#------------------------------------------------------------------------------
#$Date: 2016-03-25 15:17:58 +0100 (Fri 25 de Mar de 2016) $
#$Revision: 179962 $
#$URL: svn://www.crystallography.net/cod/cif/7/02/56/7025633.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_7025633
loop_
_publ_author_name
'Kunnas-Hiltunen, Susan'
'Haukka, Matti'
'Vepsäläinen, Jouko'
'Ahlgrén, Markku'
_publ_section_title
;
 Alkaline and alkaline earth metal complexes of dianhydride derivatives of
 clodronate and their hydrolysis products.
;
_journal_issue                   22
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5310
_journal_page_last               5318
_journal_paper_doi               10.1039/c002403a
_journal_volume                  39
_journal_year                    2010
_chemical_formula_moiety         'C5 H12 Ba Cl2 O11 P2'
_chemical_formula_sum            'C5 H12 Ba Cl2 O11 P2'
_chemical_formula_weight         518.33
_chemical_name_systematic
;
?
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 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                 118.240(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.7725(5)
_cell_length_b                   7.5324(2)
_cell_length_c                   14.5010(4)
_cell_measurement_reflns_used    9039
_cell_measurement_temperature    120(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      3.90
_cell_volume                     1517.73(8)
_computing_cell_refinement       'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_data_collection       'Collect (Nonius BV, 1997-2000)'
_computing_data_reduction        'Denzo/Scalepack (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'XP in SHELXTL v.5.1 (Bruker AXS, 1998)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       multi-scan
_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  0.0252
_diffrn_reflns_av_sigmaI/netI    0.0227
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9039
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         3.90
_exptl_absorpt_coefficient_mu    3.228
_exptl_absorpt_correction_T_max  0.7384
_exptl_absorpt_correction_T_min  0.4443
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'XPREP in SHELXL v.5.1 (Bruker AXS, 1998)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.268
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.567
_refine_diff_density_min         -0.770
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.122
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         1853
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.122
_refine_ls_R_factor_all          0.0203
_refine_ls_R_factor_gt           0.0183
_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)+(0.0090P)²+5.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0415
_refine_ls_wR_factor_ref         0.0423
_reflns_number_gt                1759
_reflns_number_total             1853
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c002403a.txt
_cod_data_source_block           Structure(2)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               7025633
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z'
'-x, -y, -z'
'x, -y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, 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 0.289533(12) 0.0000 0.056857(13) 0.00817(6) Uani 1 2 d S
Cl1 Cl 0.03309(4) 0.19314(8) 0.38035(4) 0.01472(12) Uani 1 1 d .
P1 P 0.06598(5) 0.0000 0.22140(6) 0.00776(15) Uani 1 2 d S
P2 P -0.13263(5) 0.0000 0.21335(6) 0.00821(15) Uani 1 2 d S
O1 O 0.47972(15) 0.0000 0.18668(18) 0.0159(5) Uani 1 2 d S
H1 H 0.5097 -0.0931 0.1887 0.024 Uiso 1 1 d R
O2 O 0.12959(10) 0.2325(2) 0.01942(11) 0.0121(3) Uani 1 1 d .
H2A H 0.1178 0.2391 0.0698 0.018 Uiso 1 1 d R
H2B H 0.0794 0.1992 -0.0311 0.018 Uiso 1 1 d R
O11 O 0.04819(10) 0.1706(2) 0.16407(12) 0.0123(3) Uani 1 1 d .
O12 O 0.17584(14) 0.0000 0.32221(16) 0.0119(4) Uani 1 2 d S
O13 O 0.24535(16) 0.0000 0.21880(18) 0.0183(5) Uani 1 2 d S
O21 O -0.16168(10) -0.1683(2) 0.15380(12) 0.0125(3) Uani 1 1 d .
