#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:13:12 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178640 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/51/4075143.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_4075143
loop_
_publ_author_name
'García, Felipe'
'Hopkins, Alexander D.'
'Kowenicki, Richard A.'
'McPartlin, Mary'
'Rogers, Michael C.'
'Silvia, Jared S.'
'Wright, Dominic S.'
_publ_section_title
;
 Syntheses and Structure of Heterometallic Complexes Containing Tripodal
 Group 13 Ligands [RE(2-py)3]-(E = Al, In)†
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2561
_journal_paper_doi               10.1021/om0600691
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C53 H54 Al2 Ca N6'
_chemical_formula_weight         869.06
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 94.80(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4930(19)
_cell_length_b                   22.857(5)
_cell_length_c                   22.727(5)
_cell_measurement_reflns_used    20959
_cell_measurement_temperature    393(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.00
_cell_volume                     4914.0(18)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;
 HKL Denzo and Scalepack (Otwinowski & Minor 1997)
;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice ω and φ 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  0.0412
_diffrn_reflns_av_sigmaI/netI    0.0463
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            20493
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         3.57
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.204
_exptl_absorpt_correction_T_max  0.980
_exptl_absorpt_correction_T_min  0.949
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
multi-scan from symmetry-related measurements 
 Sortav (Blessing 1995)
;
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1840
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.893
_refine_diff_density_min         -0.500
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         5569
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.0674
_refine_ls_R_factor_gt           0.0490
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0588P)²+7.0076P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1211
_refine_ls_wR_factor_ref         0.1312
_reflns_number_gt                4480
_reflns_number_total             5569
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0600691si20060130_121303.cif
_cod_data_source_block           dw0528
_cod_original_cell_volume        4913.9(17)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               4075143
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
_atom_site_disorder_assembly
_atom_site_disorder_group
Ca1 Ca 0.7500 0.2500 0.0000 0.02072(13) Uani 1 2 d S . .
Al1 Al 1.01182(5) 0.16139(2) 0.08460(2) 0.02186(14) Uani 1 1 d . . .
N16 N 0.72046(16) 0.19951(7) 0.09483(7) 0.0266(3) Uani 1 1 d . . .
N26 N 0.98821(15) 0.28181(7) 0.04017(7) 0.0248(3) Uani 1 1 d . . .
N36 N 0.86099(16) 0.15845(7) -0.03331(7) 0.0252(3) Uani 1 1 d . . .
C1 C 1.1547(2) 0.11418(9) 0.13177(10) 0.0356(5) Uani 1 1 d . . .
H1A H 1.1195 0.0752 0.1362 0.053 Uiso 1 1 calc R . .
H1B H 1.1739 0.1317 0.1700 0.053 Uiso 1 1 calc R . .
H1C H 1.2402 0.1128 0.1120 0.053 Uiso 1 1 calc R . .
C15 C 0.5949(2) 0.20293(10) 0.11817(9) 0.0343(5) Uani 1 1 d . . .
H15 H 0.5230 0.2244 0.0979 0.041 Uiso 1 1 calc R . .
C14 C 0.5671(2) 0.17640(10) 0.17043(9) 0.0381(5) Uani 1 1 d . . .
H14 H 0.4783 0.1792 0.1847 0.046 Uiso 1 1 calc R . .
C13 C 0.6748(2) 0.14551(10) 0.20112(9) 0.0371(5) Uani 1 1 d . . .
H13 H 0.6605 0.1274 0.2368 0.045 Uiso 1 1 calc R . .
C12 C 0.8044(2) 0.14220(9) 0.17761(9) 0.0315(4) Uani 1 1 d . . .
H12 H 0.8777 0.1218 0.1982 0.038 Uiso 1 1 calc R . .
C11 C 0.82877(19) 0.16862(8) 0.12372(8) 0.0242(4) Uani 1 1 d . . .
C25 C 1.0315(2) 0.33671(8) 0.03084(9) 0.0303(4) Uani 1 1 d . . .
