#------------------------------------------------------------------------------
#$Date: 2016-02-16 21:30:59 +0100 (mar 16 de feb de 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/31/93/4319309.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_4319309
loop_
_publ_author_name
'Vernon C. Gibson'
'Sergio Mastroianni'
'Andrew J. P. White'
'David J. Williams'
_publ_section_title
;
 Formation and Unexpected Catalytic Reactivity of Organoaluminum
 Boryloxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              826
_journal_page_last               827
_journal_paper_doi               10.1021/ic000895g
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C40 H56 Al2 B2 O2'
_chemical_formula_weight         644.43
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 113.89(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.1456(12)
_cell_length_b                   16.4011(14)
_cell_length_c                   11.5273(14)
_cell_measurement_reflns_used    22
_cell_measurement_temperature    203(2)
_cell_measurement_theta_max      27.82
_cell_measurement_theta_min      5.03
_cell_volume                     1926.7(5)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      203(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       'ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0580
_diffrn_reflns_av_sigmaI/netI    0.0400
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -5
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -5
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            2955
_diffrn_reflns_theta_max         60.01
_diffrn_reflns_theta_min         5.11
_diffrn_standards_decay_%        2.88
_diffrn_standards_interval_count 797
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.910
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Clear
_exptl_crystal_density_diffrn    1.111
_exptl_crystal_description       Rhombs
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.37
_refine_diff_density_max         0.235
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.051
_refine_ls_extinction_coef       0.0109(27)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.060
_refine_ls_goodness_of_fit_obs   1.112
_refine_ls_matrix_type           full
_refine_ls_number_parameters     209
_refine_ls_number_reflns         2819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.083
_refine_ls_restrained_S_obs      1.112
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_obs          0.0648
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1116P)²+0.8791P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1929
_refine_ls_wR_factor_obs         0.1734
_reflns_number_observed          2166
_reflns_number_total             2833
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000895g_2.cif
_cod_data_source_block           VG9712
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+0.8791P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.1116P)^2^+0.8791P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        1926.7(4)
_cod_original_formula_sum        'C40 H56 B2 O2 Al2'
_cod_database_code               4319309
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Al Al 0.59159(9) 0.50041(7) 0.44215(9) 0.0470(4) Uani 1 d . .
O O 0.5694(2) 0.45187(13) 0.5795(2) 0.0423(6) Uani 1 d . .
B B 0.6452(3) 0.3976(2) 0.6730(3) 0.0396(9) Uani 1 d . .
C1 C 0.7429(3) 0.5703(3) 0.4822(4) 0.0678(12) Uani 1 d . .
H1A H 0.7442(3) 0.5918(3) 0.4043(4) 0.102 Uiso 1 calc R .
H1B H 0.8222(3) 0.5391(3) 0.5270(4) 0.102 Uiso 1 calc R .
H1C H 0.7381(3) 0.6150(3) 0.5352(4) 0.102 Uiso 1 calc R .
C2 C 0.5595(3) 0.4208(3) 0.3084(4) 0.0625(11) Uani 1 d . .
H2A H 0.5712(3) 0.4463(3) 0.2377(4) 0.094 Uiso 1 calc R .
H2B H 0.4705(3) 0.4004(3) 0.2802(4) 0.094 Uiso 1 calc R .
H2C H 0.6209(3) 0.3759(3) 0.3404(4) 0.094 Uiso 1 calc R .
C3 C 0.8004(3) 0.3996(2) 0.7176(3) 0.0378(8) Uani 1 d . .
C4 C 0.8760(3) 0.4684(2) 0.7777(3) 0.0420(8) Uani 1 d . .
C5 C 1.0126(3) 0.4656(2) 0.8191(3) 0.0457(8) Uani 1 d . .
H5A H 1.0618(3) 0.5117(2) 0.8597(3) 0.055 Uiso 1 calc R .
C6 C 1.0774(3) 0.3990(2) 0.8031(3) 0.0449(8) Uani 1 d . .
C7 C 1.0033(3) 0.3314(2) 0.7431(3) 0.0459(8) Uani 1 d . .
H7A H 1.0459(3) 0.2851(2) 0.7299(3) 0.055 Uiso 1 calc R .
C8 C 0.8670(3) 0.3306(2) 0.7019(3) 0.0408(8) Uani 1 d . .
C9 C 0.8178(3) 0.5454(2) 0.8047(3) 0.0508(9) Uani 1 d . .
H9A H 0.8567(3) 0.5919(2) 0.7827(3) 0.076 Uiso 1 d R .
H9B H 0.7246(3) 0.5460(2) 0.7564(3) 0.076 Uiso 1 d R .
H9C H 0.8344(3) 0.5475(2) 0.8931(3) 0.076 Uiso 1 d R .
C10 C 1.2253(3) 0.3978(3) 0.8481(4) 0.0619(11) Uani 1 d . .
H10A H 1.2546(3) 0.4488(3) 0.8277(4) 0.093 Uiso 1 d R .
H10B H 1.2504(3) 0.3539(3) 0.8075(4) 0.093 Uiso 1 d R .
H10C H 1.2658(3) 0.3891(3) 0.9381(4) 0.093 Uiso 1 d R .
C11 C 0.7950(3) 0.2543(2) 0.6384(4) 0.0560(10) Uani 1 d . .
H11A H 0.7472(3) 0.2333(2) 0.6850(4) 0.084 Uiso 1 d R .
H11B H 0.7354(3) 0.2662(2) 0.5529(4) 0.084 Uiso 1 d R .
H11C H 0.8565(3) 0.2141(2) 0.6357(4) 0.084 Uiso 1 d R .