O22 O -0.16190(15) 0.0000 0.30779(17) 0.0132(5) Uani 1 2 d S
O23 O -0.32053(16) 0.0000 0.19486(18) 0.0168(5) Uani 1 2 d S
C1 C 0.0002(2) 0.0000 0.2992(2) 0.0090(6) Uani 1 2 d S
C11 C 0.2537(2) 0.0000 0.3057(2) 0.0117(6) Uani 1 2 d S
C12 C 0.3469(2) 0.0000 0.4043(3) 0.0208(7) Uani 1 2 d S
H12A H 0.3346 0.0000 0.4645 0.031 Uiso 1 2 d SR
H12B H 0.3838 0.1062 0.4067 0.031 Uiso 1 1 d R
C21 C -0.2571(2) 0.0000 0.2835(3) 0.0125(6) Uani 1 2 d S
C22 C -0.2694(2) 0.0000 0.3794(3) 0.0201(7) Uani 1 2 d S
H22A H -0.2061 0.0000 0.4417 0.030 Uiso 1 2 d SR
H22B H -0.3051 -0.1062 0.3797 0.030 Uiso 1 1 d 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'
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'
Cl Cl 0.1484 0.1585 '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
O1 Ba1 O13 92.97(7) . .
O1 Ba1 O21 72.32(3) . 3
O13 Ba1 O21 71.97(4) . 3
O1 Ba1 O21 72.32(3) . 8_545
O13 Ba1 O21 71.97(4) . 8_545
O21 Ba1 O21 127.10(6) 3 8_545
O1 Ba1 O2 73.58(5) . 4_545
O13 Ba1 O2 131.90(3) . 4_545
O21 Ba1 O2 139.06(4) 3 4_545
O21 Ba1 O2 59.93(4) 8_545 4_545
O1 Ba1 O2 73.58(5) . 7
O13 Ba1 O2 131.90(3) . 7
O21 Ba1 O2 59.93(4) 3 7
O21 Ba1 O2 139.06(4) 8_545 7
O2 Ba1 O2 89.12(6) 4_545 7
O1 Ba1 O2 135.66(4) . 6
O13 Ba1 O2 67.08(5) . 6
O21 Ba1 O2 129.97(4) 3 6
O21 Ba1 O2 64.04(4) 8_545 6
O2 Ba1 O2 90.56(4) 4_545 6
O2 Ba1 O2 148.899(17) 7 6
O1 Ba1 O2 135.66(4) . .
O13 Ba1 O2 67.08(5) . .
O21 Ba1 O2 64.04(4) 3 .
O21 Ba1 O2 129.97(4) 8_545 .
O2 Ba1 O2 148.899(17) 4_545 .
O2 Ba1 O2 90.56(4) 7 .
O2 Ba1 O2 74.20(6) 6 .
O1 Ba1 O21 134.22(5) . 2
O13 Ba1 O21 123.01(5) . 2
O21 Ba1 O21 140.91(4) 3 2
O21 Ba1 O21 91.52(4) 8_545 2
O2 Ba1 O21 61.51(4) 4_545 2
O2 Ba1 O21 96.34(4) 7 2
O2 Ba1 O21 56.91(4) 6 2
O2 Ba1 O21 87.65(4) . 2
O1 Ba1 O21 134.22(5) . 5
O13 Ba1 O21 123.01(5) . 5
O21 Ba1 O21 91.52(4) 3 5
O21 Ba1 O21 140.91(4) 8_545 5
O2 Ba1 O21 96.34(4) 4_545 5
O2 Ba1 O21 61.51(4) 7 5
O2 Ba1 O21 87.65(4) 6 5
O2 Ba1 O21 56.91(4) . 5
O21 Ba1 O21 49.49(6) 2 5
O1 Ba1 Ba1 108.137(12) . 7
O13 Ba1 Ba1 101.163(16) . 7
O21 Ba1 Ba1 48.18(3) 3 7
O21 Ba1 Ba1 173.11(3) 8_545 7
O2 Ba1 Ba1 126.94(3) 4_545 7
O2 Ba1 Ba1 45.60(3) 7 7
O2 Ba1 Ba1 114.24(3) 6 7
O2 Ba1 Ba1 44.96(3) . 7
O21 Ba1 Ba1 92.79(3) 2 7
O21 Ba1 Ba1 43.35(3) 5 7
O11 P1 O11 120.07(13) 6 .
