#------------------------------------------------------------------------------
#$Date: 2016-03-23 16:22:53 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179374 $
#$URL: svn://www.crystallography.net/cod/cif/4/32/71/4327138.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_4327138
loop_
_publ_author_name
'John A. T. Norman'
'Melanie Perez'
'M. S. Kim'
'Xinjian Lei'
'Sergei Ivanov'
'Agnes Derecskei-Kovacs'
'Laura Matz'
'Iain Buchanan'
'Arnold L. Rheingold'
_publ_section_title
;
 New Volatile Strontium and Barium Imidazolate Complexes for the
 Deposition of Group 2 Metal Oxides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              12396
_journal_page_last               12398
_journal_paper_doi               10.1021/ic201751q
_journal_volume                  50
_journal_year                    2011
_chemical_formula_sum            'C60 H108 Ba2 N8'
_chemical_formula_weight         1216.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                95.888(6)
_cell_angle_beta                 105.336(5)
_cell_angle_gamma                97.627(6)
_cell_formula_units_Z            1
_cell_length_a                   10.1060(7)
_cell_length_b                   11.0806(8)
_cell_length_c                   14.7829(10)
_cell_measurement_reflns_used    5955
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      66.13
_cell_measurement_theta_min      3.13
_cell_volume                     1565.8(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.857
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and 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  0.0524
_diffrn_reflns_av_sigmaI/netI    0.0685
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            9857
_diffrn_reflns_theta_full        55.00
_diffrn_reflns_theta_max         66.46
_diffrn_reflns_theta_min         3.13
_exptl_absorpt_coefficient_mu    10.017
_exptl_absorpt_correction_T_max  0.4341
_exptl_absorpt_correction_T_min  0.1530
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_description       block
_exptl_crystal_F_000             636
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.530
_refine_diff_density_min         -1.440
_refine_diff_density_rms         0.142
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     316
_refine_ls_number_reflns         4724
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.055
_refine_ls_R_factor_all          0.0644
_refine_ls_R_factor_gt           0.0528
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0900P)²+1.5000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1320
_refine_ls_wR_factor_ref         0.1406
_reflns_number_gt                4040
_reflns_number_total             4724
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic201751q_si_002_2.cif
_cod_data_source_block           ap131
_cod_original_cell_volume        1565.82(19)
_cod_database_code               4327138
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
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
Ba1 Ba 0.71201(4) 0.62824(4) 0.68120(2) 0.01720(16) Uani 1 1 d .
N1 N 0.8479(6) 0.7047(6) 0.8844(4) 0.0235(13) Uani 1 1 d .
N2 N 0.9430(6) 0.8202(6) 0.7935(4) 0.0228(13) Uani 1 1 d .
N3 N 0.4097(6) 0.2950(5) 0.4928(4) 0.0199(12) Uani 1 1 d .
N4 N 0.5800(5) 0.3776(5) 0.6260(4) 0.0175(12) Uani 1 1 d .
C1 C 0.9451(6) 0.7216(7) 0.8390(4) 0.0207(15) Uani 1 1 d .
C2 C 0.8389(7) 0.8762(6) 0.8140(5) 0.0198(15) Uani 1 1 d .
C3 C 0.7786(7) 0.8040(7) 0.8710(5) 0.0203(15) Uani 1 1 d .
C4 C 1.0559(7) 0.6395(7) 0.8425(5) 0.0241(15) Uani 1 1 d .
C5 C 0.9963(9) 0.5037(9) 0.8416(8) 0.052(2) Uani 1 1 d .
H5A H 0.9599 0.4965 0.8963 0.077 Uiso 1 1 calc R
H5B H 1.0701 0.4539 0.8447 0.077 Uiso 1 1 calc R
H5C H 0.9211 0.4746 0.7830 0.077 Uiso 1 1 calc R
C6 C 1.1120(10) 0.6473(11) 0.7552(7) 0.057(3) Uani 1 1 d .
