#------------------------------------------------------------------------------
#$Date: 2016-03-22 23:20:45 +0200 (Tue, 22 Mar 2016) $
#$Revision: 179056 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/18/4301820.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_4301820
loop_
_publ_author_name
'Chengfu Pi'
'Li Wan'
'Weiping Liu'
'Zaifu Pan'
'Haoyu Wu'
'Yunhua Wang'
'Wenjun Zheng'
'Linhong Weng'
'Zhenxia Chen'
'Limin Wu'
_publ_section_title
;
1,2,4-Diazaphospholide Complexes of Barium: Mechanism of Formation and
Crystallographic Characterization
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2967
_journal_page_last               2975
_journal_paper_doi               10.1021/ic802157g
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C44 H52 Ba N4 O4 P2'
_chemical_formula_weight         900.18
_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                 126.997(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.256(10)
_cell_length_b                   19.749(10)
_cell_length_c                   14.175(7)
_cell_measurement_reflns_used    819
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23.713
_cell_measurement_theta_min      2.895
_cell_volume                     4529(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SHELXTL'
_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      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0447
_diffrn_reflns_av_sigmaI/netI    0.0570
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            10071
_diffrn_reflns_theta_full        26.01
_diffrn_reflns_theta_max         26.01
_diffrn_reflns_theta_min         1.63
_exptl_absorpt_coefficient_mu    0.991
_exptl_absorpt_correction_T_max  0.9074
_exptl_absorpt_correction_T_min  0.8904
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.320
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.785
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.035
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     250
_refine_ls_number_reflns         4447
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0784
_refine_ls_R_factor_gt           0.0499
_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)+(0.0876P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1544
_refine_ls_wR_factor_ref         0.1647
_reflns_number_gt                2772
_reflns_number_total             4447
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802157g_si_001.cif
_cod_data_source_block           f80714b
_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 
;
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4301820
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
Ba1 Ba 0.0000 0.36528(2) 0.2500 0.0737(2) Uani 1 2 d S . .
P1 P 0.0000 0.62996(9) 0.2500 0.0768(6) Uani 1 2 d S . .
P2 P 0.0000 0.10051(9) 0.2500 0.0721(5) Uani 1 2 d S . .
N1 N 0.0417(3) 0.5033(2) 0.2795(4) 0.0703(12) Uani 1 1 d . . .
N2 N -0.0087(3) 0.2279(2) 0.1953(4) 0.0759(12) Uani 1 1 d . . .
O1 O 0.1357(3) 0.3646(2) 0.4826(4) 0.1090(15) Uani 1 1 d . . .
O2 O -0.0946(4) 0.3648(2) 0.3283(6) 0.1222(19) Uani 1 1 d . . .
C1 C 0.0732(3) 0.5656(2) 0.3005(4) 0.0613(12) Uani 1 1 d . . .
C2 C 0.1631(3) 0.5751(3) 0.3644(5) 0.0762(15) Uani 1 1 d . . .
C3 C 0.2161(4) 0.5182(4) 0.4081(6) 0.0965(19) Uani 1 1 d . . .
H3A H 0.1941 0.4749 0.3954 0.116 Uiso 1 1 calc R . .
C4 C 0.2998(5) 0.5264(6) 0.4693(8) 0.129(3) Uani 1 1 d . . .
H4A H 0.3341 0.4886 0.4972 0.155 Uiso 1 1 calc R . .
C5 C 0.3333(6) 0.5900(9) 0.4897(9) 0.156(5) Uani 1 1 d . . .
H5A H 0.3899 0.5949 0.5299 0.187 Uiso 1 1 calc R . .
C6 C 0.2845(6) 0.6452(6) 0.4518(8) 0.145(4) Uani 1 1 d . . .
H6A H 0.3077 0.6881 0.4675 0.174 Uiso 1 1 calc R . .
C7 C 0.1982(4) 0.6381(4) 0.3883(6) 0.101(2) Uani 1 1 d . . .
H7A H 0.1649 0.6764 0.3625 0.121 Uiso 1 1 calc R . .
C8 C -0.0150(3) 0.1654(3) 0.1532(5) 0.0656(13) Uani 1 1 d . . .
C9 C -0.0337(3) 0.1565(3) 0.0359(5) 0.0721(14) Uani 1 1 d . . .
C10 C -0.0377(5) 0.2127(4) -0.0279(7) 0.105(2) Uani 1 1 d . . .
