#------------------------------------------------------------------------------
#$Date: 2016-02-14 06:40:26 +0200 (Sun, 14 Feb 2016) $
#$Revision: 176432 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/20/4072002.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_4072002
loop_
_publ_author_name
'Krieck, Sven'
'Görls, Helmar'
'Westerhausen, Matthias'
_publ_section_title
;
 Synthesis and Properties of Calcium Tetraorganylalanates with
 [Me4−nAlPhn]−Anions
;
_journal_issue                   19
_journal_name_full               Organometallics
_journal_page_first              5052
_journal_paper_doi               10.1021/om800509p
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C24 H48 Ca O6, 2(C9 H14 Al), 2(C7 H8)'
_chemical_formula_sum            'C56 H92 Al2 Ca O6'
_chemical_formula_weight         955.34
_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-97
_cell_angle_alpha                90.00
_cell_angle_beta                 93.245(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.5891(3)
_cell_length_b                   16.7864(3)
_cell_length_c                   13.8631(3)
_cell_measurement_reflns_used    20524
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      2.45
_cell_volume                     2924.93(11)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0373
_diffrn_reflns_av_sigmaI/netI    0.0389
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            20524
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.45
_exptl_absorpt_coefficient_mu    0.181
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1044
_exptl_crystal_size_max          0.04
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.490
_refine_diff_density_min         -0.312
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.992
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6676
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.992
_refine_ls_R_factor_all          0.0678
_refine_ls_R_factor_gt           0.0455
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0613P)²+1.0066P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1254
_reflns_number_gt                5121
_reflns_number_total             6676
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800509p_si_001.cif
_cod_data_source_block           FO3399
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'NONE' changed to 'none'
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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_Hall     -P2yn
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               4072002
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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Al Al -0.02224(4) 0.25602(3) -0.07852(4) 0.03630(14) Uani 1 1 d .
C1 C 0.11408(16) 0.19983(13) -0.10354(17) 0.0577(5) Uani 1 1 d .
H1A H 0.1678 0.2124 -0.0518 0.087 Uiso 1 1 calc R
H1B H 0.1393 0.2174 -0.1657 0.087 Uiso 1 1 calc R
H1C H 0.1018 0.1422 -0.1054 0.087 Uiso 1 1 calc R
C2 C -0.07307(17) 0.22175(14) 0.04887(14) 0.0557(5) Uani 1 1 d .
H2A H -0.0210 0.2376 0.1005 0.084 Uiso 1 1 calc R
H2B H -0.0816 0.1637 0.0494 0.084 Uiso 1 1 calc R
H2C H -0.1416 0.2471 0.0592 0.084 Uiso 1 1 calc R
C3 C -0.00599(16) 0.37426(11) -0.08623(15) 0.0487(4) Uani 1 1 d .
H3A H 0.0333 0.3936 -0.0278 0.073 Uiso 1 1 calc R
H3B H -0.0765 0.3992 -0.0916 0.073 Uiso 1 1 calc R
H3C H 0.0332 0.3879 -0.1431 0.073 Uiso 1 1 calc R
C4 C -0.13348(14) 0.22610(10) -0.18310(12) 0.0369(4) Uani 1 1 d .
C5 C -0.11779(17) 0.16982(13) -0.25415(15) 0.0563(5) Uani 1 1 d .
H5A H -0.0517 0.1424 -0.2529 0.068 Uiso 1 1 calc R
C6 C -0.1941(2) 0.15162(18) -0.32702(18) 0.0791(8) Uani 1 1 d .
H6A H -0.1789 0.1132 -0.3746 0.095 Uiso 1 1 calc R
C7 C -0.2910(2) 0.18864(18) -0.33081(17) 0.0728(7) Uani 1 1 d .
H7A H -0.3433 0.1762 -0.3806 0.087 Uiso 1 1 calc R
C8 C -0.31145(18) 0.24368(15) -0.26194(17) 0.0629(6) Uani 1 1 d .
H8A H -0.3787 0.2695 -0.2632 0.075 Uiso 1 1 calc R
C9 C -0.23380(16) 0.26213(12) -0.18969(15) 0.0503(5) Uani 1 1 d .
H9A H -0.2498 0.3009 -0.1428 0.060 Uiso 1 1 calc R
Ca Ca 0.5000 0.0000 0.0000 0.02545(11) Uani 1 2 d S
O1 O 0.43495(9) 0.03390(7) -0.15583(8) 0.0351(3) Uani 1 1 d .
O2 O 0.52079(10) 0.13585(7) 0.03505(9) 0.0418(3) Uani 1 1 d .
O3 O 0.32949(9) 0.00866(7) 0.05781(9) 0.0387(3) Uani 1 1 d .
