#------------------------------------------------------------------------------
#$Date: 2016-03-21 18:22:36 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178810 $
#$URL: svn://www.crystallography.net/cod/cif/4/10/64/4106462.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4106462
loop_
_publ_author_name
'Heather C. Johnson'
'Alasdair P. M. Robertson'
'Adrian B. Chaplin'
'Laura J. Sewell'
'Amber L. Thompson'
'Mairi F. Haddow'
'Ian Manners'
'Andrew S. Weller'
_publ_section_title
;
 Catching the First Oligomerization Event in the Catalytic Formation of
 Polyaminoboranes: H3B.NMeHBH2.NMeH2 Bound to Iridium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11076
_journal_page_last               11079
_journal_paper_doi               10.1021/ja2040738
_journal_volume                  133
_journal_year                    2011
_chemical_formula_moiety         'C2 H14 B2 N2'
_chemical_formula_sum            'C2 H14 B2 N2'
_chemical_formula_weight         87.77
_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                 96.081(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.7173(4)
_cell_length_b                   8.5002(3)
_cell_length_c                   9.0429(3)
_cell_measurement_reflns_used    4823
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      3.30
_cell_volume                     666.30(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Apex II kappa CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0186
_diffrn_reflns_av_sigmaI/netI    0.0164
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            8590
_diffrn_reflns_theta_full        29.60
_diffrn_reflns_theta_max         29.60
_diffrn_reflns_theta_min         3.30
_exptl_absorpt_coefficient_mu    0.051
_exptl_absorpt_correction_T_max  0.7459
_exptl_absorpt_correction_T_min  0.6824
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS-2008/1
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.875
_exptl_crystal_description       plate
_exptl_crystal_F_000             200
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.47
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.826
_refine_diff_density_min         -0.603
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.166
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     58
_refine_ls_number_reflns         1856
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.166
_refine_ls_R_factor_all          0.0762
_refine_ls_R_factor_gt           0.0710
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1682P)²+0.3377P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2593
_refine_ls_wR_factor_ref         0.2667
_reflns_number_gt                1662
_reflns_number_total             1856
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2040738_si_002.cif
_cod_data_source_block           ar4_0m
_cod_database_code               4106462
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
N1 N 0.16124(14) 0.21663(14) 0.59110(12) 0.0138(4) Uani 1 1 d .
H1 H 0.1414 0.1968 0.4897 0.017 Uiso 1 1 calc R
N2 N 0.23187(13) -0.07289(15) 0.64727(13) 0.0150(4) Uani 1 1 d .
H2A H 0.1558 -0.0819 0.7099 0.018 Uiso 1 1 calc R
H2B H 0.1884 -0.0947 0.5523 0.018 Uiso 1 1 calc R
B1 B 0.21791(18) 0.38159(19) 0.60732(18) 0.0157(4) Uani 1 1 d .
H1A H 0.2382 0.4077 0.7131 0.023 Uiso 1 1 calc R
H1B H 0.1396 0.4532 0.5597 0.023 Uiso 1 1 calc R
H1C H 0.3133 0.3924 0.5598 0.023 Uiso 1 1 calc R
B2 B 0.29476(17) 0.10237(19) 0.65311(17) 0.0149(4) Uani 1 1 d .
H2C H 0.3317 0.1311 0.7569 0.018 Uiso 1 1 calc R
H2D H 0.3824 0.1115 0.5924 0.018 Uiso 1 1 calc R
C1 C 0.00245(17) 0.19636(19) 0.66096(17) 0.0202(4) Uani 1 1 d .
H1D H 0.0190 0.2150 0.7684 0.030 Uiso 1 1 calc R
H1E H -0.0367 0.0893 0.6422 0.030 Uiso 1 1 calc R
H1F H -0.0728 0.2723 0.6153 0.030 Uiso 1 1 calc R
C2 C 0.35441(18) -0.1899(2) 0.6908(2) 0.0252(4) Uani 1 1 d .
H2E H 0.4282 -0.1915 0.6162 0.038 Uiso 1 1 calc R
H2F H 0.3080 -0.2944 0.6972 0.038 Uiso 1 1 calc R
H2G H 0.4081 -0.1613 0.7878 0.038 Uiso 1 1 calc R
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
N1 0.0155(6) 0.0130(6) 0.0127(6) -0.0001(4) 0.0009(4) 0.0001(4)
N2 0.0117(6) 0.0137(6) 0.0193(6) 0.0010(4) 0.0002(4) 0.0006(4)
B1 0.0178(7) 0.0088(7) 0.0205(7) 0.0017(5) 0.0030(6) -0.0012(5)
B2 0.0118(7) 0.0140(8) 0.0186(7) 0.0002(5) 0.0002(5) -0.0013(5)
C1 0.0195(8) 0.0215(8) 0.0197(7) -0.0013(5) 0.0017(5) 0.0021(5)
C2 0.0171(8) 0.0165(8) 0.0417(10) 0.0049(6) 0.0015(6) 0.0045(5)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
B1 N1 B2 108.73(11)
B1 N1 C1 110.89(11)
B2 N1 C1 115.71(11)
B1 N1 H1 107.0
B2 N1 H1 107.0
C1 N1 H1 107.0
C2 N2 B2 112.62(11)
C2 N2 H2A 109.1
B2 N2 H2A 109.1
C2 N2 H2B 109.1
B2 N2 H2B 109.1
H2A N2 H2B 107.8
N1 B1 H1A 109.5
N1 B1 H1B 109.5
H1A B1 H1B 109.5
N1 B1 H1C 109.5
H1A B1 H1C 109.5
H1B B1 H1C 109.5
N1 B2 N2 109.14(10)
N1 B2 H2C 109.9
N2 B2 H2C 109.9
N1 B2 H2D 109.9
N2 B2 H2D 109.9
H2C B2 H2D 108.3
N1 C1 H1D 109.5
N1 C1 H1E 109.5
H1D C1 H1E 109.5
N1 C1 H1F 109.5
H1D C1 H1F 109.5
H1E C1 H1F 109.5
N2 C2 H2E 109.5
N2 C2 H2F 109.5
H2E C2 H2F 109.5
N2 C2 H2G 109.5
H2E C2 H2G 109.5
H2F C2 H2G 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 B1 1.4887(19)
N1 B2 1.5730(19)
N1 C1 1.5906(19)
N1 H1 0.9300
N2 C2 1.4822(19)
N2 B2 1.5864(19)
N2 H2A 0.9200
N2 H2B 0.9200
B1 H1A 0.9800
B1 H1B 0.9800
B1 H1C 0.9800
B2 H2C 0.9900
B2 H2D 0.9900
C1 H1D 0.9800
C1 H1E 0.9800
C1 H1F 0.9800
C2 H2E 0.9800
C2 H2F 0.9800
C2 H2G 0.9800
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
B1 N1 B2 N2 175.90(10)
C1 N1 B2 N2 50.36(15)
C2 N2 B2 N1 174.70(12)
