#------------------------------------------------------------------------------
#$Date: 2021-09-06 12:11:57 +0300 (Mon, 06 Sep 2021) $
#$Revision: 268543 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/12/84/7128479.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_7128479
loop_
_publ_author_name
'Ben Uliel, Tal'
'Farber, Eliyahu M.'
'Aviv, Hagit'
'Stroek, Wowa'
'Farbinteanu, Marilena'
'Tischler, Yaakov R.'
'Eisenberg, David'
_publ_section_title
;
 Combining polarized low-frequency Raman with XRD to identify directional
 structural motifs in a pyrolysis precursor.
;
_journal_issue                   57
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7015
_journal_page_last               7018
_journal_paper_doi               10.1039/d1cc00420d
_journal_volume                  57
_journal_year                    2021
_chemical_formula_moiety         'C10 H20 Ba N2 O11, H2 O'
_chemical_formula_sum            'C10 H22 Ba N2 O12'
_chemical_formula_weight         499.63
_chemical_name_common            'Eisenberg2 (Eliyahu)'
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2021-01-10 deposited with the CCDC.	2021-06-09 downloaded from the CCDC.
;
_cell_angle_alpha                99.936(3)
_cell_angle_beta                 100.163(3)
_cell_angle_gamma                110.800(3)
_cell_formula_units_Z            2
_cell_length_a                   7.2640(4)
_cell_length_b                   9.1520(4)
_cell_length_c                   14.5730(9)
_cell_measurement_reflns_used    2897
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      25.046
_cell_measurement_theta_min      2.938
_cell_volume                     861.85(9)
_computing_cell_refinement       'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius, 2006)'
_computing_data_reduction        'DENZO HKL2000 (Otwinowski & Minor 1997)'
_computing_molecular_graphics    'Mercury 3.10.1'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      296(2)
_diffrn_detector_area_resol_mean 95
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'phi- and omega-scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0440
_diffrn_reflns_av_unetI/netI     0.0286
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            2897
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        25.046
_diffrn_reflns_theta_max         25.046
_diffrn_reflns_theta_min         2.938
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.369
_exptl_absorpt_correction_T_max  0.680
_exptl_absorpt_correction_T_min  0.547
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
'HKL Denzo and Scalepack (Otwinowski & Minor 1997)'  
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.925
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.270
_exptl_crystal_size_mid          0.210
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.784
_refine_diff_density_min         -0.623
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         2897
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0244
_refine_ls_R_factor_gt           0.0234
_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)+(0.0285P)²+0.9169P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0574
_refine_ls_wR_factor_ref         0.0579
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2796
_reflns_number_total             2897
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d1cc00420d2.cif
_cod_data_source_block           Eisenberg2
_cod_depositor_comments
'Adding full bibliography for 7128478--7128480.cif.'
_cod_original_cell_volume        861.85(8)
_cod_database_code               7128479
_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.
;
_shelx_estimated_absorpt_t_min   0.567
_shelx_estimated_absorpt_t_max   0.718
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_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Ba1 Ba 0.67336(2) 0.42445(2) 0.39508(2) 0.02288(8) Uani 1 1 d . . . . .
O1 O 1.1478(4) 1.1408(3) 0.1218(2) 0.0546(7) Uani 1 1 d . . . . .
O2 O 1.0893(3) 0.9534(3) 0.20496(17) 0.0416(5) Uani 1 1 d . . . . .
O3 O 0.7071(4) 0.4440(3) 0.11336(17) 0.0396(5) Uani 1 1 d . . . . .
O4 O 0.6567(3) 0.5920(2) 0.23734(15) 0.0334(5) Uani 1 1 d . . . . .
O5 O 0.7724(3) 0.9444(2) 0.34332(15) 0.0319(4) Uani 1 1 d . . . . .
O6 O 0.6976(3) 1.1337(2) 0.42733(16) 0.0348(5) Uani 1 1 d . . . . .
O7 O 0.0852(3) 0.4900(3) 0.41223(15) 0.0322(4) Uani 1 1 d . . . . .
O8 O 0.4174(3) 0.5853(2) 0.42055(14) 0.0283(4) Uani 1 1 d . . . . .
