Snapshots of Magnesium-Centred Diborane Heterolysis by an Outer Sphere SN2 Process
Pecharman, Anne-Frederique; Hill, Michael; McMullon, Grace; McMullin, Claire; Mahon, Mary F.; Chemical Science  (2019) –; doi:10.1039/C9SC02087J

data_1551152
_publ_section_title
;
 Snapshots of Magnesium-Centred Diborane Heterolysis by an Outer Sphere
 SN2 Process
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/C9SC02087J
_journal_year                    2019
_chemical_formula_moiety         'C46 H68 B Mg N3 O2'
_chemical_formula_sum            'C46 H68 B Mg N3 O2'
_chemical_formula_weight         730.15
_chemical_name_systematic
;
 ?
;
_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     iterative
_audit_creation_date             2017-03-01
_audit_creation_method
;
Olex2 1.2
(compiled 2017.02.23 svn.r3390 for OlexSys, GUI svn.r5320)
;
_audit_update_record
;
2019-04-17 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.285(1)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   23.0251(3)
_cell_length_b                   18.0591(2)
_cell_length_c                   22.6756(2)
_cell_measurement_reflns_used    39731
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      73.1990
_cell_measurement_theta_min      3.2380
_cell_volume                     8724.55(18)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(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 0.996
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, 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  0.0515
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            125364
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.489
_diffrn_reflns_theta_min         3.208
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.638
_exptl_absorpt_correction_T_max  0.987
_exptl_absorpt_correction_T_min  0.964
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (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            colorless
_exptl_crystal_density_diffrn    1.112
_exptl_crystal_description       block
_exptl_crystal_F_000             3184
_exptl_crystal_size_max          0.699
_exptl_crystal_size_mid          0.222
_exptl_crystal_size_min          0.179
_refine_diff_density_max         0.456
_refine_diff_density_min         -0.425
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1077
_refine_ls_number_reflns         17508
_refine_ls_number_restraints     162
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0685
_refine_ls_R_factor_gt           0.0592
_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^)+(0.0650P)^2^+6.1338P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1484
_refine_ls_wR_factor_ref         0.1545
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14894
_reflns_number_total             17508
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02087j2.cif
_cod_data_source_block           s17msh28-16BN
_cod_depositor_comments
;

2022-11-30
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C92 H136 B2 Mg2 N6 O4'
_cod_original_formula_weight         1460.30
_cod_original_formula_moiety         '2(C46 H68 B Mg N3 O2)'
_cod_original_formula_units_Z            4
_cod_database_code               1551152
_shelxl_version_number           2014-3
_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. Uiso/Uaniso restraints and constraints
C28 \\sim C28 \\sim C28 \\sim C28 \\sim N2 \\sim C27 \\sim C27 \\sim C27 \\sim
C27 \\sim C27 \\sim C29 \\sim C29 \\sim C29 \\sim C29 \\sim C29 \\sim C24 \\sim
C24 \\sim C24 \\sim C24 \\sim C0AA \\sim C0AA \\sim C0AA \\sim C26 \\sim C26
\\sim C18 \\sim C18 \\sim C18 \\sim C18 \\sim C19 \\sim C19 \\sim C19 \\sim C19
\\sim C20 \\sim C20 \\sim C20 \\sim C20 \\sim C21 \\sim C21 \\sim C21 \\sim C21
\\sim C22 \\sim C22 \\sim C22 \\sim C22 \\sim C23 \\sim C23 \\sim C23 \\sim
C23: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.005
C2 \\sim C18A \\sim C18A \\sim C18A \\sim C18A \\sim C19A \\sim C19A \\sim C19A
\\sim C19A \\sim C19A \\sim C20A \\sim C20A \\sim C20A \\sim C21A \\sim C21A
\\sim C21A \\sim C21A \\sim C22A \\sim C22A \\sim C22A \\sim C22A \\sim C22A
\\sim C23A \\sim C23A \\sim C23A \\sim C23A \\sim C24A \\sim C24A \\sim C24A
\\sim C24A \\sim C24A \\sim C24A \\sim C26A \\sim C26A \\sim C26A \\sim C26A
\\sim C26A \\sim C26A \\sim C25 \\sim C25 \\sim C25 \\sim C25 \\sim C25 \\sim
C27A \\sim C27A \\sim C27A \\sim C27A \\sim C27A \\sim C27A \\sim C27A \\sim
C27A \\sim C29A \\sim C29A \\sim C29A \\sim C29A \\sim C29A \\sim C29A \\sim
C29A \\sim C29A \\sim N2 \\sim N2 \\sim N2 \\sim N2 \\sim Mg1 \\sim C28A \\sim
C28A \\sim C28A \\sim C28A: within 2A with sigma of 0.01 and sigma for terminal
atoms of 0.005
3. Others
 Fixed Sof: C18(0.6) C19(0.6) C20(0.6) H20(0.6) C21(0.6) H21(0.6) C22(0.6)
 H22(0.6) C23(0.6) C24(0.6) H24(0.6) C25(0.4) H25A(0.4) H25B(0.4) H25C(0.4)
 C26(0.6) H26A(0.6) H26B(0.6) H26C(0.6) C27(0.6) H27(0.6) C28(0.6) H28A(0.6)
 H28B(0.6) H28C(0.6) C29(0.6) H29A(0.6) H29B(0.6) H29C(0.6) C18A(0.4) C19A(0.4)
 C20A(0.4) H20A(0.4) C21A(0.4) H21A(0.4) C22A(0.4) H22A(0.4) C23A(0.4)
 C24A(0.4) H24A(0.4) C26A(0.4) H26D(0.4) H26E(0.4) H26F(0.4) C27A(0.4)
 H27A(0.4) C28A(0.4) H28D(0.4) H28E(0.4) H28F(0.4) C29A(0.4) H29D(0.4)
 H29E(0.4) H29F(0.4) C0AA(0.6) H0AA(0.6) H0AB(0.6) H0AC(0.6)
4.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C24(H24), C27(H27), C30(H30), C24A(H24A), C27A(H27A),
 C58(H58), C61(H61), C70(H70), C73(H73), C76(H76)
4.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22), C32(H32),
 C33(H33), C34(H34), C35(H35), C36(H36), C20A(H20A), C21A(H21A), C22A(H22A),
 C49(H49), C54(H54), C55(H55), C56(H56), C66(H66), C67(H67), C68(H68), C78(H78),
  C79(H79), C80(H80), C81(H81), C82(H82)
4.c Fitted hexagon refined as free rotating group:
 C18(C19,C20,C21,C22,C23), C18A(C19A,C20A,C21A,C22A,C23A)
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), C38(H38A,H38B,H38C), C39(H39A,
 H39B,H39C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C44(H44A,H44B,H44C),
 C45(H45A,H45B,H45C), C46(H46A,H46B,H46C), C26A(H26D,H26E,H26F), C28A(H28D,H28E,
 H28F), C29A(H29D,H29E,H29F), C0AA(H0AA,H0AB,H0AC), C47(H47A,H47B,H47C),
 C51(H51A,H51B,H51C), C59(H59A,H59B,H59C), C60(H60A,H60B,H60C), C62(H62A,H62B,
 H62C), C63(H63A,H63B,H63C), C71(H71A,H71B,H71C), C72(H72A,H72B,H72C), C74(H74A,
 H74B,H74C), C75(H75A,H75B,H75C), C84(H84A,H84B,H84C), C85(H85A,H85B,H85C),
 C86(H86A,H86B,H86C), C89(H89A,H89B,H89C), C90(H90A,H90B,H90C), C91(H91A,H91B,
 H91C), C92(H92A,H92B,H92C)
;