C10 C 0.32542(14) 0.05523(12) -0.18447(14) 0.0463(4) Uani 1 1 d .
H10A H 0.2904 0.0807 -0.1303 0.056 Uiso 1 1 calc R
H10B H 0.2841 0.0075 -0.2053 0.056 Uiso 1 1 calc R
C11 C 0.33381(17) 0.11258(12) -0.26707(13) 0.0491(5) Uani 1 1 d .
H11A H 0.3493 0.1673 -0.2436 0.059 Uiso 1 1 calc R
H11B H 0.2679 0.1131 -0.3095 0.059 Uiso 1 1 calc R
C12 C 0.42649(17) 0.07820(13) -0.31862(13) 0.0528(5) Uani 1 1 d .
H12A H 0.4034 0.0331 -0.3608 0.063 Uiso 1 1 calc R
H12B H 0.4603 0.1193 -0.3580 0.063 Uiso 1 1 calc R
C13 C 0.50131(15) 0.05057(12) -0.23657(12) 0.0452(4) Uani 1 1 d .
H13A H 0.5397 0.0020 -0.2552 0.054 Uiso 1 1 calc R
H13B H 0.5541 0.0925 -0.2188 0.054 Uiso 1 1 calc R
C14 C 0.4924(2) 0.19978(12) -0.03163(18) 0.0720(7) Uani 1 1 d .
H14A H 0.4145 0.2004 -0.0460 0.086 Uiso 1 1 calc R
H14B H 0.5276 0.1918 -0.0930 0.086 Uiso 1 1 calc R
C15 C 0.5264(3) 0.27456(14) 0.0121(2) 0.0803(8) Uani 1 1 d .
H15A H 0.4648 0.3041 0.0355 0.096 Uiso 1 1 calc R
H15B H 0.5621 0.3082 -0.0349 0.096 Uiso 1 1 calc R
C16 C 0.6029(2) 0.25198(12) 0.0954(2) 0.0673(6) Uani 1 1 d .
H16A H 0.6769 0.2500 0.0749 0.081 Uiso 1 1 calc R
H16B H 0.5990 0.2902 0.1495 0.081 Uiso 1 1 calc R
C17 C 0.56549(19) 0.17107(12) 0.12379(15) 0.0573(5) Uani 1 1 d .
H17A H 0.6256 0.1387 0.1513 0.069 Uiso 1 1 calc R
H17B H 0.5109 0.1753 0.1722 0.069 Uiso 1 1 calc R
C18 C 0.28544(15) 0.07680(12) 0.10706(16) 0.0506(5) Uani 1 1 d .
H18A H 0.2781 0.1232 0.0631 0.061 Uiso 1 1 calc R
H18B H 0.3317 0.0919 0.1643 0.061 Uiso 1 1 calc R
C19 C 0.1786(2) 0.04959(17) 0.1366(3) 0.0888(10) Uani 1 1 d .
H19A H 0.1837 0.0273 0.2029 0.107 Uiso 1 1 calc R
H19B H 0.1271 0.0942 0.1343 0.107 Uiso 1 1 calc R
C20 C 0.14595(16) -0.01315(14) 0.0644(2) 0.0690(7) Uani 1 1 d .
H20A H 0.0943 -0.0507 0.0908 0.083 Uiso 1 1 calc R
H20B H 0.1144 0.0107 0.0041 0.083 Uiso 1 1 calc R
C21 C 0.24895(15) -0.05354(13) 0.04764(19) 0.0585(6) Uani 1 1 d .
H21A H 0.2635 -0.0963 0.0958 0.070 Uiso 1 1 calc R
H21B H 0.2474 -0.0772 -0.0179 0.070 Uiso 1 1 calc R
C1T C 0.83095(15) 0.01709(11) 0.43196(13) 0.0440(4) Uani 1 1 d .
C2T C 0.78548(16) 0.08890(12) 0.40472(16) 0.0530(5) Uani 1 1 d .
H2TA H 0.7278 0.1092 0.4386 0.064 Uiso 1 1 calc R
C3T C 0.8230(2) 0.13178(13) 0.32831(19) 0.0673(7) Uani 1 1 d .
H3TA H 0.7909 0.1811 0.3099 0.081 Uiso 1 1 calc R
C4T C 0.9065(2) 0.10307(16) 0.27920(18) 0.0720(7) Uani 1 1 d .
H4TA H 0.9323 0.1322 0.2266 0.086 Uiso 1 1 calc R
C5T C 0.9521(2) 0.03257(17) 0.3064(2) 0.0717(7) Uani 1 1 d .
H5TA H 1.0100 0.0125 0.2727 0.086 Uiso 1 1 calc R
C6T C 0.91541(17) -0.00974(13) 0.38200(18) 0.0587(5) Uani 1 1 d .