O9 O 0.2790(4) 0.2125(3) 0.3763(2) 0.0538(7) Uani 1 1 d . . . . .
O10 O 0.5515(4) 0.2203(3) 0.21066(17) 0.0359(5) Uani 1 1 d . . . . .
O11 O 0.9005(3) 0.7582(3) 0.45986(18) 0.0436(6) Uani 1 1 d . . . . .
H11A H 0.8921 0.8065 0.4119 0.065 Uiso 1 1 d R U . . .
H11B H 1.0334 0.7805 0.4783 0.065 Uiso 1 1 d R U . . .
N1 N 0.6840(3) 0.8408(3) 0.14525(17) 0.0249(5) Uani 1 1 d . . . . .
H1 H 0.7465 0.8607 0.2140 0.030 Uiso 1 1 calc R U . . .
N2 N 0.3731(3) 0.7270(3) 0.27328(16) 0.0249(5) Uani 1 1 d . . . . .
H2 H 0.4889 0.6962 0.2887 0.030 Uiso 1 1 calc R U . . .
C1 C 1.0354(4) 1.0269(4) 0.1489(2) 0.0329(6) Uani 1 1 d . . . . .
C2 C 0.8077(4) 0.9788(4) 0.1103(2) 0.0310(6) Uani 1 1 d . . . . .
H2A H 0.7744 1.0710 0.1305 0.037 Uiso 1 1 calc R U . . .
H2B H 0.7728 0.9484 0.0404 0.037 Uiso 1 1 calc R U . . .
C3 C 0.6846(5) 0.6849(3) 0.0936(2) 0.0303(6) Uani 1 1 d . . . . .
H3A H 0.8052 0.7087 0.0693 0.036 Uiso 1 1 calc R U . . .
H3B H 0.5668 0.6341 0.0384 0.036 Uiso 1 1 calc R U . . .
C4 C 0.6810(4) 0.5642(3) 0.1543(2) 0.0268(6) Uani 1 1 d . . . . .
C5 C 0.4768(4) 0.8459(4) 0.1353(2) 0.0296(6) Uani 1 1 d . . . . .
H5A H 0.4939 0.9508 0.1721 0.036 Uiso 1 1 calc R U . . .
H5B H 0.4201 0.8369 0.0681 0.036 Uiso 1 1 calc R U . . .
C6 C 0.3249(4) 0.7180(4) 0.1672(2) 0.0293(6) Uani 1 1 d . . . . .
H6A H 0.3120 0.6131 0.1322 0.035 Uiso 1 1 calc R U . . .
H6B H 0.1934 0.7241 0.1488 0.035 Uiso 1 1 calc R U . . .
C7 C 0.4242(4) 0.8889(3) 0.3413(2) 0.0306(6) Uani 1 1 d . . . . .
H7A H 0.3779 0.8707 0.3984 0.037 Uiso 1 1 calc R U . . .
H7B H 0.3500 0.9443 0.3102 0.037 Uiso 1 1 calc R U . . .
C8 C 0.6516(4) 0.9982(3) 0.3721(2) 0.0262(6) Uani 1 1 d . . . . .
C9 C 0.1906(4) 0.6006(4) 0.2878(2) 0.0339(7) Uani 1 1 d . . . . .
H9C H 0.1416 0.5049 0.2347 0.041 Uiso 1 1 calc R U . . .
H9D H 0.0831 0.6403 0.2869 0.041 Uiso 1 1 calc R U . . .
C10 C 0.2353(4) 0.5551(3) 0.3813(2) 0.0235(5) Uani 1 1 d . . . . .
O12 O 0.9879(5) 0.3327(4) 0.0323(2) 0.0618(8) Uani 1 1 d G . . . .
H12A H 1.0351 0.2860 0.0701 0.093 Uiso 1 1 d G U . . .
H12B H 0.9099 0.3639 0.0601 0.093 Uiso 1 1 d G U . . .
H10A H 0.424(8) 0.195(6) 0.190(3) 0.067(14) Uiso 1 1 d . . . . .
H10B H 0.609(6) 0.283(5) 0.178(3) 0.052(12) Uiso 1 1 d . . . . .