H10A H -0.0293 0.2561 0.0028 0.126 Uiso 1 1 calc R . .
C11 C -0.0539(6) 0.2031(5) -0.1366(8) 0.127(3) Uani 1 1 d . . .
H11A H -0.0562 0.2406 -0.1781 0.152 Uiso 1 1 calc R . .
C12 C -0.0668(5) 0.1403(5) -0.1854(8) 0.119(3) Uani 1 1 d . . .
H12A H -0.0780 0.1350 -0.2589 0.142 Uiso 1 1 calc R . .
C13 C -0.0628(4) 0.0848(5) -0.1230(7) 0.105(2) Uani 1 1 d . . .
H13A H -0.0717 0.0415 -0.1543 0.126 Uiso 1 1 calc R . .
C14 C -0.0457(4) 0.0940(3) -0.0145(6) 0.0860(17) Uani 1 1 d . . .
H14A H -0.0420 0.0560 0.0271 0.103 Uiso 1 1 calc R . .
C15 C 0.2029(6) 0.3186(5) 0.5380(10) 0.168(4) Uani 1 1 d . . .
H15A H 0.1872 0.2757 0.5525 0.202 Uiso 1 1 calc R . .
H15B H 0.2200 0.3105 0.4880 0.202 Uiso 1 1 calc R . .
C16 C 0.2682(7) 0.3486(6) 0.6459(13) 0.183(4) Uani 1 1 d U . .
H16A H 0.3175 0.3504 0.6496 0.219 Uiso 1 1 calc R . .
H16B H 0.2802 0.3212 0.7114 0.219 Uiso 1 1 calc R . .
C17 C 0.2454(7) 0.4166(6) 0.6557(8) 0.176(5) Uani 1 1 d . . .
H17A H 0.2711 0.4505 0.6379 0.211 Uiso 1 1 calc R . .
H17B H 0.2608 0.4248 0.7341 0.211 Uiso 1 1 calc R . .
C18 C 0.1551(6) 0.4165(5) 0.5665(8) 0.131(3) Uani 1 1 d . . .
H18A H 0.1283 0.4072 0.6032 0.157 Uiso 1 1 calc R . .
H18B H 0.1364 0.4602 0.5276 0.157 Uiso 1 1 calc R . .
C19 C -0.1101(5) 0.4182(4) 0.3783(7) 0.113(2) Uani 1 1 d . . .
H19A H -0.1080 0.4616 0.3479 0.136 Uiso 1 1 calc R . .
H19B H -0.0699 0.4183 0.4636 0.136 Uiso 1 1 calc R . .
C20 C -0.1953(7) 0.4045(5) 0.3423(10) 0.142(3) Uani 1 1 d . . .
H20A H -0.1991 0.4163 0.4052 0.171 Uiso 1 1 calc R . .
H20B H -0.2364 0.4301 0.2721 0.171 Uiso 1 1 calc R . .
C21 C -0.2065(9) 0.3321(5) 0.3187(16) 0.217(7) Uani 1 1 d . . .
H21A H -0.1985 0.3081 0.3845 0.260 Uiso 1 1 calc R . .
H21B H -0.2618 0.3228 0.2482 0.260 Uiso 1 1 calc R . .
C22 C -0.1502(7) 0.3125(5) 0.3037(14) 0.211(7) Uani 1 1 d . . .
H22B H -0.1783 0.2976 0.2228 0.253 Uiso 1 1 calc R . .
H22A H -0.1195 0.2744 0.3551 0.253 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'
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'
P P 0.1023 0.0942 '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
_geom_angle_publ_flag
O2 Ba1 O2 179.59(19) . 2 ?
O2 Ba1 O1 92.7(2) . 2 ?
O2 Ba1 O1 87.26(19) 2 2 ?
O2 Ba1 O1 87.3(2) . . ?
O2 Ba1 O1 92.7(2) 2 . ?
O1 Ba1 O1 179.46(18) 2 . ?
O2 Ba1 N2 99.56(13) . . ?
O2 Ba1 N2 80.04(14) 2 . ?
O1 Ba1 N2 79.15(13) 2 . ?
O1 Ba1 N2 100.31(13) . . ?
O2 Ba1 N2 80.04(14) . 2 ?
O2 Ba1 N2 99.56(13) 2 2 ?
O1 Ba1 N2 100.31(13) 2 2 ?
