N4 O2, C3.5 H4'
_chemical_formula_sum            'C46.5 H71 B Mg N4 O2'
_chemical_formula_weight         753.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-03-26
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-11-17 deposited with the CCDC.	2020-12-11 downloaded from the CCDC.
;
_cell_angle_alpha                90.694(2)
_cell_angle_beta                 108.261(2)
_cell_angle_gamma                105.976(2)
_cell_formula_units_Z            2
_cell_length_a                   11.7365(2)
_cell_length_b                   12.6432(3)
_cell_length_c                   16.8901(4)
_cell_measurement_reflns_used    14650
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      73.0690
_cell_measurement_theta_min      4.8220
_cell_volume                     2274.81(9)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0262
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25194
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.093
_diffrn_reflns_theta_min         2.771
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.631
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84865
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.100
_exptl_crystal_description       block
_exptl_crystal_F_000             822
_exptl_crystal_size_max          0.315
_exptl_crystal_size_mid          0.216
_exptl_crystal_size_min          0.166
_refine_diff_density_max         0.262
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.037
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     555
_refine_ls_number_reflns         9038
_refine_ls_number_restraints     28
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0437
_refine_ls_R_factor_gt           0.0395
_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^)+(0.0536P)^2^+0.5935P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1041
_refine_ls_wR_factor_ref         0.1076
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8134
_reflns_number_total             9038
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04016a2.cif
_cod_data_source_block           s19msh49_cpd_3
_cod_depositor_comments
'Adding full bibliography for 7706050--7706056.cif.'
_cod_original_formula_sum        'C46.50 H71 B Mg N4 O2'
_cod_database_code               7706054
_shelx_shelxl_version_number     2014/7
_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. Restrained distances
 C15-C16 \\sim C15-C16A
 with sigma of 0.02
 C15-C17 \\sim C15-C17A
 with sigma of 0.02
 C27-C29 \\sim C27-C29A
 with sigma of 0.02
 C27-C28 \\sim C27-C28A
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C28 \\sim C29 \\sim C28A \\sim C29A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
C16 \\sim C17 \\sim C16A \\sim C17A: within 2A with sigma of 0.02 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: H15(0.55) H15A(0.45) H27(0.55) H27A(0.45) C16(0.55) H16A(0.55)
 H16B(0.55) H16C(0.55) C17(0.55) H17A(0.55) H17B(0.55) H17C(0.55) C28(0.55)
 H28A(0.55) H28B(0.55) H28C(0.55) C29(0.55) H29A(0.55) H29B(0.55) H29C(0.55)
 C16A(0.45) H16D(0.45) H16E(0.45) H16F(0.45) C17A(0.45) H17D(0.45) H17E(0.45)
 H17F(0.45) C28A(0.45) H28D(0.45) H28E(0.45) H28F(0.45) C29A(0.45) H29D(0.45)
 H29E(0.45) H29F(0.45) H45(0.5) C44(0.5) H44A(0.5) H44B(0.5) H44C(0.5)
5.a Ternary CH refined with riding coordinates:
 C00F(H00F), C12(H12), C15(H15), C15(H15A), C24(H24), C27(H27), C27(H27A),
 C31(H31)
5.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C45(H45),
 C46(H46), C47(H47)
5.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C32(H32A,H32B,H32C), C33(H33A,H33B,
 H33C), C36(H36A,H36B,H36C), C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C41(H41A,
 H41B,H41C), C42(H42A,H42B,H42C), C43(H43A,H43B,H43C), C16(H16A,H16B,H16C),
 C17(H17A,H17B,H17C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C16A(H16D,H16E,
 H16F), C17A(H17D,H17E,H17F), C28A(H28D,H28E,H28F), C29A(H29D,H29E,H29F),
 C44(H44A,H44B,H44C)
;