H6A H 1.1512 0.7329 0.7546 0.085 Uiso 1 1 calc R
H6B H 1.0359 0.6180 0.6972 0.085 Uiso 1 1 calc R
H6C H 1.1846 0.5961 0.7585 0.085 Uiso 1 1 calc R
C7 C 1.1749(9) 0.6844(9) 0.9305(7) 0.048(2) Uani 1 1 d .
H7A H 1.2119 0.7708 0.9305 0.072 Uiso 1 1 calc R
H7B H 1.2484 0.6346 0.9316 0.072 Uiso 1 1 calc R
H7C H 1.1419 0.6770 0.9866 0.072 Uiso 1 1 calc R
C8 C 0.8185(7) 1.0005(7) 0.7804(5) 0.0234(16) Uani 1 1 d .
C9 C 0.6785(8) 0.9884(8) 0.7018(5) 0.0308(18) Uani 1 1 d .
H9A H 0.6757 0.9250 0.6496 0.046 Uiso 1 1 calc R
H9B H 0.6707 1.0673 0.6781 0.046 Uiso 1 1 calc R
H9C H 0.6010 0.9651 0.7282 0.046 Uiso 1 1 calc R
C10 C 0.8249(8) 1.1014(7) 0.8624(5) 0.0292(17) Uani 1 1 d .
H10A H 0.9134 1.1087 0.9117 0.044 Uiso 1 1 calc R
H10B H 0.7476 1.0794 0.8893 0.044 Uiso 1 1 calc R
H10C H 0.8178 1.1802 0.8384 0.044 Uiso 1 1 calc R
C11 C 0.9335(8) 1.0452(7) 0.7365(5) 0.0289(17) Uani 1 1 d .
H11A H 1.0242 1.0545 0.7838 0.043 Uiso 1 1 calc R
H11B H 0.9198 1.1248 0.7153 0.043 Uiso 1 1 calc R
H11C H 0.9305 0.9852 0.6822 0.043 Uiso 1 1 calc R
C12 C 0.6765(7) 0.8218(7) 0.9303(5) 0.0247(16) Uani 1 1 d .
C13 C 0.6228(10) 0.6965(8) 0.9548(7) 0.045(2) Uani 1 1 d .
H13A H 0.7019 0.6584 0.9854 0.068 Uiso 1 1 calc R
H13B H 0.5668 0.6431 0.8966 0.068 Uiso 1 1 calc R
H13C H 0.5653 0.7082 0.9980 0.068 Uiso 1 1 calc R
C14 C 0.5484(7) 0.8766(9) 0.8818(5) 0.037(2) Uani 1 1 d .
H14A H 0.5789 0.9568 0.8650 0.055 Uiso 1 1 calc R
H14B H 0.4910 0.8867 0.9252 0.055 Uiso 1 1 calc R
H14C H 0.4938 0.8211 0.8243 0.055 Uiso 1 1 calc R
C15 C 0.7557(8) 0.9026(8) 1.0243(5) 0.0328(18) Uani 1 1 d .
H15A H 0.7918 0.9839 1.0120 0.049 Uiso 1 1 calc R
H15B H 0.8333 0.8643 1.0572 0.049 Uiso 1 1 calc R
H15C H 0.6928 0.9113 1.0640 0.049 Uiso 1 1 calc R
C16 C 0.5444(7) 0.3443(6) 0.5311(5) 0.0191(14) Uani 1 1 d .
C17 C 0.4602(7) 0.3402(7) 0.6523(5) 0.0209(15) Uani 1 1 d .
C18 C 0.3551(7) 0.2916(6) 0.5704(5) 0.0201(15) Uani 1 1 d .
C19 C 0.6551(7) 0.3293(7) 0.4799(4) 0.0191(15) Uani 1 1 d .
C20 C 0.6014(7) 0.3334(7) 0.3741(5) 0.0258(16) Uani 1 1 d .