H25 H 0.9685 0.3621 0.0103 0.036 Uiso 1 1 calc R . .
C24 C 1.1636(2) 0.35772(9) 0.04983(10) 0.0351(5) Uani 1 1 d . . .
H24 H 1.1888 0.3961 0.0423 0.042 Uiso 1 1 calc R . .
C23 C 1.2576(2) 0.32016(9) 0.08041(10) 0.0355(5) Uani 1 1 d . . .
H23 H 1.3480 0.3326 0.0937 0.043 Uiso 1 1 calc R . .
C22 C 1.2137(2) 0.26367(9) 0.09077(9) 0.0304(4) Uani 1 1 d . . .
H22 H 1.2757 0.2382 0.1118 0.037 Uiso 1 1 calc R . .
C21 C 1.07873(18) 0.24351(8) 0.07062(8) 0.0239(4) Uani 1 1 d . . .
C35 C 0.8256(2) 0.13808(9) -0.08814(9) 0.0309(4) Uani 1 1 d . . .
H35 H 0.7606 0.1593 -0.1125 0.037 Uiso 1 1 calc R . .
C34 C 0.8805(2) 0.08745(9) -0.11037(9) 0.0338(5) Uani 1 1 d . . .
H34 H 0.8526 0.0748 -0.1485 0.041 Uiso 1 1 calc R . .
C33 C 0.9780(2) 0.05615(9) -0.07433(9) 0.0337(5) Uani 1 1 d . . .
H33 H 1.0179 0.0220 -0.0878 0.040 Uiso 1 1 calc R . .
C32 C 1.0150(2) 0.07669(8) -0.01782(9) 0.0283(4) Uani 1 1 d . . .
H32 H 1.0800 0.0557 0.0068 0.034 Uiso 1 1 calc R . .
C31 C 0.95707(18) 0.12827(8) 0.00335(8) 0.0231(4) Uani 1 1 d . . .
C1T C 0.5000 0.3106(3) 0.2500 0.193(5) Uani 1 2 d S . .
H1TA H 0.4710 0.2966 0.2869 0.289 Uiso 0.50 1 calc PR . .
H1TB H 0.5935 0.2966 0.2447 0.289 Uiso 0.50 1 calc PR . .
H1TC H 0.4355 0.2966 0.2183 0.289 Uiso 0.50 1 calc PR . .
C2T C 0.5000 0.37473(17) 0.2500 0.0674(13) Uani 1 2 d S . .
C3T C 0.3834(3) 0.40704(17) 0.22563(11) 0.0638(9) Uani 1 1 d . . .
H3T H 0.3034 0.3879 0.2090 0.077 Uiso 1 1 calc R . .
C4T C 0.3882(4) 0.46677(17) 0.22654(13) 0.0699(9) Uani 1 1 d . . .
H4T H 0.3108 0.4879 0.2102 0.084 Uiso 1 1 calc R . .
C5T C 0.5000 0.4950(2) 0.2500 0.0745(13) Uani 1 2 d S . .
H5T H 0.5000 0.5356 0.2500 0.089 Uiso 1 2 calc SR . .
C1S C 1.0000 0.4832(6) 0.2500 0.182(5) Uani 1 2 d S . .
H1SA H 1.0900 0.4972 0.2396 0.273 Uiso 0.50 1 calc PR . .
H1SB H 0.9833 0.4972 0.2886 0.273 Uiso 0.50 1 calc PR . .
H1SC H 0.9268 0.4972 0.2218 0.273 Uiso 0.50 1 calc PR . .
C2S C 1.0000 0.4318(4) 0.2500 0.115(3) Uani 1 2 d S . .
C3S C 0.9873(4) 0.4007(3) 0.19645(18) 0.0977(16) Uani 1 1 d . . .
H3S H 0.9758 0.4207 0.1608 0.117 Uiso 1 1 calc R . .
C4S C 0.9916(4) 0.3441(3) 0.19686(17) 0.1038(17) Uani 1 1 d . . .
