#------------------------------------------------------------------------------
#$Date: 2016-02-16 02:10:39 +0100 (mar 16 de feb de 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/00/53/7005374.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_7005374
loop_
_publ_author_name
'Wann, Derek A.'
'Blockhuys, Frank'
'Van Alsenoy, Christian'
'Robertson, Heather E.'
'Himmel, Hans-Jörg'
'Tang, Christina Y.'
'Cowley, Andrew R.'
'Downs, Anthony J.'
'Rankin, David W. H.'
_publ_section_title
;
 Molecular structures of free quinuclidine and its adducts with metal
 trihydrides, MH3 (M=B, Al or Ga), studied by gas-phase electron
 diffraction, X-ray diffraction and quantum chemical calculations.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              1687
_journal_page_last               1696
_journal_paper_doi               10.1039/b701476g
_journal_year                    2007
_chemical_absolute_configuration unk
_chemical_compound_source
;
synthesis as described
;
_chemical_formula_moiety         ' C7 H16 B N '
_chemical_formula_sum            'C7 H16 B N'
_chemical_formula_weight         125.02
_chemical_name_systematic
;
?
;
_space_group_IT_number           198
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P 21 3'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.2919(4)
_cell_length_b                   9.2919(4)
_cell_length_c                   9.2919(4)
_cell_measurement_reflns_used    2063
_cell_measurement_temperature    150
_cell_measurement_theta_max      28
_cell_measurement_theta_min      5
_cell_volume                     802.26(6)
_computing_cell_refinement
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_data_collection
;
KappaCCD software 'Collect' (Nonius, 2000)
;
_computing_data_reduction
;
KappaCCD software 'DENZO' (Otwinowski & Minor, 1996)
;
_computing_publication_material
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_refinement
;
CRYSTALS (Watkin et al, 2001)
;
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type
;
Nonius KappaCCD
;
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2063
_diffrn_reflns_theta_full        27.421
_diffrn_reflns_theta_max         27.421
_diffrn_reflns_theta_min         5.375
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.058
_exptl_absorpt_correction_T_max  0.99
_exptl_absorpt_correction_T_min  0.98
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Denzo/Scalepack (Otwinowski & Minor, 1996)
;
_exptl_crystal_colour            ' colourless '
_exptl_crystal_density_diffrn    1.035
_exptl_crystal_description       ' octahedron '
_exptl_crystal_F_000             280
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.18
_exptl_crystal_thermal_history
;
The material was crystallised at ambient temperature. A suitable crystal
was cooled rapidly to 150K for single-crystal X-ray diffraction analysis.
;
_refine_diff_density_max         0.10
_refine_diff_density_min         -0.10
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   1.1445
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     32
_refine_ls_number_reflns         274
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0333
_refine_ls_shift/su_max          0.002192
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982)
[weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)]
where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)²]²
Ai are:
0.330 0.031 0.112
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0471
_refine_ls_wR_factor_gt          0.0354
_refine_ls_wR_factor_ref         0.0354
_reflns_limit_h_max              8
_reflns_limit_h_min              0
_reflns_limit_k_max              8
_reflns_limit_k_min              0
_reflns_limit_l_max              12
_reflns_limit_l_min              2
_reflns_number_gt                274
_reflns_number_total             354
_reflns_threshold_expression     I>3.00u(I)
_cod_data_source_file            b701476g.txt
_cod_data_source_block           arc1344
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Cubic' changed to 'cubic' according to
'/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_sg_symbol_H-M      'P 21 3 '
_cod_original_formula_sum        ' C7 H16 B N '
_cod_database_code               7005374
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
y,z,x
z,x,y
x+1/2,-y+1/2,-z
y+1/2,-z+1/2,-x
z+1/2,-x+1/2,-y
-y,z+1/2,-x+1/2
-z,x+1/2,-y+1/2
-z+1/2,-x,y+1/2
-x+1/2,-y,z+1/2
-y+1/2,-z,x+1/2
-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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
B1 B 0.5879(2) 0.0879(2) 0.4121(2) 0.0420 1.0000 Uani S T
N1 N 0.68782(14) 0.18782(14) 0.31218(14) 0.0256 1.0000 Uani S T
C1 C 0.67891(19) 0.34236(19) 0.35833(18) 0.0323 1.0000 Uani . .
