Donor-Acceptor Complexation and Dehydrogenation Chemistry of Aminoboranes
Adam C. Malcolm; Kyle J. Sabourin; Robert McDonald; Michael J. Ferguson; Eric Rivard; Inorganic Chemistry 51 (2012) 12905–12916; doi:10.1021/ic3018997

data_4331181
_publ_contact_author_address
;
Department of Chemistry
University of Alberta
Edmonton
AB T6G 2G2
CANADA
;
_publ_contact_author_email       ERIVARD@UALBERTA.CA
_publ_contact_author_name        'E. Rivard'
_publ_section_title
;
 Donor-Acceptor Complexation and Dehydrogenation Chemistry of Aminoboranes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12905
_journal_page_last               12916
_journal_paper_doi               10.1021/ic3018997
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C18 H39.96 B2 Cl0.04 N P, 1.5(C H2 Cl2)'
_chemical_formula_sum            'C19.5 H42.96 B2 Cl3.04 N P'
_chemical_formula_weight         450.49
_chemical_name_common            3
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 110.9230(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.9130(6)
_cell_length_b                   18.3557(10)
_cell_length_c                   13.6997(8)
_cell_measurement_reflns_used    6633
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      23.82
_cell_measurement_theta_min      2.22
_cell_volume                     2563.3(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0424
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            22370
_diffrn_reflns_theta_full        26.40
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.8957
_exptl_absorpt_correction_T_min  0.8658
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.171
_exptl_crystal_description       fragment
_exptl_crystal_F_000             975
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.29
_exptl_crystal_size_min          0.26
_platon_squeeze_details
;
Attempts to refine peaks of residual electron density as disordered 
or partial-occupancy solvent dichloromethane chlorine or carbon atoms 
were unsuccessful.  The data were corrected for disordered electron 
density through use of the SQUEEZE procedure (Sluis, P. van der; Spek, 
A. L. Acta Crystallogr. 1990, A46, 194-201) as implemented in PLATON 
(Spek, A. L. Acta Crystallogr. 1990, A46, C34; Spek, A. L. J. Appl. 
Cryst. 2003, 36, 7-13.  PLATON - a multipurpose crystallographic tool.  
Utrecht University, Utrecht, The Netherlands).  A total solvent-
accessible void volume of 734 \%A3 with a total electron count of 248 
(consistent with 6 molecules of solvent dichloromethane, or 1.5 molecules 
per formula unit of the Cy3PBH2NH2BH3 molecule) was found in the unit cell.
;
_refine_diff_density_max         0.300
_refine_diff_density_min         -0.204
_refine_diff_density_rms         0.036
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.066
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5933
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.066
_refine_ls_R_factor_all          0.0563
_refine_ls_R_factor_gt           0.0422
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0556P)^2^+0.4880P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1252
_reflns_number_gt                4489
_reflns_number_total             5933
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic3018997_si_002_1.cif
_cod_data_source_block           riv1291
_cod_original_formula_sum        'C19.50 H42.96 B2 Cl3.04 N P'
_cod_database_code               4331181