#------------------------------------------------------------------------------
#$Date: 2017-06-09 05:10:33 +0300 (Fri, 09 Jun 2017) $
#$Revision: 197673 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/22/84/7228448.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_7228448
loop_
_publ_author_name
'Gelfand, Benjamin S.'
'Taylor, Jared M.'
'Shimizu, George K. H.'
_publ_section_title
;
 Extracting structural trends from systematic variation of
 phosphonate/phosphonate monoester coordination polymers
;
_journal_name_full               CrystEngComm
_journal_paper_doi               10.1039/C7CE00579B
_journal_year                    2017
_chemical_formula_sum            'C6 H9 Ba O10 P3'
_chemical_formula_weight         471.38
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-04-28 deposited with the CCDC.
2017-05-15 downloaded from the CCDC.
;
_cell_angle_alpha                98.71(3)
_cell_angle_beta                 98.91(3)
_cell_angle_gamma                103.81(3)
_cell_formula_units_Z            2
_cell_length_a                   8.4610(17)
_cell_length_b                   8.5060(17)
_cell_length_c                   9.3020(19)
_cell_measurement_reflns_used    1640
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      27.485
_cell_measurement_theta_min      0.998
_cell_volume                     629.8(3)
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0250
_diffrn_reflns_av_unetI/netI     0.0374
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            4797
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.460
_diffrn_reflns_theta_min         3.793
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    3.582
_exptl_absorpt_correction_T_max  0.345
_exptl_absorpt_correction_T_min  0.341
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sheldrick, G. M., SADABS 1997'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.486
_exptl_crystal_description       block
_exptl_crystal_F_000             452
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.540
_refine_diff_density_min         -0.670
_refine_diff_density_rms         0.134
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     214
_refine_ls_number_reflns         2836
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0274
_refine_ls_R_factor_gt           0.0237
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0179P)²+1.1587P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0525
_refine_ls_wR_factor_ref         0.0542
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2627
_reflns_number_total             2836
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            c7ce00579b1.cif
_cod_data_source_block           2
_cod_original_cell_volume        629.8(2)
_cod_database_code               7228448
_shelx_shelxl_version_number     2014/7
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 1.26344(2) 0.56009(2) 0.95610(2) 0.00911(7) Uani 1 1 d . . .
C1 C 0.6979(4) -0.0796(4) 0.3877(3) 0.0101(6) Uani 1 1 d . . .
C2 C 0.6596(4) -0.1863(4) 0.4847(3) 0.0105(6) Uani 1 1 d . . .
H2 H 0.602(4) -0.298(5) 0.447(4) 0.013 Uiso 1 1 d U . .
C3 C 0.7026(4) -0.1290(4) 0.6383(3) 0.0096(6) Uani 1 1 d . . .
C4 C 0.7879(4) 0.0371(4) 0.6945(3) 0.0095(6) Uani 1 1 d . . .
H4 H 0.817(4) 0.080(4) 0.797(4) 0.011 Uiso 1 1 d U . .
C5 C 0.8234(4) 0.1454(4) 0.5984(3) 0.0092(6) Uani 1 1 d . . .
C6 C 0.7775(4) 0.0869(4) 0.4450(3) 0.0119(6) Uani 1 1 d . . .
H6 H 0.801(5) 0.162(5) 0.384(4) 0.014 Uiso 1 1 d U . .
O1 O 0.4923(3) -0.0798(3) 0.1332(3) 0.0149(5) Uani 1 1 d . . .
O2 O 0.5677(3) -0.3394(2) 0.1478(2) 0.0101(4) Uani 1 1 d . . .
O3 O 0.7900(3) -0.0910(3) 0.1270(2) 0.0148(5) Uani 1 1 d . . .
O4 O 0.5844(3) -0.4451(3) 0.6590(2) 0.0113(4) Uani 1 1 d . . .
O5 O 0.4828(3) -0.2352(3) 0.8103(2) 0.0117(4) Uani 1 1 d . . .
O6 O 0.7760(3) -0.2579(3) 0.8848(2) 0.0116(4) Uani 1 1 d . . .
O7 O 0.9201(3) 0.3991(2) 0.8328(2) 0.0106(4) Uani 1 1 d . . .
O8 O 1.1032(3) 0.4050(3) 0.6499(2) 0.0116(4) Uani 1 1 d . . .
O9 O 0.8235(3) 0.4576(3) 0.5735(2) 0.0113(4) Uani 1 1 d . . .