C12 C 0.5748(3) 0.3360(2) 0.7293(3) 0.0397(8) Uani 1 d . .
C13 C 0.5978(3) 0.3384(2) 0.8581(3) 0.0415(8) Uani 1 d . .
C14 C 0.5450(3) 0.2792(2) 0.9101(3) 0.0455(8) Uani 1 d . .
H14A H 0.5619(3) 0.2820(2) 0.9968(3) 0.055 Uiso 1 calc R .
C15 C 0.4683(3) 0.2163(2) 0.8374(3) 0.0470(8) Uani 1 d . .
C16 C 0.4417(3) 0.2161(2) 0.7096(3) 0.0478(9) Uani 1 d . .
H16A H 0.3873(3) 0.1749(2) 0.6582(3) 0.057 Uiso 1 calc R .
C17 C 0.4919(3) 0.2742(2) 0.6537(3) 0.0435(8) Uani 1 d . .
C18 C 0.6774(3) 0.4067(2) 0.9431(3) 0.0532(9) Uani 1 d . .
H18A H 0.6367(3) 0.4583(2) 0.9110(3) 0.080 Uiso 1 d R .
H18B H 0.6829(3) 0.3987(2) 1.0276(3) 0.080 Uiso 1 d R .
H18C H 0.7648(3) 0.4061(2) 0.9463(3) 0.080 Uiso 1 d R .
C19 C 0.4145(4) 0.1513(3) 0.8944(4) 0.0649(11) Uani 1 d . .
H19A H 0.3448(4) 0.1736(3) 0.9132(4) 0.097 Uiso 1 d R .
H19B H 0.3820(4) 0.1065(3) 0.8365(4) 0.097 Uiso 1 d R .
H19C H 0.4829(4) 0.1312(3) 0.9709(4) 0.097 Uiso 1 d R .
C20 C 0.4576(4) 0.2647(2) 0.5131(3) 0.0588(10) Uani 1 d . .
H20A H 0.5097(4) 0.2218(2) 0.5004(3) 0.088 Uiso 1 d R .
H20B H 0.3661(4) 0.2518(2) 0.4692(3) 0.088 Uiso 1 d R .
H20C H 0.4742(4) 0.3149(2) 0.4794(3) 0.088 Uiso 1 d R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.2130 0.2455 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O Al O 81.02(10) . 3_666 ?
O Al C1 116.76(14) . . ?
O Al C1 118.6(2) 3_666 . ?
O Al C2 109.91(15) . . ?
O Al C2 108.43(13) 3_666 . ?
C1 Al C2 116.8(2) . . ?
O Al Al 40.56(7) . 3_666 ?
O Al Al 40.47(7) 3_666 3_666 ?
C1 Al Al 127.65(15) . 3_666 ?
C2 Al Al 115.58(13) . 3_666 ?
B O Al 132.9(2) . . ?
B O Al 128.1(2) . 3_666 ?
Al O Al 98.98(10) . 3_666 ?
O B C12 119.0(3) . . ?
O B C3 118.5(3) . . ?
C12 B C3 122.6(3) . . ?
C8 C3 C4 117.7(3) . . ?
C8 C3 B 120.2(3) . . ?
C4 C3 B 122.0(3) . . ?
C5 C4 C3 119.5(3) . . ?
C5 C4 C9 117.1(3) . . ?
C3 C4 C9 123.3(3) . . ?
C6 C5 C4 122.9(3) . . ?
C5 C6 C7 117.9(3) . . ?
C5 C6 C10 121.8(3) . . ?
C7 C6 C10 120.3(3) . . ?
C6 C7 C8 121.5(3) . . ?
C7 C8 C3 120.5(3) . . ?
C7 C8 C11 117.7(3) . . ?
C3 C8 C11 121.7(3) . . ?
C13 C12 C17 117.9(3) . . ?
C13 C12 B 120.8(3) . . ?
C17 C12 B 121.3(3) . . ?
C14 C13 C12 120.7(3) . . ?
C14 C13 C18 118.4(3) . . ?
C12 C13 C18 120.9(3) . . ?
C15 C14 C13 121.6(3) . . ?
C16 C15 C14 117.4(3) . . ?
C16 C15 C19 121.0(3) . . ?
C14 C15 C19 121.6(3) . . ?
C15 C16 C17 122.7(3) . . ?
C16 C17 C12 119.6(3) . . ?
C16 C17 C20 116.8(3) . . ?
C12 C17 C20 123.6(3) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Al O 1.876(2) . ?
Al O 1.879(2) 3_666 ?
Al C1 1.934(4) . ?
Al C2 1.940(4) . ?
Al Al 2.855(2) 3_666 ?
O B 1.389(4) . ?
O Al 1.879(2) 3_666 ?
B C12 1.572(5) . ?
B C3 1.593(4) . ?
C3 C8 1.405(4) . ?
C3 C4 1.411(4) . ?
C4 C5 1.400(4) . ?
C4 C9 1.508(4) . ?
C5 C6 1.362(5) . ?
C6 C7 1.389(5) . ?
C6 C10 1.515(4) . ?
C7 C8 1.396(4) . ?
C8 C11 1.507(4) . ?
C12 C13 1.401(4) . ?
C12 C17 1.410(4) . ?
C13 C14 1.389(5) . ?
C13 C18 1.517(4) . ?
C14 C15 1.385(5) . ?
C15 C16 1.381(5) . ?
C15 C19 1.499(5) . ?
C16 C17 1.388(5) . ?
C17 C20 1.515(5) . ?
