#------------------------------------------------------------------------------
#$Date: 2016-02-16 22:30:59 +0200 (Tue, 16 Feb 2016) $
#$Revision: 176467 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/08/4330828.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_4330828
loop_
_publ_author_name
'Johannes Weber'
'Gisbert Grossmann'
'Konstantinos D. Demadis'
'Nikos Daskalakis'
'Erica Brendler'
'Martin Mangstl'
'Jörn Schmedt auf der Günne'
_publ_contact_author_address
;Department für Chemie
Ludwig-Maximilians-Universität München
Butenandtstr. 5-13 (Haus D)
D-81377 München
Germany
;
_publ_contact_author_email       gunnej@cup.uni-muenchen.de
_publ_contact_author_fax         +49-89-2180-77440
_publ_contact_author_name        'Jörn Schmedt auf der Günne'
_publ_contact_author_phone       +49-89-2810-77433
_publ_section_title
;
 Linking 31P Magnetic Shielding Tensors to Crystal Structures:
 Experimental and Theoretical Studies on Metal(II)
 Aminotris(methylenephosphonates)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11466
_journal_page_last               11477
_journal_paper_doi               10.1021/ic301192y
_journal_volume                  51
_journal_year                    2012
_chemical_formula_sum            'C3 H10 Ba N O9 P3'
_chemical_formula_weight         434.36
_chemical_name_systematic
;
Barium (amino-tris(methylenephosphonate))
;
_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                101.766(3)
_cell_angle_beta                 95.984(3)
_cell_angle_gamma                107.083(2)
_cell_formula_units_Z            2
_cell_length_a                   7.6382(12)
_cell_length_b                   8.4834(13)
_cell_length_c                   9.1417(14)
_cell_measurement_temperature    293(2)
_cell_volume                     545.74(15)
_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 0.910
_diffrn_measured_fraction_theta_max 0.910
_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  0.0160
_diffrn_reflns_av_sigmaI/netI    0.0242
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       8
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            3862
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.31
_exptl_absorpt_coefficient_mu    4.117
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            COLORLESS
_exptl_crystal_density_diffrn    2.643
_exptl_crystal_description       BLOCK
_exptl_crystal_F_000             416
_exptl_crystal_size_max          .18
_exptl_crystal_size_mid          .15
_exptl_crystal_size_min          .04
_refine_diff_density_max         1.024
_refine_diff_density_min         -0.643
_refine_diff_density_rms         0.141
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2468
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0263
_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)+(0.0484P)²+0.1838P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0668
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                2282
_reflns_number_total             2468
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301192y_si_002_1.cif
_cod_data_source_block           BaAMP
_cod_original_formula_sum        'C3 H10 Ba1 N1 O9 P3'
_cod_database_code               4330828
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 0.39400(3) 0.22371(3) 0.55561(2) 0.01439(8) Uani 1 1 d .
P1 P 0.20865(6) -0.16398(6) 0.17788(5) 0.01551(19) Uani 1 1 d R
P2 P 0.12650(6) -0.18596(6) 0.59365(5) 0.01359(18) Uani 1 1 d R
P3 P 0.51428(6) -0.39133(6) 0.81442(5) 0.01562(18) Uani 1 1 d R
O1 O 0.19288(6) -0.00010(6) 1.26889(5) 0.0207(5) Uani 1 1 d R
O2 O 0.39151(6) -0.19145(6) 1.20287(5) 0.0248(6) Uani 1 1 d R
O3 O 0.04496(6) -0.31989(6) 1.19392(5) 0.0260(6) Uani 1 1 d RD
O4 O 0.31282(6) -0.15150(6) 0.54622(5) 0.0211(5) Uani 1 1 d R
O5 O -0.04280(6) -0.26295(6) 0.47033(5) 0.0185(5) Uani 1 1 d R
O6 O 0.12724(6) -0.01259(6) 0.69451(5) 0.0204(5) Uani 1 1 d RD
O7 O 0.36938(6) -0.55011(6) 0.82918(5) 0.0205(5) Uani 1 1 d R
O8 O 0.56395(6) -0.40388(6) 0.66044(5) 0.0226(6) Uani 1 1 d R
O9 O 0.69570(6) -0.33765(6) 0.93600(5) 0.0235(6) Uani 1 1 d RD
N1 N 0.20926(6) -0.28618(6) 0.86850(5) 0.0152(6) Uani 1 1 d RD
C1 C 0.14740(6) -0.16517(6) 0.97893(5) 0.0187(7) Uani 1 1 d .
