#------------------------------------------------------------------------------
#$Date: 2015-09-26 05:26:33 +0300 (Sat, 26 Sep 2015) $
#$Revision: 158367 $
#$URL: svn://www.crystallography.net/cod/cif/2/24/11/2241114.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/. The original data for this entry
# were provided by IUCr Journals, http://journals.iucr.org/.
#
# The file may be used within the scientific community so long as
# proper attribution is given to the journal article from which the
# data were obtained.
#
data_2241114
loop_
_publ_author_name
'Louven, Kathrin'
'Quentin, Georgina'
'Strohmann, Carsten'
_publ_section_title
;
 Crystal structure of borated
 N,N,N',N'-tetramethyldiaminomethane
;
_journal_coeditor_code           ZQ2234
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              o743
_journal_page_last               o744
_journal_paper_doi               10.1107/S2056989015016813
_journal_volume                  71
_journal_year                    2015
_chemical_formula_moiety         'C5 H17 B N2'
_chemical_formula_sum            'C5 H17 B N2'
_chemical_formula_weight         116.01
_chemical_name_systematic
;
{[(Dimethylamino)methyl]dimethylamine}trihydridoboron
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     direct
_audit_creation_method
;
Olex2 1.2
(compiled 2014.11.20 svn.r3092 for OlexSys, GUI svn.r4949)
;
_cell_angle_alpha                69.602(10)
_cell_angle_beta                 76.519(11)
_cell_angle_gamma                74.912(10)
_cell_formula_units_Z            2
_cell_length_a                   6.0464(8)
_cell_length_b                   7.6987(9)
_cell_length_c                   9.5896(11)
_cell_measurement_reflns_used    1858
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.3
_cell_measurement_theta_min      3.0
_cell_volume                     398.94(9)
_computing_cell_refinement
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_collection
;
CrysAlisPro (Agilent, 2014)
;
_computing_data_reduction
;
CrysAlisPro (Agilent, 2014)
;
_computing_molecular_graphics
;
SHELXTL (Sheldrick, 2008)
;
_computing_publication_material
;
Olex2 (Dolomanov et al.,  2009)
;
_computing_structure_refinement
;
SHELXL96 (Sheldrick, 2008)
;
_computing_structure_solution
;
SHELXS96 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      173.15
_diffrn_detector_area_resol_mean 16.0560
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'AgilentXcalibur, Sapphire3'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            3232
_diffrn_reflns_theta_full        26.000
_diffrn_reflns_theta_max         26.995
_diffrn_reflns_theta_min         3.083
_exptl_absorpt_coefficient_mu    0.057
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.983
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(CrysAlisPro; Agilent, 2014)
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_density_diffrn    0.966
_exptl_crystal_description       block
_exptl_crystal_F_000             132
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.176
_refine_diff_density_min         -0.219
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.874
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     90
_refine_ls_number_reflns         3232
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.874