H4S H 0.9892 0.3244 0.1610 0.125 Uiso 1 1 calc R . .
C5S C 1.0000 0.3104(5) 0.2500 0.165(5) Uani 1 2 d S . .
H5S H 1.0000 0.2697 0.2500 0.198 Uiso 1 2 calc SR . .
C1R C 1.0405(5) 0.51405(18) 0.0286(2) 0.0412(11) Uani 0.50 1 d P A -1
C2R C 1.1046(3) 0.50691(11) -0.02410(14) 0.0522(7) Uani 1 1 d . A -1
H2R H 1.1981 0.5192 -0.0237 0.063 Uiso 1 1 calc R A -1
C3R C 1.0512(8) 0.4859(3) -0.0720(2) 0.0641(18) Uani 0.50 1 d P A -1
H3R H 1.1057 0.4842 -0.1041 0.077 Uiso 0.50 1 calc PR A -1
C4R C 0.9032(5) 0.46359(15) -0.07885(19) 0.0920(13) Uani 1 1 d . A -1
H4R H 0.8597 0.4472 -0.1132 0.110 Uiso 0.50 1 calc PR A -1
C5R C 0.8376(5) 0.4711(2) -0.0248(3) 0.0545(15) Uani 0.50 1 d P A -1
H5R H 0.7404 0.4588 -0.0249 0.065 Uiso 0.50 1 d P B -1
H6RA H 0.8076 0.4503 -0.0738 0.082 Uiso 0.50 1 d P C -2
H6RB H 0.8987 0.4928 -0.1093 0.082 Uiso 0.50 1 d P D -2
H6RC H 0.9577 0.4310 -0.0903 0.082 Uiso 0.50 1 d P E -2
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'
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
N26 Ca1 N26 180.00(10) . 7_655
N26 Ca1 N16 91.00(6) . 7_655
N26 Ca1 N16 89.00(6) 7_655 7_655
N26 Ca1 N16 89.00(6) . .
N26 Ca1 N16 91.00(6) 7_655 .
N16 Ca1 N16 180.00(7) 7_655 .
N26 Ca1 N36 92.17(5) . 7_655
N26 Ca1 N36 87.83(5) 7_655 7_655
N16 Ca1 N36 87.41(5) 7_655 7_655
N16 Ca1 N36 92.59(5) . 7_655
N26 Ca1 N36 87.83(5) . .
N26 Ca1 N36 92.17(5) 7_655 .
N16 Ca1 N36 92.59(5) 7_655 .
N16 Ca1 N36 87.41(5) . .
N36 Ca1 N36 180.00(8) 7_655 .
N26 Ca1 Al1 126.53(4) . 7_655
N26 Ca1 Al1 53.47(4) 7_655 7_655
N16 Ca1 Al1 53.31(4) 7_655 7_655
N16 Ca1 Al1 126.69(4) . 7_655
N36 Ca1 Al1 53.38(4) 7_655 7_655
N36 Ca1 Al1 126.62(4) . 7_655
N26 Ca1 Al1 53.47(4) . .
N26 Ca1 Al1 126.53(4) 7_655 .
N16 Ca1 Al1 126.69(4) 7_655 .
N16 Ca1 Al1 53.31(4) . .
N36 Ca1 Al1 126.62(4) 7_655 .
N36 Ca1 Al1 53.38(4) . .
Al1 Ca1 Al1 180.00(2) 7_655 .
C1 Al1 C21 112.50(9) . .
C1 Al1 C31 113.75(9) . .
C21 Al1 C31 105.36(8) . .
C1 Al1 C11 112.44(9) . .
C21 Al1 C11 106.66(8) . .
C31 Al1 C11 105.49(8) . .
C1 Al1 Ca1 179.00(7) . .
C21 Al1 Ca1 66.90(5) . .
C31 Al1 Ca1 67.24(6) . .
C11 Al1 Ca1 67.18(5) . .