C2 C 0.7903(2) 0.43414(18) 0.2794(2) 0.0360 1.0000 Uani . .
C3 C 0.84827(19) 0.34827(19) 0.15173(19) 0.0340 1.0000 Uani S T
H1 H 0.597(3) -0.025(3) 0.362(2) 0.058(7) 1.0000 Uiso . .
H11 H 0.6969 0.3485 0.4643 0.0388 1.0000 Uiso . .
H12 H 0.5805 0.3800 0.3365 0.0388 1.0000 Uiso . .
H21 H 0.8710 0.4586 0.3462 0.0432 1.0000 Uiso . .
H22 H 0.7442 0.5248 0.2441 0.0432 1.0000 Uiso . .
H31 H 0.9104 0.4104 0.0896 0.0408 1.0000 Uiso . .
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
B1 0.0420(10) 0.0420(10) 0.0420(10) 0.0084(10) 0.0084(10) -0.0084(10)
N1 0.0256(5) 0.0256(5) 0.0256(5) -0.0023(6) -0.0023(6) 0.0023(6)
C1 0.0366(9) 0.0288(9) 0.0315(9) -0.0049(7) 0.0032(7) 0.0039(8)
C2 0.0420(11) 0.0257(9) 0.0402(10) -0.0022(7) -0.0025(9) -0.0016(8)
C3 0.0340(7) 0.0340(7) 0.0340(7) 0.0034(8) 0.0034(8) -0.0034(8)
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
'C ' 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 International_Tables_Vol_IV_Table_2.2B
'H ' 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 International_Tables_Vol_IV_Table_2.2B
'B ' 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 International_Tables_Vol_IV_Table_2.2B
'N ' 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 International_Tables_Vol_IV_Table_2.2B
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
N1 . B1 . H1 . 104.5(12) no
N1 . B1 . H1 5_556 104.5(12) no
H1 . B1 . H1 5_556 114.0(10) no
N1 . B1 . H1 8_645 104.5(12) no
H1 . B1 . H1 8_645 114.0(10) no
H1 5_556 B1 . H1 8_645 114.0(10) no
B1 . N1 . C1 . 110.83(11) yes
B1 . N1 . C1 5_556 110.83(11) yes
C1 . N1 . C1 5_556 108.08(11) yes
B1 . N1 . C1 8_645 110.83(11) yes
C1 . N1 . C1 8_645 108.08(11) yes
C1 5_556 N1 . C1 8_645 108.08(11) yes
N1 . C1 . C2 . 111.06(15) yes
N1 . C1 . H11 . 109.074 no
C2 . C1 . H11 . 109.074 no
N1 . C1 . H12 . 109.075 no
C2 . C1 . H12 . 109.075 no
H11 . C1 . H12 . 109.467 no
C1 . C2 . C3 . 108.66(16) yes
C1 . C2 . H21 . 109.675 no
C3 . C2 . H21 . 109.675 no
C1 . C2 . H22 . 109.675 no
C3 . C2 . H22 . 109.675 no
H21 . C2 . H22 . 109.467 no
C2 . C3 . C2 5_556 108.42(13) yes
C2 . C3 . C2 8_645 108.42(13) yes
C2 5_556 C3 . C2 8_645 108.42(13) yes
C2 . C3 . H31 . 110.506 no
C2 5_556 C3 . H31 . 110.506 no
C2 8_645 C3 . H31 . 110.506 no
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
B1 . N1 . 1.608(5) yes
B1 . H1 . 1.15(2) no
B1 . H1 5_556 1.15(2) no
B1 . H1 8_645 1.15(2) no
N1 . C1 . 1.5009(18) yes
N1 . C1 5_556 1.5009(18) yes
N1 . C1 8_645 1.5009(18) yes
C1 . C2 . 1.529(2) yes
C1 . H11 . 1.000 no
C1 . H12 . 1.000 no
C2 . C3 . 1.528(2) yes
C2 . H21 . 1.000 no
C2 . H22 . 1.000 no
C3 . H31 . 1.000 no
