Diborane Heterolysis: Breaking and Making B-B bonds at Magnesium
Hill, Michael; Mahon, Mary F.; Pecharman, Anne-Frederique; Dalton Transactions  (2018) –; doi:10.1039/C8DT01451E

data_7046275
_publ_section_title
;
 Diborane Heterolysis: Breaking and Making B-B bonds at Magnesium
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/C8DT01451E
_journal_year                    2018
_chemical_formula_moiety         'C45 H74 B2 Mg N2 O4'
_chemical_formula_sum            'C45 H74 B2 Mg N2 O4'
_chemical_formula_weight         752.99
_space_group_crystal_system      orthorhombic
_space_group_IT_number           60
_space_group_name_Hall           '-P 2n 2ab'
_space_group_name_H-M_alt        'P b c n'
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2018-02-19
_audit_creation_method
;
Olex2 1.2
(compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381)
;
_audit_update_record
;
2018-02-19 deposited with the CCDC.
2018-05-09 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   15.16029(17)
_cell_length_b                   27.6648(3)
_cell_length_c                   21.7294(2)
_cell_measurement_reflns_used    21393
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      72.3090
_cell_measurement_theta_min      3.1940
_cell_volume                     9113.45(17)
_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_temperature      150.00(10)
_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_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0544
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            62560
_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         73.161
_diffrn_reflns_theta_min         3.195
_exptl_absorpt_coefficient_mu    0.645
_exptl_absorpt_correction_T_max  0.993
_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    1.098
_exptl_crystal_description       block
_exptl_crystal_F_000             3296
_exptl_crystal_size_max          0.246
_exptl_crystal_size_mid          0.161
_exptl_crystal_size_min          0.091
_refine_diff_density_max         0.624
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.059
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     647
_refine_ls_number_reflns         9102
_refine_ls_number_restraints     87
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0646
_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^)+(0.0862P)^2^+5.3552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1671
_refine_ls_wR_factor_ref         0.1759
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7638
_reflns_number_total             9102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt01451e2.cif
_cod_data_source_block           s16msh60
_cod_original_cell_volume        9113.46(16)
_cod_database_code               7046275
_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
 C41-C39 \\sim C41A-C39A \\sim C40-C39 \\sim C40A-C39A
 with sigma of 0.005
 C32A-C31 \\sim C32-C31A
 with sigma of 0.005
 C31A-C30A \\sim C31-C30
 with sigma of 0.005
 C33-C32A \\sim C33A-C32
 with sigma of 0.005
 C34A-C33 \\sim C34-C33A \\sim C35-C33 \\sim C35A-C33A
 with sigma of 0.005
 C33-C32 \\sim C33A-C32A \\sim C32A-C31A \\sim C32-C31
 with sigma of 0.005
 O2-C33 \\sim O2-C33A \\sim O1-C31A \\sim O1-C31
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
C39A \\sim C37A \\sim C41A \\sim C36A \\sim C38A \\sim C40A: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.01
C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41: within 2A with sigma of
0.01 and sigma for terminal atoms of 0.01
4. Others
 Fixed Sof: C24(0.55) H24(0.55) C25(0.55) H25A(0.55) H25B(0.55) H25C(0.55)
 C26(0.55) H26A(0.55) H26B(0.55) H26C(0.55) C30(0.55) H30A(0.55) H30B(0.55)
 H30C(0.55) C31(0.55) H31(0.55) C32(0.55) H32A(0.55) H32B(0.55) C33(0.55)
 C34(0.55) H34A(0.55) H34B(0.55) H34C(0.55) C35(0.55) H35A(0.55) H35B(0.55)
 H35C(0.55) C36(0.55) H36A(0.55) H36B(0.55) H36C(0.55) C37(0.55) H37(0.55)
 C38(0.55) H38A(0.55) H38B(0.55) C39(0.55) C40(0.55) H40A(0.55) H40B(0.55)
 H40C(0.55) C41(0.55) H41A(0.55) H41B(0.55) H41C(0.55) C39A(0.45) C31A(0.45)
 H31A(0.45) C24A(0.45) H24A(0.45) C35A(0.45) H35D(0.45) H35E(0.45) H35F(0.45)
 C26A(0.45) H26D(0.45) H26E(0.45) H26F(0.45) C33A(0.45) C37A(0.45) H37A(0.45)
 C41A(0.45) H41D(0.45) H41E(0.45) H41F(0.45) C25A(0.45) H25D(0.45) H25E(0.45)
 H25F(0.45) C30A(0.45) H30D(0.45) H30E(0.45) H30F(0.45) C32A(0.45) H32C(0.45)
 H32D(0.45) C34A(0.45) H34D(0.45) H34E(0.45) H34F(0.45) C36A(0.45) H36D(0.45)
 H36E(0.45) H36F(0.45) C38A(0.45) H38C(0.45) H38D(0.45) C40A(0.45) H40D(0.45)
 H40E(0.45) H40F(0.45)
5.a Ternary CH refined with riding coordinates:
 C12(H12), C15(H15), C27(H27), C24(H24), C31(H31), C37(H37), C31A(H31A),
 C24A(H24A), C37A(H37A)
5.b Secondary CH2 refined with riding coordinates:
 C42(H42A,H42B), C43(H43A,H43B), C32(H32A,H32B), C38(H38A,H38B), C44(H44A,
 H44B), C32A(H32C,H32D), C38A(H38C,H38D)
5.c Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C9(H9), C10(H10), C20(H20), C21(H21), C22(H22)
5.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), C28(H28A,H28B,H28C), C29(H29A,H29B,
 H29C), C25(H25A,H25B,H25C), C26(H26A,H26B,H26C), C30(H30A,H30B,H30C), C34(H34A,
 H34B,H34C), C35(H35A,H35B,H35C), C36(H36A,H36B,H36C), C40(H40A,H40B,H40C),
 C41(H41A,H41B,H41C), C45(H45A,H45B,H45C), C35A(H35D,H35E,H35F), C26A(H26D,H26E,
 H26F), C41A(H41D,H41E,H41F), C25A(H25D,H25E,H25F), C30A(H30D,H30E,H30F),
 C34A(H34D,H34E,H34F), C36A(H36D,H36E,H36F), C40A(H40D,H40E,H40F)
;
_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
;