H9A H 0.210(6) 0.133(5) 0.337(3) 0.044(11) Uiso 1 1 d . . . . .
H9B H 0.225(7) 0.220(5) 0.417(3) 0.055(13) Uiso 1 1 d . . . . .
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'
Ba Ba -0.3244 2.2819 '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'
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
O9 Ba1 O10 74.96(9) . . ?
O9 Ba1 O8 68.05(7) . . ?
O10 Ba1 O8 111.91(6) . . ?
O9 Ba1 O7 151.08(8) . 1_655 ?
O10 Ba1 O7 93.33(7) . 1_655 ?
O8 Ba1 O7 140.20(6) . 1_655 ?
O9 Ba1 O11 136.97(8) . . ?
O10 Ba1 O11 129.96(7) . . ?
O8 Ba1 O11 69.72(6) . . ?
O7 Ba1 O11 70.48(6) 1_655 . ?
O9 Ba1 O6 73.58(8) . 1_545 ?
O10 Ba1 O6 76.04(6) . 1_545 ?
O8 Ba1 O6 136.35(6) . 1_545 ?
O7 Ba1 O6 77.99(6) 1_655 1_545 ?
O11 Ba1 O6 139.13(6) . 1_545 ?
O9 Ba1 O7 111.06(8) . 2_666 ?
O10 Ba1 O7 146.58(6) . 2_666 ?
O8 Ba1 O7 100.34(6) . 2_666 ?
O7 Ba1 O7 65.21(7) 1_655 2_666 ?
O11 Ba1 O7 68.95(6) . 2_666 ?
O6 Ba1 O7 74.61(6) 1_545 2_666 ?
O9 Ba1 O8 67.89(8) . 2_666 ?
O10 Ba1 O8 138.36(7) . 2_666 ?
O8 Ba1 O8 70.94(6) . 2_666 ?
O7 Ba1 O8 110.22(6) 1_655 2_666 ?
O11 Ba1 O8 90.92(7) . 2_666 ?
O6 Ba1 O8 76.03(6) 1_545 2_666 ?
O7 Ba1 O8 45.74(5) 2_666 2_666 ?
O9 Ba1 O4 106.82(8) . . ?
O10 Ba1 O4 66.03(6) . . ?
O8 Ba1 O4 72.90(6) . . ?
O7 Ba1 O4 91.58(6) 1_655 . ?
O11 Ba1 O4 67.46(7) . . ?
O6 Ba1 O4 139.99(6) 1_545 . ?
O7 Ba1 O4 135.42(6) 2_666 . ?
O8 Ba1 O4 142.55(5) 2_666 . ?
O9 Ba1 C10 88.24(9) . 2_666 ?
O10 Ba1 C10 145.13(7) . 2_666 ?
O8 Ba1 C10 88.61(6) . 2_666 ?
O7 Ba1 C10 86.90(6) 1_655 2_666 ?
O11 Ba1 C10 82.82(7) . 2_666 ?
O6 Ba1 C10 69.91(6) 1_545 2_666 ?
O7 Ba1 C10 23.12(6) 2_666 2_666 ?
O8 Ba1 C10 23.32(6) 2_666 2_666 ?
O4 Ba1 C10 148.84(6) . 2_666 ?
O9 Ba1 Ba1 62.57(6) . 2_666 ?
O10 Ba1 Ba1 133.78(5) . 2_666 ?
O8 Ba1 Ba1 36.19(4) . 2_666 ?
O7 Ba1 Ba1 132.78(4) 1_655 2_666 ?
O11 Ba1 Ba1 78.53(5) . 2_666 ?
O6 Ba1 Ba1 106.60(5) 1_545 2_666 ?
O7 Ba1 Ba1 70.86(4) 2_666 2_666 ?
O8 Ba1 Ba1 34.75(4) 2_666 2_666 ?
O4 Ba1 Ba1 108.58(4) . 2_666 ?
C10 Ba1 Ba1 53.96(5) 2_666 2_666 ?
O9 Ba1 Ba1 136.86(7) . 2_766 ?
O10 Ba1 Ba1 122.31(5) . 2_766 ?
O8 Ba1 Ba1 123.99(4) . 2_766 ?
