#------------------------------------------------------------------------------
#$Date: 2016-02-16 03:10:39 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176453 $
#$URL: svn://www.crystallography.net/cod/cif/7/01/09/7010981.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_7010981
loop_
_publ_author_name
'Paul A. Cameron'
'Vernon C. Gibson'
'Carl Redshaw'
'John A. Segal'
'Andrew J. P. White'
'David J. Williams'
_publ_section_title
;
 Synthesis and characterisation of neutral and cationic alkyl aluminium
 complexes bearing N,O-Schiff base chelates with pendant donor arms
;
_journal_issue                   3
_journal_name_full               'J. Chem. Soc., Dalton Trans.'
_journal_page_first              415
_journal_page_last               422
_journal_paper_doi               10.1039/b106131n
_journal_year                    2002
_chemical_formula_sum            'C21 H37 Al N2 O'
_chemical_formula_weight         360.51
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.984(12)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.332(2)
_cell_length_b                   24.982(4)
_cell_length_c                   9.729(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.46
_cell_measurement_theta_min      4.64
_cell_volume                     2257.4(8)
_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      293(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0963
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            3134
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        43.58
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.100
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.061
_exptl_crystal_description       'platy needles'
_exptl_crystal_F_000             792
_exptl_crystal_size_max          0.93
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.260
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   0.993
_refine_ls_goodness_of_fit_obs   1.082
_refine_ls_matrix_type           full
_refine_ls_number_parameters     226
_refine_ls_number_reflns         2534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_restrained_S_obs      1.082
_refine_ls_R_factor_all          0.1359
_refine_ls_R_factor_obs          0.0673
_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)+(0.0963P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1994
_refine_ls_wR_factor_obs         0.1557
_reflns_number_observed          1646
_reflns_number_total             2934
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            b106131n.txt
_cod_data_source_block           VG9808
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0963P)^2^+0.0000P] 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^)+(0.0963P)^2^+0.0000P] 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        2257.4(7)
_cod_original_sg_symbol_H-M      P2(1)/c
_cod_original_formula_sum        'C21 H37 N2 O Al'
_cod_database_code               7010981
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_thermal_displace_type
_atom_site_occupancy
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_group
Al Al 0.1911(2) 0.00561(6) 0.3436(2) 0.0397(4) Uani 1 d . .
N1 N 0.2132(5) -0.0898(2) 0.3854(5) 0.0521(12) Uani 1 d . .
C2 C 0.1317(7) -0.1083(2) 0.2279(7) 0.057(2) Uani 1 d . .
H2A H 0.1211(7) -0.1469(2) 0.2268(7) 0.069 Uiso 1 calc R .
H2B H 0.1835(7) -0.0994(2) 0.1686(7) 0.069 Uiso 1 calc R .
C3 C -0.0143(6) -0.0825(2) 0.1578(7) 0.057(2) Uani 1 d . .
H3A H -0.0578(6) -0.0869(2) 0.0476(7) 0.069 Uiso 1 calc R .
H3B H -0.0764(6) -0.0993(2) 0.1964(7) 0.069 Uiso 1 calc R .
N4 N 0.0014(4) -0.0245(2) 0.1970(5) 0.0438(11) Uani 1 d . .
C5 C -0.1168(5) 0.0028(2) 0.1408(6) 0.0425(12) Uani 1 d . .
H5A H -0.2014(5) -0.0164(2) 0.0885(6) 0.051 Uiso 1 calc R .
C6 C -0.1321(5) 0.0596(2) 0.1504(6) 0.0408(12) Uani 1 d . .
C7 C -0.2721(6) 0.0803(2) 0.0875(6) 0.0493(14) Uani 1 d . .
H7A H -0.3499(6) 0.0569(2) 0.0495(6) 0.059 Uiso 1 calc R .
C8 C -0.2974(6) 0.1352(2) 0.0804(6) 0.0474(13) Uani 1 d . .
C9 C -0.1733(6) 0.1676(2) 0.1458(7) 0.0507(14) Uani 1 d . .
H9A H -0.1875(6) 0.2043(2) 0.1455(7) 0.061 Uiso 1 calc R .
C10 C -0.0339(6) 0.1499(2) 0.2097(6) 0.0415(12) Uani 1 d . .