C2 C 0.09491(6) -0.33799(6) 0.71045(5) 0.0169(7) Uani 1 1 d R
C3 C 0.41667(6) -0.21967(6) 0.87127(5) 0.0179(7) Uani 1 1 d R
H1 H 0.0304 -0.3044 1.2826 0.031 Uiso 1 1 d RD
H2 H 0.0253 -0.0128 0.7104 0.024 Uiso 1 1 d RD
H3 H 0.6706 -0.3741 1.0095 0.028 Uiso 1 1 d RD
H4 H 0.1837 -0.3944 0.8958 0.018 Uiso 1 1 d RD
H5 H 0.0134 -0.1945 0.9537 0.022 Uiso 1 1 calc R
H6 H 0.2022 -0.0511 0.9666 0.022 Uiso 1 1 calc R
H7 H -0.0352 -0.3733 0.7204 0.020 Uiso 1 1 calc R
H8 H 0.1188 -0.4376 0.6547 0.020 Uiso 1 1 calc R
H9 H 0.4782 -0.1535 0.9729 0.021 Uiso 1 1 calc R
H10 H 0.4410 -0.1447 0.8033 0.021 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
Ba Ba -0.3244 2.2819 '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'
C C 0.0033 0.0016 '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'
N N 0.0061 0.0033 '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'
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
O4 Ba1 O2 73.2 2_656 2_656
O4 Ba1 O8 80.5 2_656 2_666
O2 Ba1 O8 138.0 2_656 2_666
O4 Ba1 O5 155.9 2_656 2_556
O2 Ba1 O5 130.1 2_656 2_556
O8 Ba1 O5 82.8 2_666 2_556
O4 Ba1 O1 83.2 2_656 .
O2 Ba1 O1 134.6 2_656 .
O8 Ba1 O1 71.6 2_666 .
O5 Ba1 O1 75.0 2_556 .
O4 Ba1 O7 131.4 2_656 .
O2 Ba1 O7 70.3 2_656 .
O8 Ba1 O7 107.0 2_666 .
O5 Ba1 O7 70.4 2_556 .
O1 Ba1 O7 145.2 . .
O4 Ba1 O8 98.3 2_656 .
O2 Ba1 O8 89.1 2_656 .
O8 Ba1 O8 62.7 2_666 .
O5 Ba1 O8 89.4 2_556 .
O1 Ba1 O8 133.1 . .
O7 Ba1 O8 51.0 . .
O4 Ba1 O6 122.0 2_656 .
O2 Ba1 O6 75.5 2_656 .
O8 Ba1 O6 146.4 2_666 .
O5 Ba1 O6 67.2 2_556 .
O1 Ba1 O6 85.8 . .
O7 Ba1 O6 77.8 . .
O8 Ba1 O6 128.6 . .
O4 Ba1 O4 76.1 2_656 .
O2 Ba1 O4 70.7 2_656 .
O8 Ba1 O4 133.5 2_666 .
O5 Ba1 O4 103.7 2_556 .
O1 Ba1 O4 66.2 . .
O7 Ba1 O4 118.7 . .
O8 Ba1 O4 159.7 . .
O6 Ba1 O4 47.8 . .
O4 Ba1 P3 113.5 2_656 .
O2 Ba1 P3 75.2 2_656 .
O8 Ba1 P3 86.4 2_666 .
O5 Ba1 P3 82.6 2_556 .
O1 Ba1 P3 150.1 . .
O7 Ba1 P3 26.0 . .
O8 Ba1 P3 25.6 . .
O6 Ba1 P3 103.6 . .
O4 Ba1 P3 139.8 . .
O4 Ba1 P2 100.4 2_656 .
O2 Ba1 P2 78.9 2_656 .
O8 Ba1 P2 138.9 2_666 .
O5 Ba1 P2 81.0 2_556 .
O1 Ba1 P2 67.8 . .
O7 Ba1 P2 102.7 . .
O8 Ba1 P2 153.7 . .
O6 Ba1 P2 25.6 . .
O4 Ba1 P2 24.4 . .
P3 Ba1 P2 128.2 . .
O4 Ba1 Ba1 40.742(10) 2_656 2_656
O2 Ba1 Ba1 66.723(13) 2_656 2_656
O8 Ba1 Ba1 111.367(14) 2_666 2_656
O5 Ba1 Ba1 134.697(13) 2_556 2_656
O1 Ba1 Ba1 70.048(13) . 2_656
O7 Ba1 Ba1 135.857(12) . 2_656
O8 Ba1 Ba1 135.777(14) . 2_656
O6 Ba1 Ba1 82.199(15) . 2_656
O4 Ba1 Ba1 35.356(11) . 2_656
P3 Ba1 Ba1 138.686(12) . 2_656
P2 Ba1 Ba1 59.690(13) . 2_656
N1 C1 P1 114.6 1_554 .