O1 Ba1 N2 79.15(13) . 2 ?
N2 Ba1 N2 28.27(19) . 2 ?
O2 Ba1 N1 99.49(13) . . ?
O2 Ba1 N1 80.91(14) 2 . ?
O1 Ba1 N1 100.23(13) 2 . ?
O1 Ba1 N1 80.31(13) . . ?
N2 Ba1 N1 160.95(15) . . ?
N2 Ba1 N1 159.45(15) 2 . ?
O2 Ba1 N1 80.91(14) . 2 ?
O2 Ba1 N1 99.49(13) 2 2 ?
O1 Ba1 N1 80.31(13) 2 2 ?
O1 Ba1 N1 100.23(13) . 2 ?
N2 Ba1 N1 159.45(14) . 2 ?
N2 Ba1 N1 160.95(15) 2 2 ?
N1 Ba1 N1 28.06(17) . 2 ?
C1 P1 C1 86.6(3) 2 . ?
C8 P2 C8 86.9(4) 2 . ?
C1 N1 N1 112.7(3) . 2 ?
C1 N1 Ba1 171.3(3) . . ?
N1 N1 Ba1 75.97(9) 2 . ?
C8 N2 N2 113.3(3) . 2 ?
C8 N2 Ba1 170.9(4) . . ?
N2 N2 Ba1 75.87(9) 2 . ?
C15 O1 C18 107.8(6) . . ?
C15 O1 Ba1 127.1(5) . . ?
C18 O1 Ba1 124.8(4) . . ?
C22 O2 C19 106.7(6) . . ?
C22 O2 Ba1 123.7(5) . . ?
C19 O2 Ba1 128.7(4) . . ?
N1 C1 C2 119.9(4) . . ?
N1 C1 P1 114.0(3) . . ?
C2 C1 P1 126.0(4) . . ?
C7 C2 C3 118.0(6) . . ?
C7 C2 C1 122.0(5) . . ?
C3 C2 C1 119.9(5) . . ?
C4 C3 C2 120.4(8) . . ?
C4 C3 H3A 119.8 . . ?
C2 C3 H3A 119.8 . . ?
C5 C4 C3 120.5(9) . . ?
C5 C4 H4A 119.8 . . ?
C3 C4 H4A 119.8 . . ?
C6 C5 C4 120.3(9) . . ?
C6 C5 H5A 119.8 . . ?
C4 C5 H5A 119.8 . . ?
C5 C6 C7 120.3(10) . . ?
C5 C6 H6A 119.9 . . ?
C7 C6 H6A 119.9 . . ?
C2 C7 C6 120.4(8) . . ?
C2 C7 H7A 119.8 . . ?
C6 C7 H7A 119.8 . . ?
N2 C8 C9 120.1(5) . . ?
N2 C8 P2 113.3(4) . . ?
C9 C8 P2 126.6(4) . . ?
C14 C9 C10 116.8(6) . . ?
C14 C9 C8 122.6(5) . . ?
C10 C9 C8 120.5(6) . . ?
C11 C10 C9 119.6(7) . . ?
C11 C10 H10A 120.2 . . ?
C9 C10 H10A 120.2 . . ?
C12 C11 C10 122.3(8) . . ?
C12 C11 H11A 118.9 . . ?
C10 C11 H11A 118.9 . . ?
C11 C12 C13 118.4(8) . . ?
C11 C12 H12A 120.8 . . ?
C13 C12 H12A 120.8 . . ?
C14 C13 C12 119.5(8) . . ?
C14 C13 H13A 120.3 . . ?
C12 C13 H13A 120.3 . . ?
C13 C14 C9 123.4(7) . . ?
C13 C14 H14A 118.3 . . ?
C9 C14 H14A 118.3 . . ?
C16 C15 O1 107.0(8) . . ?
C16 C15 H15A 110.3 . . ?
O1 C15 H15A 110.3 . . ?
C16 C15 H15B 110.3 . . ?
O1 C15 H15B 110.3 . . ?
H15A C15 H15B 108.6 . . ?
C15 C16 C17 110.2(9) . . ?
C15 C16 H16A 109.6 . . ?
C17 C16 H16A 109.6 . . ?
C15 C16 H16B 109.6 . . ?
C17 C16 H16B 109.6 . . ?
H16A C16 H16B 108.1 . . ?
C16 C17 C18 102.6(9) . . ?
C16 C17 H17A 111.2 . . ?