C11 C -0.0105(5) 0.0932(2) 0.2150(6) 0.0378(12) Uani 1 d . .
O12 O 0.1197(3) 0.07316(13) 0.2705(5) 0.0475(10) Uani 1 d . .
C13 C 0.2268(7) 0.0161(2) 0.5589(7) 0.0580(15) Uani 1 d . .
H13A H 0.1379(7) 0.0124(2) 0.5672(7) 0.087 Uiso 1 d R .
H13B H 0.2657(7) 0.0512(2) 0.5920(7) 0.087 Uiso 1 d R .
H13C H 0.2941(7) -0.0103(2) 0.6220(7) 0.087 Uiso 1 d R .
C14 C 0.3448(5) 0.0054(2) 0.2746(6) 0.0515(13) Uani 1 d . .
H14A H 0.4363(5) 0.0000(2) 0.3609(6) 0.077 Uiso 1 d R .
H14B H 0.3452(5) 0.0391(2) 0.2273(6) 0.077 Uiso 1 d R .
H14C H 0.3275(5) -0.0230(2) 0.2021(6) 0.077 Uiso 1 d R .
C15 C 0.3613(7) -0.1099(3) 0.4462(10) 0.084(2) Uani 1 d . .
H15A H 0.4052(7) -0.0975(3) 0.3832(10) 0.127 Uiso 1 calc R .
H15B H 0.3603(7) -0.1484(3) 0.4464(10) 0.127 Uiso 1 calc R .
H15C H 0.4153(7) -0.0971(3) 0.5488(10) 0.127 Uiso 1 calc R .
C16 C 0.1456(9) -0.1084(2) 0.4799(8) 0.074(2) Uani 1 d . .
H16A H 0.1999(9) -0.0961(2) 0.5829(8) 0.112 Uiso 1 calc R .
H16B H 0.1429(9) -0.1469(2) 0.4789(8) 0.112 Uiso 1 calc R .
H16C H 0.0492(9) -0.0947(2) 0.4403(8) 0.112 Uiso 1 calc R .
C17 C -0.4474(6) 0.1597(3) 0.0106(7) 0.060(2) Uani 1 d . .
C18 C -0.5640(8) 0.1184(4) -0.0403(15) 0.138(5) Uani 1 d . .
H18A H -0.5541(8) 0.0950(4) -0.1134(15) 0.207 Uiso 1 calc R .
H18B H -0.6561(8) 0.1358(4) -0.0866(15) 0.207 Uiso 1 calc R .
H18C H -0.5566(8) 0.0980(4) 0.0464(15) 0.207 Uiso 1 calc R .
C19 C -0.4671(10) 0.1953(5) 0.1245(12) 0.132(4) Uani 1 d . .
H19A H -0.3935(10) 0.2223(5) 0.1593(12) 0.198 Uiso 1 calc R .
H19B H -0.4605(10) 0.1743(5) 0.2100(12) 0.198 Uiso 1 calc R .
H19C H -0.5600(10) 0.2121(5) 0.0770(12) 0.198 Uiso 1 calc R .
C20 C -0.4639(11) 0.1933(5) -0.1266(12) 0.143(5) Uani 1 d . .
H20A H -0.3893(11) 0.2199(5) -0.0948(12) 0.214 Uiso 1 calc R .
H20B H -0.5562(11) 0.2106(5) -0.1690(12) 0.214 Uiso 1 calc R .
H20C H -0.4565(11) 0.1706(5) -0.2026(12) 0.214 Uiso 1 calc R .
C21 C 0.0965(6) 0.1876(2) 0.2793(7) 0.0488(14) Uani 1 d . .
C22 C 0.1921(7) 0.1816(2) 0.1965(9) 0.070(2) Uani 1 d . .
H22A H 0.2729(7) 0.2054(2) 0.2413(9) 0.106 Uiso 1 calc R .
H22B H 0.1375(7) 0.1903(2) 0.0903(9) 0.106 Uiso 1 calc R .
H22C H 0.2259(7) 0.1454(2) 0.2059(9) 0.106 Uiso 1 calc R .
C23 C 0.1834(7) 0.1768(3) 0.4517(8) 0.068(2) Uani 1 d . .
H23A H 0.1217(7) 0.1807(3) 0.5016(8) 0.102 Uiso 1 calc R .
