Use of crown ethers to isolate intermediates in ammonia-borane dehydrocoupling reactions.
Less, Robert J.; García-Rodríguez, Raúl; Simmonds, Hayley R.; Allen, Lucy K.; Bond, Andrew D.; Wright, Dominic S.; Chemical communications (Cambridge, England) 52 (2016) 3650–3652; doi:10.1039/c6cc00088f

data_7118674
_publ_section_title
;
 Use of crown ethers to isolate intermediates in ammonia-borane
 dehydrocoupling reactions.
;
_journal_issue                   18
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              3650
_journal_page_last               3652
_journal_paper_doi               10.1039/c6cc00088f
_journal_volume                  52
_journal_year                    2016
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C12 H24 O6, C4 H13 B O N +, Al Cl4 -'
_chemical_formula_sum            'C16 H37 Al B Cl4 N O7'
_chemical_formula_weight         535.05
_space_group_crystal_system      orthorhombic
_space_group_IT_number           33
_space_group_name_Hall           'P 2c -2n'
_space_group_name_H-M_alt        'P n a 21'
_symmetry_space_group_name_Hall  'P 2c -2n'
_symmetry_space_group_name_H-M   'P n a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-12-18 deposited with the CCDC.
2016-01-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   19.0847(7)
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_cell_length_c                   8.8244(3)
_cell_measurement_reflns_used    9906
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      66.70
_cell_measurement_theta_min      3.60
_cell_volume                     2700.79(17)
_computing_cell_refinement       'SAINT (Bruker, 2014)'
_computing_data_collection       'APEX2 (Bruker, 2014)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'Mercury (Macrae et al., 2008)'
_computing_publication_material  SHELXL
_computing_structure_refinement  'SHELXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Bruker D8-QUEST PHOTON-100'
_diffrn_measurement_method       '\w and \f-scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0600
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_laue_measured_fraction_full 0.987
_diffrn_reflns_laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            16779
_diffrn_reflns_point_group_measured_fraction_full 0.839
_diffrn_reflns_point_group_measured_fraction_max 0.839
_diffrn_reflns_theta_full        66.693
_diffrn_reflns_theta_max         66.693
_diffrn_reflns_theta_min         3.600
_diffrn_source                   'Incoatec I\mS Cu microsource'
_exptl_absorpt_coefficient_mu    4.589
_exptl_absorpt_correction_T_max  0.7528
_exptl_absorpt_correction_T_min  0.4258
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.316
_exptl_crystal_description       needle
_exptl_crystal_F_000             1128
_exptl_crystal_size_max          0.350
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.663
_refine_diff_density_min         -0.413
_refine_diff_density_rms         0.103
_refine_ls_abs_structure_details
;
Flack x determined using 1124 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.018(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.424
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     272
_refine_ls_number_reflns         4023
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.424
_refine_ls_R_factor_all          0.1032
_refine_ls_R_factor_gt           0.0987
_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^)+(0.0515P)^2^+10.9569P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2169
_refine_ls_wR_factor_ref         0.2191
_reflns_Friedel_coverage         0.587
_reflns_friedel_fraction_full    0.668
_reflns_friedel_fraction_max     0.668
_reflns_number_gt                3875
_reflns_number_total             4023
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6cc00088f2.cif
_cod_data_source_block           DW_B2_0025
_cod_depositor_comments
'Adding full bibliography for 7118673--7118675.cif.'
_cod_database_code               7118674
_cambridge_user_name             'Rob Less'
_cambridge_user_crsid            rjl1003
_cambridge_supervisor_name       'Dominic Wright'
_cambridge_supervisor_crsid      dsw1000
_cambridge_crystallographer_name 'Andrew Bond'
_cambridge_crystallographer_crsid adb29
_cambridge_sample_id             RL1347A1
_cambridge_data_id               dw_b2_0025
_shelx_estimated_absorpt_t_min   0.297
_shelx_estimated_absorpt_t_max   0.710
_shelx_res_checksum              50999