O1W O 1.1003(4) 0.7647(3) 0.8633(3) 0.0223(6) Uani 1 1 d . . .
P1 P 0.63535(10) -0.15584(9) 0.19164(8) 0.00831(16) Uani 1 1 d . . .
P2 P 0.63237(9) -0.26958(9) 0.75652(8) 0.00777(15) Uani 1 1 d . . .
P3 P 0.91508(9) 0.36418(9) 0.66888(8) 0.00774(16) Uani 1 1 d . . .
H1WA H 1.019(7) 0.756(7) 0.863(6) 0.041(17) Uiso 1 1 d . . .
H8 H 1.123(7) 0.450(7) 0.576(7) 0.069(19) Uiso 1 1 d . . .
H1WB H 1.136(8) 0.872(8) 0.870(7) 0.069(19) Uiso 1 1 d . . .
H1 H 0.508(9) 0.008(8) 0.143(8) 0.09(3) Uiso 1 1 d . . .
H4A H 0.675(7) -0.484(6) 0.634(6) 0.052(15) Uiso 1 1 d . . .
H6A H 0.783(9) -0.172(9) 0.998(9) 0.10(2) Uiso 1 1 d . A 1
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'
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
O1W Ba1 O7 77.46(8) . 2_767
O1W Ba1 O2 123.72(8) . 1_666
O7 Ba1 O2 96.12(7) 2_767 1_666
O1W Ba1 O2 140.62(8) . 2_756
O7 Ba1 O2 138.59(6) 2_767 2_756
O2 Ba1 O2 76.08(7) 1_666 2_756
O1W Ba1 O7 67.70(8) . .
O7 Ba1 O7 70.57(7) 2_767 .
O2 Ba1 O7 161.14(6) 1_666 .
O2 Ba1 O7 104.70(7) 2_756 .
O1W Ba1 O5 74.76(8) . 1_665
O7 Ba1 O5 137.77(6) 2_767 1_665
O2 Ba1 O5 74.39(7) 1_666 1_665
O2 Ba1 O5 80.04(6) 2_756 1_665
O7 Ba1 O5 124.46(6) . 1_665
O1W Ba1 O8 75.25(8) . .
O7 Ba1 O8 120.77(6) 2_767 .
O2 Ba1 O8 142.44(7) 1_666 .
O2 Ba1 O8 71.52(6) 2_756 .
O7 Ba1 O8 50.56(7) . .
O5 Ba1 O8 81.69(7) 1_665 .
O1W Ba1 O6 141.63(8) . 2_757
O7 Ba1 O6 71.15(6) 2_767 2_757
O2 Ba1 O6 81.79(6) 1_666 2_757
O2 Ba1 O6 67.51(6) 2_756 2_757
O7 Ba1 O6 81.24(6) . 2_757
O5 Ba1 O6 143.51(6) 1_665 2_757
O8 Ba1 O6 102.38(6) . 2_757
O1W Ba1 O1 76.30(8) . 1_666
O7 Ba1 O1 82.98(7) 2_767 1_666
O2 Ba1 O1 47.53(6) 1_666 1_666
O2 Ba1 O1 115.86(6) 2_756 1_666
O7 Ba1 O1 138.83(6) . 1_666
O5 Ba1 O1 59.98(6) 1_665 1_666
O8 Ba1 O1 136.97(6) . 1_666
O6 Ba1 O1 119.88(6) 2_757 1_666
O1W Ba1 P1 101.56(7) . 1_666
O7 Ba1 P1 92.17(5) 2_767 1_666
O2 Ba1 P1 22.16(4) 1_666 1_666
O2 Ba1 P1 93.48(5) 2_756 1_666
O7 Ba1 P1 161.00(5) . 1_666
O5 Ba1 P1 63.55(5) 1_665 1_666
O8 Ba1 P1 144.29(5) . 1_666
O6 Ba1 P1 101.12(5) 2_757 1_666
O1 Ba1 P1 25.57(4) 1_666 1_666
O1W Ba1 Ba1 147.50(7) . 2_867
O7 Ba1 Ba1 122.99(5) 2_767 2_867
O2 Ba1 Ba1 38.12(5) 1_666 2_867
O2 Ba1 Ba1 37.96(5) 2_756 2_867
O7 Ba1 Ba1 139.56(4) . 2_867
O5 Ba1 Ba1 73.71(5) 1_665 2_867
O8 Ba1 Ba1 107.51(5) . 2_867
O6 Ba1 Ba1 70.50(5) 2_757 2_867
O1 Ba1 Ba1 81.34(5) 1_666 2_867
P1 Ba1 Ba1 56.74(2) 1_666 2_867
O1W Ba1 Ba1 68.40(7) . 2_767
O7 Ba1 Ba1 36.38(5) 2_767 2_767
O2 Ba1 Ba1 131.20(5) 1_666 2_767
O2 Ba1 Ba1 127.34(5) 2_756 2_767
O7 Ba1 Ba1 34.19(4) . 2_767
O5 Ba1 Ba1 142.86(4) 1_665 2_767
O8 Ba1 Ba1 84.56(5) . 2_767
O6 Ba1 Ba1 73.24(5) 2_757 2_767
O1 Ba1 Ba1 113.62(5) 1_666 2_767
P1 Ba1 Ba1 128.12(2) 1_666 2_767
Ba1 Ba1 Ba1 143.436(14) 2_867 2_767
C2 C1 C6 119.4(3) . .