O7 Ba1 Ba1 32.98(4) 1_655 2_766 ?
O11 Ba1 Ba1 65.69(5) . 2_766 ?
O6 Ba1 Ba1 73.65(4) 1_545 2_766 ?
O7 Ba1 Ba1 32.24(4) 2_666 2_766 ?
O8 Ba1 Ba1 77.56(4) 2_666 2_766 ?
O4 Ba1 Ba1 116.31(4) . 2_766 ?
C10 Ba1 Ba1 54.33(5) 2_666 2_766 ?
Ba1 Ba1 Ba1 101.687(7) 2_666 2_766 ?
C4 O4 Ba1 132.68(18) . . ?
C8 O6 Ba1 132.68(18) . 1_565 ?
C10 O7 Ba1 145.14(18) . 1_455 ?
C10 O7 Ba1 93.08(16) . 2_666 ?
Ba1 O7 Ba1 114.79(7) 1_455 2_666 ?
C10 O8 Ba1 133.65(17) . . ?
C10 O8 Ba1 91.07(16) . 2_666 ?
Ba1 O8 Ba1 109.06(6) . 2_666 ?
C3 N1 C2 111.0(2) . . ?
C3 N1 C5 115.1(2) . . ?
C2 N1 C5 106.4(2) . . ?
C9 N2 C6 105.6(2) . . ?
C9 N2 C7 110.3(2) . . ?
C6 N2 C7 116.5(2) . . ?
O2 C1 O1 127.2(3) . . ?
O2 C1 C2 117.5(3) . . ?
O1 C1 C2 115.2(3) . . ?
N1 C2 C1 111.8(2) . . ?
N1 C3 C4 115.1(2) . . ?
O4 C4 O3 126.3(3) . . ?
O4 C4 C3 119.9(2) . . ?
O3 C4 C3 113.7(2) . . ?
C6 C5 N1 116.1(2) . . ?
C5 C6 N2 116.1(2) . . ?
N2 C7 C8 113.9(2) . . ?
O5 C8 O6 126.4(3) . . ?
O5 C8 C7 118.4(2) . . ?
O6 C8 C7 115.2(2) . . ?
N2 C9 C10 112.8(2) . . ?
O7 C10 O8 126.1(3) . . ?
O7 C10 C9 116.1(2) . . ?
O8 C10 C9 117.8(2) . . ?
O7 C10 Ba1 63.80(15) . 2_666 ?
O8 C10 Ba1 65.62(15) . 2_666 ?
C9 C10 Ba1 160.44(19) . 2_666 ?
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 O9 2.763(3) . ?
Ba1 O10 2.784(2) . ?
Ba1 O8 2.7859(19) . ?
Ba1 O7 2.7896(19) 1_655 ?
Ba1 O11 2.796(2) . ?
Ba1 O6 2.840(2) 1_545 ?
Ba1 O7 2.846(2) 2_666 ?
Ba1 O8 2.886(2) 2_666 ?
Ba1 O4 2.983(2) . ?
Ba1 C10 3.168(3) 2_666 ?
Ba1 Ba1 4.6194(3) 2_666 ?
Ba1 Ba1 4.7478(4) 2_766 ?
O1 C1 1.250(4) . ?
O2 C1 1.240(4) . ?
O3 C4 1.251(4) . ?
O4 C4 1.249(4) . ?
O5 C8 1.247(3) . ?
O6 C8 1.250(3) . ?
O6 Ba1 2.840(2) 1_565 ?
O7 C10 1.246(3) . ?
O7 Ba1 2.7896(19) 1_455 ?
O7 Ba1 2.846(2) 2_666 ?
O8 C10 1.254(3) . ?
O8 Ba1 2.886(2) 2_666 ?
N1 C3 1.496(4) . ?
N1 C2 1.497(4) . ?
N1 C5 1.504(3) . ?
N2 C9 1.494(3) . ?
N2 C6 1.504(4) . ?
N2 C7 1.513(4) . ?
C1 C2 1.521(4) . ?
C3 C4 1.526(4) . ?
C5 C6 1.502(4) . ?
C7 C8 1.530(4) . ?
C9 C10 1.507(4) . ?
C10 Ba1 3.168(3) 2_666 ?