H20A H 0.5752 0.4141 0.3639 0.039 Uiso 1 1 calc R
H20B H 0.5199 0.2691 0.3463 0.039 Uiso 1 1 calc R
H20C H 0.6745 0.3197 0.3438 0.039 Uiso 1 1 calc R
C21 C 0.6940(7) 0.2021(7) 0.4939(5) 0.0277(17) Uani 1 1 d .
H21A H 0.7286 0.1979 0.5619 0.042 Uiso 1 1 calc R
H21B H 0.7667 0.1883 0.4632 0.042 Uiso 1 1 calc R
H21C H 0.6117 0.1387 0.4657 0.042 Uiso 1 1 calc R
C22 C 0.7832(7) 0.4272(7) 0.5202(5) 0.0271(16) Uani 1 1 d .
H22A H 0.7581 0.5084 0.5110 0.041 Uiso 1 1 calc R
H22B H 0.8534 0.4121 0.4875 0.041 Uiso 1 1 calc R
H22C H 0.8211 0.4243 0.5880 0.041 Uiso 1 1 calc R
C23 C 0.4730(7) 0.3447(7) 0.7588(5) 0.0227(15) Uani 1 1 d .
C24 C 0.4368(8) 0.2138(7) 0.7814(5) 0.0283(16) Uani 1 1 d .
H24A H 0.4935 0.1600 0.7576 0.043 Uiso 1 1 calc R
H24B H 0.3380 0.1821 0.7507 0.043 Uiso 1 1 calc R
H24C H 0.4559 0.2160 0.8501 0.043 Uiso 1 1 calc R
C25 C 0.3848(7) 0.4290(7) 0.7957(5) 0.0277(16) Uani 1 1 d .
H25A H 0.4081 0.5122 0.7813 0.041 Uiso 1 1 calc R
H25B H 0.4039 0.4314 0.8645 0.041 Uiso 1 1 calc R
H25C H 0.2860 0.3975 0.7651 0.041 Uiso 1 1 calc R
C26 C 0.6251(7) 0.3902(7) 0.8162(5) 0.0264(16) Uani 1 1 d .
H26A H 0.6546 0.4737 0.8045 0.040 Uiso 1 1 calc R
H26B H 0.6841 0.3352 0.7968 0.040 Uiso 1 1 calc R
H26C H 0.6339 0.3909 0.8839 0.040 Uiso 1 1 calc R
C27 C 0.2051(7) 0.2209(7) 0.5500(5) 0.0219(15) Uani 1 1 d .
C28 C 0.2153(8) 0.0826(7) 0.5531(5) 0.0300(17) Uani 1 1 d .
H28A H 0.1218 0.0350 0.5405 0.045 Uiso 1 1 calc R
H28B H 0.2721 0.0724 0.6159 0.045 Uiso 1 1 calc R
H28C H 0.2585 0.0533 0.5048 0.045 Uiso 1 1 calc R
C29 C 0.1173(7) 0.2297(6) 0.4498(5) 0.0214(15) Uani 1 1 d .
H29A H 0.1078 0.3158 0.4444 0.032 Uiso 1 1 calc R
H29B H 0.0249 0.1801 0.4376 0.032 Uiso 1 1 calc R
H29C H 0.1629 0.1989 0.4035 0.032 Uiso 1 1 calc R
C30 C 0.1226(7) 0.2627(8) 0.6167(5) 0.0297(17) Uani 1 1 d .
H30A H 0.1166 0.3500 0.6150 0.044 Uiso 1 1 calc R
H30B H 0.1695 0.2507 0.6814 0.044 Uiso 1 1 calc R
H30C H 0.0287 0.2142 0.5966 0.044 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 0.0181 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'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ba Ba -1.0456 8.4617 '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
N3 Ba1 C1 135.59(18) 2_666 .
N3 Ba1 N4 95.43(16) 2_666 .
