#------------------------------------------------------------------------------
#$Date: 2016-03-21 08:08:33 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178596 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/07/4070790.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_4070790
loop_
_publ_author_name
'Datta, Simmi'
'Gamer, Michael T.'
'Roesky, Peter W.'
_publ_section_title
;
 Aminotroponiminate Complexes of the Heavy Alkaline Earth and the Divalent
 Lanthanide Metals as Catalysts for the Hydroamination/Cyclization
 Reaction
;
_journal_issue                   6
_journal_name_full               Organometallics
_journal_page_first              1207
_journal_paper_doi               10.1021/om701014d
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C34 H54 Ba N4 O2'
_chemical_formula_sum            'C34 H54 Ba N4 O2'
_chemical_formula_weight         688.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           60
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      60
_symmetry_space_group_name_Hall  '-P 2n 2ab'
_symmetry_space_group_name_H-M   'P b c n'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             06-11-09
_audit_creation_method           'STOE X-RED'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.5788(10)
_cell_length_b                   11.1267(7)
_cell_length_c                   19.8676(11)
_cell_measurement_reflns_used    14734
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      3.04
_cell_volume                     3443.9(4)
_computing_cell_refinement       'STOE X-AREA, PLATON (A.L.Spek, 2005)'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED, PLATON (A.L.Spek, 2005)'
_computing_molecular_graphics    'Diamond 2.1e'
_computing_publication_material  'X-STEP32, Microsoft Word'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'area detector'
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.0232
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            13055
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.04
_exptl_absorpt_coefficient_mu    1.187
_exptl_absorpt_correction_T_max  0.9234
_exptl_absorpt_correction_T_min  0.7663
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED & X-SHAPE'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.327
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1432
_exptl_crystal_size_max          0.523
_exptl_crystal_size_mid          0.416
_exptl_crystal_size_min          0.274
_refine_diff_density_max         0.566
_refine_diff_density_min         -0.470
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3027
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0368
_refine_ls_R_factor_gt           0.0252
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0445P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0643
_refine_ls_wR_factor_ref         0.0678
_reflns_number_gt                2327
_reflns_number_total             3027
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om701014d-file001.cif
_cod_data_source_block           4
_cod_database_code               4070790
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y+1/2, z+1/2'
'x+1/2, -y+1/2, -z'
'-x, y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z-1/2'
'-x-1/2, y-1/2, z'
'x, -y, 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
C1 C 0.36025(15) 0.7007(2) 0.88564(12) 0.0283(5) Uani 1 1 d .
C2 C 0.29862(17) 0.6982(2) 0.93929(13) 0.0403(6) Uani 1 1 d .
H2 H 0.2673 0.6250 0.9414 0.048 Uiso 1 1 calc R
C3 C 0.27535(18) 0.7788(3) 0.98812(13) 0.0451(7) Uani 1 1 d .
H3 H 0.2311 0.7520 1.0174 0.054 Uiso 1 1 calc R
C4 C 0.30597(18) 0.8931(2) 1.00157(14) 0.0446(7) Uani 1 1 d .
H4 H 0.2764 0.9399 1.0342 0.054 Uiso 1 1 calc R
C5 C 0.37650(18) 0.9434(2) 0.97068(14) 0.0394(6) Uani 1 1 d .
H5 H 0.3880 1.0243 0.9831 0.047 Uiso 1 1 calc R
C6 C 0.43321(17) 0.8952(2) 0.92462(13) 0.0335(6) Uani 1 1 d .
H6 H 0.4803 0.9466 0.9149 0.040 Uiso 1 1 calc R
C7 C 0.43606(15) 0.78369(19) 0.88833(11) 0.0270(5) Uani 1 1 d .
C8 C 0.28683(16) 0.5395(2) 0.83009(13) 0.0331(5) Uani 1 1 d .
H8 H 0.2775 0.5020 0.8752 0.040 Uiso 1 1 calc R
C9 C 0.20448(17) 0.6025(2) 0.80863(16) 0.0415(6) Uani 1 1 d .
H9A H 0.1926 0.6692 0.8395 0.062 Uiso 1 1 calc R
H9B H 0.1567 0.5452 0.8099 0.062 Uiso 1 1 calc R
H9C H 0.2112 0.6336 0.7628 0.062 Uiso 1 1 calc R
C10 C 0.30999(19) 0.4411(2) 0.78001(16) 0.0424(6) Uani 1 1 d .
H10A H 0.3189 0.4766 0.7354 0.064 Uiso 1 1 calc R
H10B H 0.2632 0.3823 0.7778 0.064 Uiso 1 1 calc R
H10C H 0.3628 0.4009 0.7946 0.064 Uiso 1 1 calc R
C11 C 0.58448(16) 0.8139(2) 0.86096(13) 0.0341(6) Uani 1 1 d .
H11 H 0.5889 0.8445 0.9082 0.041 Uiso 1 1 calc R
C12 C 0.5903(2) 0.9208(3) 0.81243(17) 0.0550(8) Uani 1 1 d .
H12A H 0.5935 0.8911 0.7660 0.082 Uiso 1 1 calc R
H12B H 0.6418 0.9679 0.8226 0.082 Uiso 1 1 calc R
H12C H 0.5393 0.9715 0.8176 0.082 Uiso 1 1 calc R
C13 C 0.65850(16) 0.7284(3) 0.84786(15) 0.0491(7) Uani 1 1 d .