O11 P1 O12 109.64(7) 6 .
O11 P1 O12 109.64(7) . .
O11 P1 C1 109.16(7) 6 .
O11 P1 C1 109.16(7) . .
O12 P1 C1 96.63(12) . .
O21 P2 O21 117.97(13) . 6
O21 P2 O22 110.84(7) . .
O21 P2 O22 110.84(7) 6 .
O21 P2 C1 109.25(7) . .
O21 P2 C1 109.25(7) 6 .
O22 P2 C1 96.55(12) . .
Ba1 O1 H1 116.7 . .
Ba1 O2 Ba1 89.44(4) 7 .
Ba1 O2 H2A 128.2 7 .
Ba1 O2 H2A 113.9 . .
Ba1 O2 H2B 106.7 7 .
Ba1 O2 H2B 111.5 . .
H2A O2 H2B 106.2 . .
C11 O12 P1 120.00(19) . .
C11 O13 Ba1 161.5(2) . .
P2 O21 Ba1 175.41(9) . 3_445
P2 O21 Ba1 95.99(7) . 5
Ba1 O21 Ba1 88.48(4) 3_445 5
C21 O22 P2 119.5(2) . .
Cl1 C1 Cl1 109.02(15) . 6
Cl1 C1 P1 109.17(11) . .
Cl1 C1 P1 109.17(11) 6 .
Cl1 C1 P2 108.91(11) . .
Cl1 C1 P2 108.91(11) 6 .
P1 C1 P2 111.62(15) . .
O13 C11 O12 121.6(3) . .
O13 C11 C12 125.1(3) . .
O12 C11 C12 113.2(3) . .
C11 C12 H12A 109.5 . .
C11 C12 H12B 109.5 . .
H12A C12 H12B 109.5 . .
O23 C21 O22 122.3(3) . .
O23 C21 C22 126.0(3) . .
O22 C21 C22 111.7(3) . .
C21 C22 H22A 109.5 . .
C21 C22 H22B 109.5 . .
H22A C22 H22B 109.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 O1 2.683(2) .
Ba1 O13 2.747(2) .
Ba1 O21 2.7902(15) 3
Ba1 O21 2.7902(15) 8_545
Ba1 O2 2.8716(15) 4_545
Ba1 O2 2.8716(15) 7
Ba1 O2 2.9034(15) 6
Ba1 O2 2.9034(15) .
Ba1 O21 3.0293(15) 2
Ba1 O21 3.0293(15) 5
Ba1 Ba1 4.06356(16) 7
Cl1 C1 1.7867(17) .
P1 O11 1.4833(16) 6
P1 O11 1.4833(16) .
P1 O12 1.656(2) .
P1 C1 1.859(3) .
P2 O21 1.4796(16) .
P2 O21 1.4796(16) 6
P2 O22 1.639(2) .
P2 C1 1.863(3) .
O1 H1 0.8389 .
O2 H2A 0.8362 .
O2 H2B 0.8226 .
O12 C11 1.358(4) .
O13 C11 1.203(4) .
O22 C21 1.370(4) .
O23 C21 1.198(4) .
C1 Cl1 1.7867(17) 6
C11 C12 1.489(4) .
C12 H12A 0.9800 .
C12 H12B 0.9800 .
C21 C22 1.493(4) .
C22 H22A 0.9800 .
C22 H22B 0.9800 .
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O1 H1 O11 0.84 1.97 2.7866(19) 165.4 3_545
O2 H2A O11 0.84 2.18 2.969(2) 156.8 .
O2 H2A O23 0.84 2.54 3.043(2) 120.2 3
O2 H2B O11 0.82 2.04 2.846(2) 168.2 2