_refine_ls_R_factor_all          0.0769
_refine_ls_R_factor_gt           0.0409
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0498P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.0993
_reflns_number_gt                1828
_reflns_number_total             3232
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            zq2234sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        398.95(9)
_cod_database_code               2241114
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_occupancy
N N1 0.17275(18) 0.17659(15) 0.69988(12) 0.0182(3) Uani d 1
C C3 0.2336(2) -0.00477(18) 0.82279(15) 0.0214(3) Uani d 1
H H3A 0.2756 0.0246 0.9048 0.026 Uiso calc 1
H H3B 0.0951 -0.0634 0.8648 0.026 Uiso calc 1
N N2 0.42225(19) -0.13895(16) 0.77307(13) 0.0226(3) Uani d 1
C C2 0.1062(3) 0.1356(2) 0.57701(16) 0.0274(4) Uani d 1
H H2A 0.2389 0.0568 0.5326 0.041 Uiso calc 1
H H2B 0.0591 0.2545 0.4995 0.041 Uiso calc 1
H H2C -0.0233 0.0685 0.6177 0.041 Uiso calc 1
C C1 0.3751(2) 0.2702(2) 0.63738(18) 0.0293(4) Uani d 1
H H1A 0.4230 0.2959 0.7179 0.044 Uiso calc 1
H H1B 0.3328 0.3894 0.5589 0.044 Uiso calc 1
H H1C 0.5036 0.1873 0.5939 0.044 Uiso calc 1
C C5 0.3510(3) -0.3102(2) 0.78120(19) 0.0340(4) Uani d 1
H H5A 0.2924 -0.3745 0.8861 0.051 Uiso calc 1
H H5B 0.4844 -0.3946 0.7432 0.051 Uiso calc 1
H H5C 0.2284 -0.2762 0.7197 0.051 Uiso calc 1
B B1 -0.0405(3) 0.3123(3) 0.7713(2) 0.0289(4) Uani d 1
C C4 0.6200(3) -0.1878(2) 0.85213(18) 0.0333(4) Uani d 1
H H4A 0.6693 -0.0721 0.8429 0.050 Uiso calc 1
H H4B 0.7483 -0.2698 0.8077 0.050 Uiso calc 1
H H4C 0.5749 -0.2542 0.9588 0.050 Uiso calc 1
H H1D -0.083(2) 0.4427(19) 0.6758(15) 0.032(4) Uiso d 1
H H1E -0.189(2) 0.2332(19) 0.8155(16) 0.034(4) Uiso d 1
H H1F 0.023(2) 0.3383(19) 0.8634(17) 0.036(4) Uiso d 1
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
C3 N1 B1 108.16(10)
C2 N1 C3 109.62(10)
C2 N1 B1 110.43(11)
C1 N1 C3 110.11(10)
C1 N1 C2 108.59(10)
C1 N1 B1 109.93(12)
N1 C3 H3A 108.8
N1 C3 H3B 108.8
H3A C3 H3B 107.7
N2 C3 N1 113.61(10)
N2 C3 H3A 108.8
N2 C3 H3B 108.8
C3 N2 C5 112.85(12)
C3 N2 C4 112.82(11)
C4 N2 C5 110.31(11)
N1 C2 H2A 109.5
N1 C2 H2B 109.5
N1 C2 H2C 109.5
H2A C2 H2B 109.5
H2A C2 H2C 109.5
H2B C2 H2C 109.5
N1 C1 H1A 109.5
N1 C1 H1B 109.5
N1 C1 H1C 109.5
H1A C1 H1B 109.5
H1A C1 H1C 109.5
H1B C1 H1C 109.5
N2 C5 H5A 109.5
N2 C5 H5B 109.5
N2 C5 H5C 109.5
H5A C5 H5B 109.5
H5A C5 H5C 109.5
H5B C5 H5C 109.5
N1 B1 H1D 105.7(7)
N1 B1 H1E 106.1(7)
N1 B1 H1F 106.4(7)
H1D B1 H1E 111.1(10)
H1D B1 H1F 113.7(10)
H1E B1 H1F 113.2(10)
N2 C4 H4A 109.5
N2 C4 H4B 109.5
N2 C4 H4C 109.5
H4A C4 H4B 109.5
H4A C4 H4C 109.5
H4B C4 H4C 109.5
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
N1 C3 1.5039(16)
N1 C2 1.4818(17)
N1 C1 1.4806(17)
N1 B1 1.615(2)
C3 H3A 0.9900
C3 H3B 0.9900
C3 N2 1.4393(17)
N2 C5 1.4622(18)
N2 C4 1.4612(18)
C2 H2A 0.9800
C2 H2B 0.9800
C2 H2C 0.9800
C1 H1A 0.9800
C1 H1B 0.9800
C1 H1C 0.9800
C5 H5A 0.9800
C5 H5B 0.9800
C5 H5C 0.9800
B1 H1D 1.117(13)
B1 H1E 1.131(14)
B1 H1F 1.137(14)
C4 H4A 0.9800
C4 H4B 0.9800
C4 H4C 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
N1 C3 N2 C5 -114.53(13)
N1 C3 N2 C4 119.61(12)
C2 N1 C3 N2 59.36(14)
C1 N1 C3 N2 -60.04(14)
B1 N1 C3 N2 179.82(13)

_cod_database_fobs_code 2241114