H6TA H 0.9488 -0.0586 0.4004 0.070 Uiso 1 1 calc R
C7T C 0.7892(2) -0.03209(16) 0.51250(17) 0.0683(6) Uani 1 1 d .
H7TA H 0.7314 -0.0033 0.5416 0.102 Uiso 1 1 calc R
H7TB H 0.8467 -0.0419 0.5617 0.102 Uiso 1 1 calc R
H7TC H 0.7624 -0.0830 0.4866 0.102 Uiso 1 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'
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'
Ca Ca 0.2262 0.3064 '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
C2 Al C3 111.86(9) . .
C2 Al C1 109.74(10) . .
C3 Al C1 111.50(9) . .
C2 Al C4 108.61(8) . .
C3 Al C4 106.10(8) . .
C1 Al C4 108.90(9) . .
C5 C4 C9 114.37(17) . .
C5 C4 Al 123.91(14) . .
C9 C4 Al 121.72(13) . .
C6 C5 C4 123.1(2) . .
C7 C6 C5 120.5(2) . .
C8 C7 C6 119.0(2) . .
C7 C8 C9 120.1(2) . .
C8 C9 C4 123.0(2) . .
O1 Ca O1 180.0 . 3_655
O1 Ca O3 91.22(4) . .
O1 Ca O3 88.78(4) 3_655 .
O1 Ca O3 88.78(4) . 3_655
O1 Ca O3 91.22(4) 3_655 3_655
O3 Ca O3 180.0 . 3_655
O1 Ca O2 90.92(4) . 3_655
O1 Ca O2 89.08(4) 3_655 3_655
O3 Ca O2 92.16(4) . 3_655
O3 Ca O2 87.84(4) 3_655 3_655
O1 Ca O2 89.08(4) . .
O1 Ca O2 90.92(4) 3_655 .
O3 Ca O2 87.84(4) . .
O3 Ca O2 92.16(4) 3_655 .
O2 Ca O2 180.0 3_655 .
C10 O1 C13 108.51(13) . .
C10 O1 Ca 126.03(10) . .
C13 O1 Ca 124.69(10) . .
C14 O2 C17 108.03(14) . .
C14 O2 Ca 124.62(11) . .
C17 O2 Ca 127.33(11) . .
C21 O3 C18 109.07(13) . .
C21 O3 Ca 124.74(11) . .
C18 O3 Ca 126.18(10) . .
O1 C10 C11 104.98(15) . .
C10 C11 C12 101.78(15) . .
C13 C12 C11 103.06(15) . .
O1 C13 C12 106.07(15) . .
O2 C14 C15 108.57(19) . .
C14 C15 C16 105.3(2) . .
C17 C16 C15 103.43(18) . .
O2 C17 C16 105.05(17) . .
O3 C18 C19 105.06(16) . .
C20 C19 C18 104.4(2) . .
C21 C20 C19 102.47(19) . .
O3 C21 C20 105.38(16) . .
C6T C1T C2T 117.96(18) . .
C6T C1T C7T 120.3(2) . .
C2T C1T C7T 121.7(2) . .
C1T C2T C3T 120.6(2) . .
C4T C3T C2T 120.1(2) . .
C5T C4T C3T 119.4(2) . .
C4T C5T C6T 120.6(2) . .
C5T C6T C1T 121.3(2) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Al C2 1.997(2) .
Al C3 1.9988(19) .
Al C1 2.006(2) .
Al C4 2.0213(17) .
C4 C5 1.387(3) .
C4 C9 1.399(3) .
C5 C6 1.388(3) .
C6 C7 1.367(4) .
C7 C8 1.364(4) .
C8 C9 1.394(3) .
Ca O1 2.3370(11) .
Ca O1 2.3370(11) 3_655
Ca O3 2.3380(11) .
Ca O3 2.3380(11) 3_655
Ca O2 2.3432(11) 3_655
Ca O2 2.3433(11) .
O1 C10 1.458(2) .
O1 C13 1.461(2) .
O2 C14 1.448(2) .
O2 C17 1.449(2) .
O3 C21 1.457(2) .
O3 C18 1.458(2) .
C10 C11 1.504(3) .
C11 C12 1.516(3) .
C12 C13 1.508(3) .
C14 C15 1.448(3) .
C15 C16 1.509(4) .
C16 C17 1.497(3) .
C18 C19 1.499(3) .
C19 C20 1.495(4) .
C20 C21 1.493(3) .
C1T C6T 1.377(3) .
C1T C2T 1.378(3) .
C1T C7T 1.507(3) .
C2T C3T 1.386(3) .
C3T C4T 1.371(4) .
C4T C5T 1.359(4) .
C5T C6T 1.367(3) .
