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_1551156
_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         'C54 H75 B Mg N4 O2'
_chemical_formula_sum            'C54 H75 B Mg N4 O2'
_chemical_formula_weight         847.30
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2016-11-30
_audit_creation_method
;
Olex2 1.2
(compiled 2016.11.24 svn.r3356 for OlexSys, GUI svn.r5267)
;
_audit_update_record
;
2019-04-17 deposited with the CCDC.    2019-05-24 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.065(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.6101(2)
_cell_length_b                   15.4868(2)
_cell_length_c                   17.9575(2)
_cell_measurement_reflns_used    17145
_cell_measurement_temperature    291.55(10)
_cell_measurement_theta_max      73.2510
_cell_measurement_theta_min      3.7590
_cell_volume                     5041.6(2)
_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      air
_diffrn_ambient_temperature      291.55(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 0.9998
_diffrn_measured_fraction_theta_max 0.7564
_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           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0414
_diffrn_reflns_av_unetI/netI     0.0302
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29358
_diffrn_reflns_point_group_measured_fraction_max 0.762
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.354
_diffrn_reflns_theta_min         3.754
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    0.623
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.965
_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    1.116
_exptl_crystal_description       block
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.323
_exptl_crystal_size_mid          0.099
_exptl_crystal_size_min          0.084
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.210
_refine_diff_density_rms         0.040
_refine_ls_abs_structure_details
;
 Flack x determined using 2385 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.01(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     579
_refine_ls_number_reflns         7701
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0402
_refine_ls_R_factor_gt           0.0383
_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^)+(0.0755P)^2^+0.5839P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1056
_reflns_Friedel_coverage         0.523
_reflns_Friedel_fraction_full    0.546
_reflns_Friedel_fraction_max     0.524
_reflns_number_gt                7383
_reflns_number_total             7701
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c9sc02087j2.cif
_cod_data_source_block           s16msh99-cpd14
_cod_original_cell_volume        5041.57(10)
_cod_database_code               1551156
_shelx_shelxl_version_number     2014/7