N1 C1 H5 108.6 1_554 .
P1 C1 H5 108.6 . .
N1 C1 H6 108.6 1_554 .
P1 C1 H6 108.6 . .
H5 C1 H6 107.6 . .
N1 C2 P2 119.4 . .
N1 C2 H7 107.5 . .
P2 C2 H7 107.5 . .
N1 C2 H8 107.5 . .
P2 C2 H8 107.5 . .
H7 C2 H8 107.0 . .
N1 C3 P3 112.3 1_565 .
N1 C3 H9 109.1 1_565 .
P3 C3 H9 109.1 . .
N1 C3 H10 109.1 1_565 .
P3 C3 H10 109.1 . .
H9 C3 H10 107.9 . .
C1 N1 C3 111.4 1_556 1_545
C1 N1 C2 112.8 1_556 .
C3 N1 C2 113.4 1_545 .
C1 N1 H4 110.0 1_556 .
C3 N1 H4 106.9 1_545 .
C2 N1 H4 101.8 . .
P1 O1 Ba1 132.0 . .
P1 O2 Ba1 134.7 . 2_656
P1 O3 H1 108.6 . .
P2 O4 Ba1 157.3 . 2_656
P2 O4 Ba1 98.6 . .
Ba1 O4 Ba1 103.901(15) 2_656 .
P2 O5 Ba1 132.3 . 2_556
P2 O6 Ba1 98.8 . .
P2 O6 H2 113.1 . .
Ba1 O6 H2 128.7 . .
P3 O7 Ba1 97.4 . .
P3 O9 H3 109.5 . .
P3 O8 Ba1 140.0 . 2_666
P3 O8 Ba1 95.6 . .
Ba1 O8 Ba1 117.310(18) 2_666 .
O2 P1 O1 117.1 . .
O2 P1 O3 111.9 . .
O1 P1 O3 109.9 . .
O2 P1 C1 109.5 . .
O1 P1 C1 105.6 . .
O3 P1 C1 101.5 . .
O4 P2 O5 117.5 . .
O4 P2 O6 105.8 . .
O5 P2 O6 111.4 . .
O4 P2 C2 111.0 . .
O5 P2 C2 103.2 . .
O6 P2 C2 107.7 . .
O4 P2 Ba1 57.0 . .
O5 P2 Ba1 110.2 . .
O6 P2 Ba1 55.6 . .
C2 P2 Ba1 146.3 . .
O8 P3 O7 113.7 . .
O8 P3 O9 109.5 . .
O7 P3 O9 112.3 . .
O8 P3 C3 112.8 . .
O7 P3 C3 104.9 . .
O9 P3 C3 103.1 . .
O8 P3 Ba1 58.9 . .
O7 P3 Ba1 56.6 . .
O9 P3 Ba1 118.1 . .
C3 P3 Ba1 138.6 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 O4 2.6954 2_656
Ba1 O2 2.7183 2_656
Ba1 O8 2.7231 2_666
Ba1 O5 2.7905 2_556
Ba1 O1 2.8727 .
Ba1 O7 2.8851 .
Ba1 O8 2.9464 .
Ba1 O6 2.9933 .
Ba1 O4 3.0401 .
Ba1 P3 3.4263 .
Ba1 P2 3.5837 .
Ba1 Ba1 4.5215(7) 2_656
C1 N1 1.5027 1_554
C1 P1 1.8273 .
C1 H5 0.9700 .
C1 H6 0.9700 .
C2 N1 1.5153 .
C2 P2 1.8150 .
C2 H7 0.9700 .
C2 H8 0.9700 .
C3 N1 1.5131 1_565
C3 P3 1.8322 .
C3 H9 0.9700 .
C3 H10 0.9700 .
N1 C1 1.5027 1_556
N1 C3 1.5131 1_545
N1 H4 0.9705 .
O1 P1 1.5123 .
O2 P1 1.4845 .
O2 Ba1 2.7183 2_656
O3 P1 1.5747 .
O3 H1 0.8186 .
O4 P2 1.4949 .
O4 Ba1 2.6954 2_656
O5 P2 1.5065 .
O5 Ba1 2.7905 2_556
O6 P2 1.5666 .
O6 H2 0.8061 .
O7 P3 1.5123 .
O9 P3 1.5699 .
O9 H3 0.8131 .
O8 P3 1.4869 .
O8 Ba1 2.7231 2_666
