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.
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.; Dalton transactions (Cambridge, England : 2003)  (2007) 1687–1696; doi:10.1039/b701476g

data_7005374
_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
_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       \w
_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/[A~0~*T~0~(x)+A~1~*T~1~(x) ... +A~n-1~]*T~n-1~(x)]
where A~i~ are the Chebychev coefficients listed below and x= Fcalc/Fmax
Method = Robust Weighting (Prince, 1982)
W = [weight] * [1-(deltaF/6*sigmaF)^2^]^2^
A~i~ 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