C1 Ba1 N4 126.34(17) . .
N3 Ba1 N1 145.97(17) 2_666 .
C1 Ba1 N1 26.64(17) . .
N4 Ba1 N1 116.22(16) . .
N3 Ba1 N2 109.09(16) 2_666 .
C1 Ba1 N2 26.80(18) . .
N4 Ba1 N2 151.97(15) . .
N1 Ba1 N2 45.11(15) . .
N3 Ba1 C3 121.08(17) 2_666 .
C1 Ba1 C3 42.17(18) . .
N4 Ba1 C3 131.81(16) . .
N1 Ba1 C3 26.28(17) . .
N2 Ba1 C3 43.65(16) . .
N3 Ba1 C2 102.69(17) 2_666 .
C1 Ba1 C2 42.16(18) . .
N4 Ba1 C2 158.03(15) . .
N1 Ba1 C2 43.77(17) . .
N2 Ba1 C2 26.05(15) . .
C3 Ba1 C2 26.32(16) . .
N3 Ba1 C20 59.13(15) 2_666 2_666
C1 Ba1 C20 133.81(19) . 2_666
N4 Ba1 C20 80.73(18) . 2_666
N1 Ba1 C20 111.64(17) . 2_666
N2 Ba1 C20 123.26(18) . 2_666
C3 Ba1 C20 91.64(18) . 2_666
C2 Ba1 C20 97.90(19) . 2_666
N3 Ba1 C29 54.47(16) 2_666 2_666
C1 Ba1 C29 87.45(18) . 2_666
N4 Ba1 C29 121.45(17) . 2_666
N1 Ba1 C29 111.70(17) . 2_666
N2 Ba1 C29 67.05(16) . 2_666
C3 Ba1 C29 105.84(18) . 2_666
C2 Ba1 C29 79.73(17) . 2_666
C20 Ba1 C29 110.74(16) 2_666 2_666
N3 Ba1 C22 76.38(17) 2_666 .
C1 Ba1 C22 113.04(18) . .
N4 Ba1 C22 55.21(16) . .
N1 Ba1 C22 131.31(17) . .
N2 Ba1 C22 116.79(16) . .
C3 Ba1 C22 155.14(17) . .
C2 Ba1 C22 141.37(16) . .
C20 Ba1 C22 113.13(19) 2_666 .
C29 Ba1 C22 68.38(18) 2_666 .
C1 N1 C3 104.8(6) . .
C1 N1 Ba1 72.3(4) . .
C3 N1 Ba1 83.8(4) . .
C1 N2 C2 104.9(5) . .
C1 N2 Ba1 72.1(4) . .
C2 N2 Ba1 84.0(4) . .
C16 N3 C18 104.4(5) . .
C16 N3 Ba1 113.8(4) . 2_666
C18 N3 Ba1 126.8(4) . 2_666
C16 N4 C17 105.2(6) . .
C16 N4 Ba1 112.1(4) . .
C17 N4 Ba1 118.2(4) . .
N1 C1 N2 114.9(6) . .
N1 C1 C4 123.0(6) . .
N2 C1 C4 122.1(6) . .
N1 C1 Ba1 81.0(4) . .
N2 C1 Ba1 81.1(4) . .
C4 C1 Ba1 109.4(4) . .
N2 C2 C3 107.7(5) . .
N2 C2 C8 118.3(5) . .
C3 C2 C8 133.7(6) . .
N2 C2 Ba1 70.0(4) . .
C3 C2 Ba1 76.7(4) . .
C8 C2 Ba1 122.0(4) . .
N1 C3 C2 107.6(5) . .
N1 C3 C12 116.5(6) . .
C2 C3 C12 135.1(6) . .
N1 C3 Ba1 69.9(4) . .
C2 C3 Ba1 77.0(4) . .
C12 C3 Ba1 125.5(5) . .
C7 C4 C1 109.0(6) . .
C7 C4 C5 110.1(7) . .