H23B H 0.2614(7) 0.2018(3) 0.4943(8) 0.102 Uiso 1 calc R .
H23C H 0.2210(7) 0.1410(3) 0.4668(8) 0.102 Uiso 1 calc R .
C24 C 0.0469(7) 0.2471(2) 0.2613(9) 0.077(2) Uani 1 d . .
H24A H -0.0136(7) 0.2525(2) 0.3120(9) 0.115 Uiso 1 calc R .
H24B H -0.0060(7) 0.2555(2) 0.1547(9) 0.115 Uiso 1 calc R .
H24C H 0.1296(7) 0.2700(2) 0.3062(9) 0.115 Uiso 1 calc R .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 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'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Al Al 0.0645 0.0514 '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
O12 Al C14 96.6(2) . . ?
O12 Al C13 98.3(2) . . ?
C14 Al C13 123.7(3) . . ?
O12 Al N4 88.2(2) . . ?
C14 Al N4 116.0(2) . . ?
C13 Al N4 118.4(2) . . ?
O12 Al N1 163.0(2) . . ?
C14 Al N1 91.4(2) . . ?
C13 Al N1 89.5(2) . . ?
N4 Al N1 74.9(2) . . ?
C16 N1 C2 110.2(5) . . ?
C16 N1 C15 110.0(6) . . ?
C2 N1 C15 109.5(5) . . ?
C16 N1 Al 112.7(4) . . ?
C2 N1 Al 99.6(3) . . ?
C15 N1 Al 114.3(4) . . ?
N1 C2 C3 110.0(5) . . ?
N4 C3 C2 109.1(4) . . ?
C5 N4 C3 115.4(4) . . ?
C5 N4 Al 123.5(3) . . ?
C3 N4 Al 120.8(3) . . ?
N4 C5 C6 127.2(4) . . ?
C7 C6 C11 121.6(5) . . ?
C7 C6 C5 117.3(5) . . ?
C11 C6 C5 121.1(4) . . ?
C8 C7 C6 121.4(5) . . ?
C7 C8 C9 115.4(5) . . ?
C7 C8 C17 123.4(5) . . ?
C9 C8 C17 121.2(5) . . ?
C10 C9 C8 126.0(5) . . ?
C9 C10 C11 117.6(5) . . ?
C9 C10 C21 123.1(5) . . ?
C11 C10 C21 119.2(4) . . ?
O12 C11 C6 120.7(4) . . ?
O12 C11 C10 121.3(4) . . ?
C6 C11 C10 118.0(4) . . ?
C11 O12 Al 132.1(3) . . ?
C18 C17 C19 107.6(8) . . ?
C18 C17 C8 112.7(6) . . ?
C19 C17 C8 110.4(6) . . ?
C18 C17 C20 109.0(8) . . ?
C19 C17 C20 108.7(8) . . ?
C8 C17 C20 108.3(6) . . ?
C22 C21 C10 110.6(5) . . ?
C22 C21 C23 110.7(5) . . ?
C10 C21 C23 110.6(5) . . ?
C22 C21 C24 106.9(5) . . ?
C10 C21 C24 110.7(5) . . ?
C23 C21 C24 107.2(5) . . ?
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 O12 1.854(4) . ?
Al C14 1.976(5) . ?
Al C13 1.978(6) . ?
Al N4 1.998(4) . ?
Al N1 2.413(5) . ?
N1 C16 1.453(8) . ?
N1 C2 1.463(8) . ?
N1 C15 1.466(8) . ?
C2 C3 1.502(8) . ?
C3 N4 1.488(7) . ?
N4 C5 1.294(6) . ?
C5 C6 1.434(7) . ?
C6 C7 1.399(7) . ?
C6 C11 1.409(7) . ?
C7 C8 1.392(8) . ?
C8 C9 1.410(8) . ?
C8 C17 1.521(8) . ?
C9 C10 1.368(8) . ?
C10 C11 1.433(7) . ?
C10 C21 1.538(7) . ?
C11 O12 1.310(6) . ?
C17 C18 1.495(11) . ?
C17 C19 1.504(11) . ?
C17 C20 1.522(11) . ?
C21 C22 1.531(9) . ?
C21 C23 1.541(9) . ?
C21 C24 1.556(8) . ?
