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_7706052
_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         'C50 H83 B2 Mg N3 O4, C2.5 H6'
_chemical_formula_sum            'C52.5 H89 B2 Mg N3 O4'
_chemical_formula_weight         872.19
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2019-08-13
_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
_cell_angle_beta                 99.6600(10)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   36.7820(6)
_cell_length_b                   15.5738(2)
_cell_length_c                   19.0103(3)
_cell_measurement_reflns_used    12464
_cell_measurement_temperature    150.01(10)
_cell_measurement_theta_max      72.2810
_cell_measurement_theta_min      3.0800
_cell_volume                     10735.4(3)
_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 1.000
_diffrn_measured_fraction_theta_max 0.994
_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  0.0473
_diffrn_reflns_av_unetI/netI     0.0434
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45878
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.126
_diffrn_reflns_theta_min         3.088
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.612
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.81605
_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_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.079
_exptl_crystal_description       block
_exptl_crystal_F_000             3832
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.094
_exptl_crystal_size_min          0.092
_refine_diff_density_max         0.536
_refine_diff_density_min         -0.301
_refine_diff_density_rms         0.042
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     650
_refine_ls_number_reflns         10690
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.023
_refine_ls_R_factor_all          0.0652
_refine_ls_R_factor_gt           0.0509
_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^)+(0.0734P)^2^+5.0077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1311
_refine_ls_wR_factor_ref         0.1417
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8526
_reflns_number_total             10690
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0dt04016a2.cif
_cod_data_source_block           s19msh139_cpd_2
_cod_depositor_comments
'Adding full bibliography for 7706050--7706056.cif.'
_cod_original_formula_sum        'C52.50 H89 B2 Mg N3 O4'
_cod_database_code               7706052
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O3-C36 \\sim O3-C36A
 with sigma of 0.02
 C37-C36 \\sim C37-C36A
 with sigma of 0.02
 C36-C38 \\sim C36A-C38A
 with sigma of 0.02
 C36-C39 \\sim C36A-C39A
 with sigma of 0.02
 O3-C38 \\sim O3-C38A
 with sigma of 0.04
 O3-C39 \\sim O3-C39A
 with sigma of 0.04
 C37-C38 \\sim C37-C38A
 with sigma of 0.04
 C37-C39 \\sim C37-C39A
 with sigma of 0.04
 C38-C39 \\sim C38A-C39A
 with sigma of 0.04
 C37-C41 \\sim C37-C41A
 with sigma of 0.02
 C37-C40 \\sim C37-C40A
 with sigma of 0.02
 C37-C36A \\sim C37-C36
 with sigma of 0.005
 C51-H51_$1 \\sim C51-H51
 with sigma of 0.005
 C52-C53 \\sim C52-C53A
 with sigma of 0.02
3. Others
 Fixed Sof: C36(0.75) C38(0.75) H38A(0.75) H38B(0.75) H38C(0.75) C39(0.75)
 H39A(0.75) H39B(0.75) H39C(0.75) C40(0.75) H40A(0.75) H40B(0.75) H40C(0.75)
 C41(0.75) H41A(0.75) H41B(0.75) H41C(0.75) C36A(0.25) C38A(0.25) H38D(0.25)
 H38E(0.25) H38F(0.25) C39A(0.25) H39D(0.25) H39E(0.25) H39F(0.25) C40A(0.25)
 H40D(0.25) H40E(0.25) H40F(0.25) C41A(0.25) H41D(0.25) H41E(0.25) H41F(0.25)
 H52A(0.5) H52B(0.5) H52C(0.5) H52D(0.5) C53(0.5) H53A(0.5) H53B(0.5) H53C(0.5)
 C53A(0.5) H53D(0.5) H53E(0.5) H53F(0.5)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27)
4.b Secondary CH2 refined with riding coordinates:
 C47(H47A,H47B), C48(H48A,H48B), C49(H49A,H49B), C52(H52A,H52B), C52(H52C,H52D)
4.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
4.d Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C13(H13A,H13B,H13C), C14(H14A,H14B,H14C),
 C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C25(H25A,H25B,H25C), C26(H26A,H26B,
 H26C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C32(H32A,H32B,H32C), C33(H33A,
 H33B,H33C), C34(H34A,H34B,H34C), C35(H35A,H35B,H35C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C50(H50A,H50B,H50C), C38(H38A,H38B,
 H38C), C39(H39A,H39B,H39C), C40(H40A,H40B,H40C), C41(H41A,H41B,H41C),
 C38A(H38D,H38E,H38F), C39A(H39D,H39E,H39F), C40A(H40D,H40E,H40F), C41A(H41D,
 H41E,H41F), C53(H53A,H53B,H53C), C53A(H53D,H53E,H53F)
;