C1 C4 C5 111.5(6) . .
C7 C4 C6 108.4(7) . .
C1 C4 C6 109.8(6) . .
C5 C4 C6 108.0(8) . .
C11 C8 C2 110.0(5) . .
C11 C8 C10 106.9(6) . .
C2 C8 C10 112.5(5) . .
C11 C8 C9 106.6(5) . .
C2 C8 C9 110.8(6) . .
C10 C8 C9 109.9(6) . .
C15 C12 C13 106.7(6) . .
C15 C12 C14 109.7(6) . .
C13 C12 C14 107.2(7) . .
C15 C12 C3 108.7(6) . .
C13 C12 C3 109.0(6) . .
C14 C12 C3 115.2(5) . .
N3 C16 N4 113.9(5) . .
N3 C16 C19 122.8(6) . .
N4 C16 C19 120.9(6) . .
C18 C17 N4 107.6(5) . .
C18 C17 C23 133.8(6) . .
N4 C17 C23 118.0(6) . .
C17 C18 N3 108.8(6) . .
C17 C18 C27 134.2(5) . .
N3 C18 C27 116.3(6) . .
C22 C19 C20 108.2(6) . .
C22 C19 C16 112.0(6) . .
C20 C19 C16 112.4(5) . .
C22 C19 C21 109.6(5) . .
C20 C19 C21 108.5(6) . .
C16 C19 C21 106.1(5) . .
C19 C20 Ba1 110.9(4) . 2_666
C19 C22 Ba1 107.3(4) . .
C25 C23 C26 107.3(6) . .
C25 C23 C24 109.7(6) . .
C26 C23 C24 105.6(5) . .
C25 C23 C17 114.5(5) . .
C26 C23 C17 109.4(5) . .
C24 C23 C17 109.9(6) . .
C30 C27 C29 106.0(5) . .
C30 C27 C18 115.9(6) . .
C29 C27 C18 111.3(5) . .
C30 C27 C28 109.5(5) . .
C29 C27 C28 106.4(6) . .
C18 C27 C28 107.3(5) . .
C27 C29 Ba1 115.0(4) . 2_666
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 N3 2.812(5) 2_666
Ba1 C1 2.831(7) .
Ba1 N4 2.852(6) .
Ba1 N1 2.935(6) .
Ba1 N2 2.939(6) .
Ba1 C3 3.107(7) .
Ba1 C2 3.110(7) .
Ba1 C20 3.152(7) 2_666
Ba1 C29 3.299(6) 2_666
Ba1 C22 3.375(7) .
N1 C1 1.332(8) .
N1 C3 1.384(9) .
N2 C1 1.341(9) .
N2 C2 1.374(8) .
N3 C16 1.343(9) .
N3 C18 1.400(8) .
N3 Ba1 2.812(5) 2_666
N4 C16 1.350(9) .
N4 C17 1.393(8) .
C1 C4 1.527(9) .
C2 C3 1.416(9) .
C2 C8 1.532(9) .
C3 C12 1.539(8) .
C4 C7 1.505(11) .
C4 C5 1.541(13) .
C4 C6 1.547(10) .
C8 C11 1.527(9) .
C8 C10 1.544(10) .
C8 C9 1.555(10) .
C12 C15 1.529(11) .
C12 C13 1.535(11) .
C12 C14 1.538(10) .
C16 C19 1.524(8) .
C17 C18 1.384(10) .
C17 C23 1.541(9) .
C18 C27 1.548(10) .
C19 C22 1.515(10) .
C19 C20 1.522(8) .
C19 C21 1.533(10) .
C20 Ba1 3.152(7) 2_666
C23 C25 1.529(9) .
C23 C26 1.534(10) .
C23 C24 1.539(10) .
C27 C30 1.525(9) .
C27 C29 1.532(9) .
C27 C28 1.553(11) .
C29 Ba1 3.298(6) 2_666