H13A H 0.6515 0.6562 0.8756 0.074 Uiso 1 1 calc R
H13B H 0.7127 0.7680 0.8594 0.074 Uiso 1 1 calc R
H13C H 0.6590 0.7058 0.8002 0.074 Uiso 1 1 calc R
C14 C 0.5185(3) 0.4383(3) 0.91640(19) 0.0655(10) Uani 1 1 d .
H14A H 0.4830 0.5119 0.9191 0.079 Uiso 1 1 calc R
H14B H 0.5713 0.4506 0.9432 0.079 Uiso 1 1 calc R
C15 C 0.4704(3) 0.3335(4) 0.9413(2) 0.0758(11) Uani 1 1 d .
H15A H 0.4079 0.3444 0.9344 0.091 Uiso 1 1 calc R
H15B H 0.4814 0.3201 0.9898 0.091 Uiso 1 1 calc R
C16 C 0.5038(2) 0.2296(3) 0.8997(2) 0.0709(11) Uani 1 1 d .
H16A H 0.5383 0.1741 0.9278 0.085 Uiso 1 1 calc R
H16B H 0.4559 0.1841 0.8791 0.085 Uiso 1 1 calc R
C17 C 0.5580(3) 0.2866(3) 0.8469(2) 0.0773(11) Uani 1 1 d .
H17A H 0.6196 0.2728 0.8565 0.093 Uiso 1 1 calc R
H17B H 0.5446 0.2521 0.8022 0.093 Uiso 1 1 calc R
N1 N 0.35931(12) 0.62478(16) 0.83501(10) 0.0284(4) Uani 1 1 d .
N2 N 0.50395(12) 0.74790(19) 0.85387(9) 0.0303(4) Uani 1 1 d .
O O 0.53935(18) 0.41129(16) 0.84782(12) 0.0584(6) Uani 1 1 d .
Ba Ba 0.5000 0.585403(16) 0.7500 0.02823(9) Uani 1 2 d S
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'
Ba Ba -0.3244 2.2819 '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
N1 C1 C2 123.3(2) . .
N1 C1 C7 115.6(2) . .
C2 C1 C7 120.8(2) . .
C3 C2 C1 133.7(2) . .
C2 C3 C4 130.3(3) . .
C5 C4 C3 124.2(3) . .
C4 C5 C6 130.4(2) . .
C5 C6 C7 133.5(2) . .
N2 C7 C6 123.1(2) . .
N2 C7 C1 115.2(2) . .
C6 C7 C1 121.7(2) . .
N1 C8 C9 111.52(19) . .
N1 C8 C10 108.9(2) . .
C9 C8 C10 110.3(2) . .
N2 C11 C13 108.7(2) . .
N2 C11 C12 112.3(2) . .
C13 C11 C12 109.5(2) . .
O C14 C15 105.6(3) . .
C14 C15 C16 104.3(3) . .
C17 C16 C15 104.7(3) . .
O C17 C16 107.0(3) . .
C1 N1 C8 118.1(2) . .
C1 N1 Ba 123.62(15) . .
C8 N1 Ba 117.23(14) . .
C7 N2 C11 119.1(2) . .
C7 N2 Ba 124.77(15) . .
C11 N2 Ba 115.03(14) . .
C17 O C14 105.3(3) . .
C17 O Ba 135.2(2) . .
C14 O Ba 117.59(17) . .
N2 Ba N2 97.58(9) . 4_656
N2 Ba N1 57.40(5) . .
N2 Ba N1 109.43(6) 4_656 .
N2 Ba N1 109.43(6) . 4_656
N2 Ba N1 57.40(5) 4_656 4_656
N1 Ba N1 162.00(8) . 4_656
N2 Ba O 168.12(6) . 4_656
N2 Ba O 85.95(7) 4_656 4_656
N1 Ba O 110.73(7) . 4_656
N1 Ba O 82.05(6) 4_656 4_656
N2 Ba O 85.95(7) . .
N2 Ba O 168.12(6) 4_656 .
N1 Ba O 82.05(6) . .
N1 Ba O 110.73(6) 4_656 .
O Ba O 92.90(10) 4_656 .
N2 Ba C10 114.90(7) . 4_656
N2 Ba C10 101.40(6) 4_656 4_656
N1 Ba C10 148.84(6) . 4_656
N1 Ba C10 44.86(6) 4_656 4_656
O Ba C10 75.21(8) 4_656 4_656
O Ba C10 66.94(7) . 4_656
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
C1 N1 1.313(3) .
C1 C2 1.435(3) .
C1 C7 1.501(3) .
C2 C3 1.370(4) .
C3 C4 1.384(4) .
C4 C5 1.377(4) .
C5 C6 1.380(4) .
C6 C7 1.435(3) .
C7 N2 1.321(3) .
C8 N1 1.478(3) .
C8 C9 1.523(4) .
C8 C10 1.523(4) .
C11 N2 1.460(3) .
C11 C13 1.517(4) .
C11 C12 1.534(4) .
C14 O 1.433(4) .
C14 C15 1.473(5) .
C15 C16 1.514(6) .
C16 C17 1.488(5) .
C17 O 1.418(3) .
N1 Ba 2.8014(19) .
N2 Ba 2.744(2) .
O Ba 2.812(2) .
Ba N2 2.744(2) 4_656
Ba N1 2.801(2) 4_656
Ba O 2.812(2) 4_656
Ba C10 3.420(3) 4_656