C15 N16 C11 119.67(16) . .
C15 N16 Ca1 118.90(13) . .
C11 N16 Ca1 121.43(12) . .
C25 N26 C21 119.24(15) . .
C25 N26 Ca1 119.90(12) . .
C21 N26 Ca1 120.84(11) . .
C35 N36 C31 119.38(16) . .
C35 N36 Ca1 119.56(13) . .
C31 N36 Ca1 121.06(12) . .
N16 C15 C14 123.58(19) . .
C15 C14 C13 118.22(19) . .
C14 C13 C12 118.49(18) . .
C13 C12 C11 122.05(19) . .
N16 C11 C12 117.97(17) . .
N16 C11 Al1 118.01(13) . .
C12 C11 Al1 123.98(14) . .
N26 C25 C24 123.98(18) . .
C25 C24 C23 118.24(18) . .
C24 C23 C22 118.30(18) . .
C23 C22 C21 122.09(18) . .
N26 C21 C22 118.14(16) . .
N26 C21 Al1 118.76(13) . .
C22 C21 Al1 123.10(14) . .
N36 C35 C34 123.76(19) . .
C33 C34 C35 118.08(19) . .
C34 C33 C32 118.63(18) . .
C33 C32 C31 121.79(18) . .
N36 C31 C32 118.36(17) . .
N36 C31 Al1 118.29(13) . .
C32 C31 Al1 123.33(14) . .
C3T C2T C3T 116.6(4) 2_655 .
C3T C2T C1T 121.71(19) 2_655 .
C3T C2T C1T 121.71(19) . .
C4T C3T C2T 119.7(3) . .
C5T C4T C3T 121.3(3) . .
C4T C5T C4T 121.4(5) . 2_655
C1S C2S C3S 120.4(4) . .
C1S C2S C3S 120.4(4) . 2_755
C3S C2S C3S 119.3(8) . 2_755
C4S C3S C2S 119.9(5) . .
C3S C4S C5S 122.9(6) . .
C4S C5S C4S 114.9(9) 2_755 .
C3R C2R C1R 127.9(4) . .
C2R C3R C4R 121.9(5) . .
C5R C4R C3R 110.0(4) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ca1 N26 2.4758(16) .
Ca1 N26 2.4758(16) 7_655
Ca1 N16 2.4813(16) 7_655
Ca1 N16 2.4813(16) .
Ca1 N36 2.4891(16) 7_655
Ca1 N36 2.4891(16) .
Ca1 Al1 3.6298(10) 7_655
Ca1 Al1 3.6298(10) .
Al1 C1 1.978(2) .
Al1 C21 2.0152(19) .
Al1 C31 2.023(2) .
Al1 C11 2.024(2) .
N16 C15 1.347(2) .
N16 C11 1.369(2) .
N26 C25 1.343(2) .
N26 C21 1.373(2) .
N36 C35 1.346(2) .
N36 C31 1.369(2) .
C15 C14 1.378(3) .
C14 C13 1.382(3) .
C13 C12 1.384(3) .
C12 C11 1.402(3) .
C25 C24 1.378(3) .
C24 C23 1.383(3) .
C23 C22 1.383(3) .
C22 C21 1.402(3) .
C35 C34 1.382(3) .
C34 C33 1.383(3) .
C33 C32 1.385(3) .
C32 C31 1.403(3) .
C1T C2T 1.467(7) .
C2T C3T 1.405(4) 2_655
C2T C3T 1.405(4) .
C3T C4T 1.366(5) .
C4T C5T 1.316(4) .
C5T C4T 1.316(4) 2_655
C1S C2S 1.175(11) .
C2S C3S 1.406(5) .
C2S C3S 1.406(5) 2_755
C3S C4S 1.295(7) .
C4S C5S 1.428(8) .
C5S C4S 1.428(8) 2_755
C1R C2R 1.397(6) .
C2R C3R 1.257(7) .
C3R C4R 1.491(8) .
C4R C5R 1.434(8) .