C18 C17 H17A 111.2 . . ?
C16 C17 H17B 111.2 . . ?
C18 C17 H17B 111.2 . . ?
H17A C17 H17B 109.2 . . ?
O1 C18 C17 107.1(7) . . ?
O1 C18 H18A 110.3 . . ?
C17 C18 H18A 110.3 . . ?
O1 C18 H18B 110.3 . . ?
C17 C18 H18B 110.3 . . ?
H18A C18 H18B 108.6 . . ?
O2 C19 C20 104.6(6) . . ?
O2 C19 H19A 110.8 . . ?
C20 C19 H19A 110.8 . . ?
O2 C19 H19B 110.8 . . ?
C20 C19 H19B 110.8 . . ?
H19A C19 H19B 108.9 . . ?
C21 C20 C19 104.2(7) . . ?
C21 C20 H20A 110.9 . . ?
C19 C20 H20A 110.9 . . ?
C21 C20 H20B 110.9 . . ?
C19 C20 H20B 110.9 . . ?
H20A C20 H20B 108.9 . . ?
C22 C21 C20 106.9(8) . . ?
C22 C21 H21A 110.3 . . ?
C20 C21 H21A 110.3 . . ?
C22 C21 H21B 110.3 . . ?
C20 C21 H21B 110.3 . . ?
H21A C21 H21B 108.6 . . ?
C21 C22 O2 112.4(8) . . ?
C21 C22 H22B 109.1 . . ?
O2 C22 H22B 109.1 . . ?
C21 C22 H22A 109.1 . . ?
O2 C22 H22A 109.1 . . ?
H22B C22 H22A 107.9 . . ?
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
Ba1 O2 2.732(5) . ?
Ba1 O2 2.732(5) 2 ?
Ba1 O1 2.742(5) 2 ?
Ba1 O1 2.742(5) . ?
Ba1 N2 2.797(4) . ?
Ba1 N2 2.797(4) 2 ?
Ba1 N1 2.809(4) . ?
Ba1 N1 2.809(4) 2 ?
P1 C1 1.745(5) 2 ?
P1 C1 1.745(5) . ?
P2 C8 1.766(5) 2 ?
P2 C8 1.766(5) . ?
N1 C1 1.335(6) . ?
N1 N1 1.362(8) 2 ?
N2 C8 1.344(6) . ?
N2 N2 1.366(9) 2 ?
O1 C15 1.418(9) . ?
O1 C18 1.433(9) . ?
O2 C22 1.408(10) . ?
O2 C19 1.408(8) . ?
C1 C2 1.480(7) . ?
C2 C7 1.370(8) . ?
C2 C3 1.413(9) . ?
C3 C4 1.373(11) . ?
C3 H3A 0.9300 . ?
C4 C5 1.372(15) . ?
C4 H4A 0.9300 . ?
C5 C6 1.348(16) . ?
C5 H5A 0.9300 . ?
C6 C7 1.411(12) . ?
C6 H6A 0.9300 . ?
C7 H7A 0.9300 . ?
C8 C9 1.476(8) . ?
C9 C14 1.373(8) . ?
C9 C10 1.404(8) . ?
C10 C11 1.381(11) . ?
C10 H10A 0.9300 . ?
C11 C12 1.366(11) . ?
C11 H11A 0.9300 . ?
C12 C13 1.380(11) . ?
C12 H12A 0.9300 . ?
C13 C14 1.369(9) . ?
C13 H13A 0.9300 . ?
C14 H14A 0.9300 . ?
C15 C16 1.415(14) . ?
C15 H15A 0.9700 . ?
C15 H15B 0.9700 . ?
C16 C17 1.453(15) . ?
C16 H16A 0.9700 . ?
C16 H16B 0.9700 . ?
C17 C18 1.469(12) . ?
C17 H17A 0.9700 . ?
C17 H17B 0.9700 . ?
C18 H18A 0.9700 . ?
C18 H18B 0.9700 . ?
C19 C20 1.500(12) . ?
C19 H19A 0.9700 . ?
C19 H19B 0.9700 . ?
C20 C21 1.455(15) . ?
C20 H20A 0.9700 . ?
C20 H20B 0.9700 . ?
C21 C22 1.337(12) . ?
C21 H21A 0.9700 . ?
C21 H21B 0.9700 . ?
C22 H22B 0.9700 . ?
C22 H22A 0.9700 . ?