C2 C1 P1 119.5(2) . .
C6 C1 P1 121.0(2) . .
C1 C2 C3 120.8(3) . .
C2 C3 C4 119.2(3) . .
C2 C3 P2 118.2(2) . .
C4 C3 P2 122.4(2) . .
C5 C4 C3 120.4(3) . .
C4 C5 C6 119.7(3) . .
C4 C5 P3 120.9(2) . .
C6 C5 P3 119.3(2) . .
C1 C6 C5 120.5(3) . .
P1 O1 Ba1 91.23(11) . 1_444
P1 O2 Ba1 113.80(11) . 1_444
P1 O2 Ba1 126.17(12) . 2_756
Ba1 O2 Ba1 103.92(7) 1_444 2_756
P2 O5 Ba1 126.96(11) . 1_445
P2 O6 Ba1 115.62(11) . 2_757
P3 O7 Ba1 144.59(12) . 2_767
P3 O7 Ba1 103.40(11) . .
Ba1 O7 Ba1 109.43(7) 2_767 .
P3 O8 Ba1 98.95(11) . .
O2 P1 O3 112.41(13) . .
O2 P1 O1 106.64(13) . .
O3 P1 O1 110.37(13) . .
O2 P1 C1 114.43(13) . .
O3 P1 C1 105.38(14) . .
O1 P1 C1 107.54(14) . .
O2 P1 Ba1 44.04(8) . 1_444
O3 P1 Ba1 120.61(9) . 1_444
O1 P1 Ba1 63.20(10) . 1_444
C1 P1 Ba1 133.65(11) . 1_444
O5 P2 O6 112.51(13) . .
O5 P2 O4 109.85(13) . .
O6 P2 O4 108.40(13) . .
O5 P2 C3 110.16(13) . .
O6 P2 C3 109.68(13) . .
O4 P2 C3 106.01(13) . .
O7 P3 O9 117.61(13) . .
O7 P3 O8 106.10(12) . .
O9 P3 O8 108.64(12) . .
O7 P3 C5 108.57(13) . .
O9 P3 C5 107.95(13) . .
O8 P3 C5 107.58(13) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ba1 O1W 2.630(3) .
Ba1 O7 2.717(2) 2_767
Ba1 O2 2.757(2) 1_666
Ba1 O2 2.767(2) 2_756
Ba1 O7 2.868(2) .
Ba1 O5 2.875(2) 1_665
Ba1 O8 2.916(2) .
Ba1 O6 3.131(2) 2_757
Ba1 O1 3.240(3) 1_666
Ba1 P1 3.6295(19) 1_666
Ba1 Ba1 4.3508(10) 2_867
Ba1 Ba1 4.5597(11) 2_767
C1 C2 1.393(4) .
C1 C6 1.395(4) .
C1 P1 1.790(3) .
C2 C3 1.398(4) .
C3 C4 1.401(4) .
C3 P2 1.804(3) .
C4 C5 1.393(4) .
C5 C6 1.398(4) .
C5 P3 1.810(3) .
O1 P1 1.567(2) .
O2 P1 1.497(2) .
O3 P1 1.542(2) .
O4 P2 1.551(2) .
O5 P2 1.506(2) .
O6 P2 1.539(2) .
O7 P3 1.501(2) .
O8 P3 1.590(2) .
O9 P3 1.520(2) .
