Crystal structure of poly[di-µ2-aqua-aqua-nitrato-κ2 O,O′-(µ3-2-nitroisophthalato-κ4 O,O′:O″:O′″)barium(II)natrium(II)] monohydrate, C8H11BaN2NaO13
Huang, Guang; Xing, Yalong; Zeitschrift für Kristallographie - New Crystal Structures 238 (2023) 207–209; doi:10.1515/ncrs-2022-0545

data_8107396
_publ_section_title
;
 Crystal structure of poly[di-&#x00B5;2-aqua-aqua-nitrato-\k2
 O,O&#x2032;-(&#x00B5;3-2-nitroisophthalato-\k4
 O,O&#x2032;:O&#x2033;:O&#x2032;&#x2033;)barium(II)natrium(II)]
 monohydrate, C8H11BaN2NaO13
;
_journal_issue                   2
_journal_name_full
'Zeitschrift f\"ur Kristallographie - New Crystal Structures'
_journal_page_first              207
_journal_page_last               209
_journal_paper_doi               10.1515/ncrs-2022-0545
_journal_volume                  238
_journal_year                    2023
_chemical_formula_moiety         'C8 H9 Ba N2 Na O12, H2 O'
_chemical_formula_sum            'C8 H11 Ba N2 Na O13'
_chemical_formula_weight         503.52
_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
_atom_sites_solution_primary     dual
_cell_angle_alpha                106.813(7)
_cell_angle_beta                 98.508(6)
_cell_angle_gamma                107.024(7)
_cell_formula_units_Z            2
_cell_length_a                   7.4892(6)
_cell_length_b                   9.9140(9)
_cell_length_c                   11.3274(7)
_cell_measurement_reflns_used    3432
_cell_measurement_temperature    292.6(6)
_cell_measurement_theta_max      29.1150
_cell_measurement_theta_min      2.9500
_cell_volume                     744.53(12)
_computing_cell_refinement
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_data_collection
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_data_reduction
'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015) [1]'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009) [2]'
_computing_structure_refinement  'SHELXL 2019/2 (Sheldrick, 2015) [3]'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018) [4]'
_diffrn_ambient_environment      air
_diffrn_ambient_temperature      292.6(6)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2684
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
--------------------------------------------------------------------------
  1  \w    -58.00  33.00   1.00    1.00    --   11.90 -57.00-150.00   91
  2  \w    -13.00  74.00   1.00    1.00    --   11.90  77.00 120.00   87
  3  \w    -16.00  82.00   1.00    1.00    --   11.90  57.00   0.00   98
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0781150000
_diffrn_orient_matrix_UB_12      -0.0045824000
_diffrn_orient_matrix_UB_13      -0.0275536000
_diffrn_orient_matrix_UB_21      0.0104411000
_diffrn_orient_matrix_UB_22      0.0697884000
_diffrn_orient_matrix_UB_23      -0.0084908000
_diffrn_orient_matrix_UB_31      0.0654028000
_diffrn_orient_matrix_UB_32      0.0386959000
_diffrn_orient_matrix_UB_33      0.0611817000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0413
_diffrn_reflns_av_unetI/netI     0.0650
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            5469
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.997
_diffrn_reflns_theta_min         2.295
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    2.774
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.03921
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    2.246
_exptl_crystal_description       block
_exptl_crystal_F_000             488
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.770
_refine_diff_density_min         -1.112
_refine_diff_density_rms         0.154
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     248
_refine_ls_number_reflns         3208
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0199P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0615
_refine_ls_wR_factor_ref         0.0663
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2905
_reflns_number_total             3208
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            suppl_j_ncrs-2022-0545_suppl.cif
_cod_data_source_block           e06
_cod_original_cell_volume        744.53(11)
_cod_database_code               8107396
_shelx_estimated_absorpt_t_max   0.732
_shelx_estimated_absorpt_t_min   0.532
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 O1W-H1WB
 0.85 with sigma of 0.02
 Ba1-H2WA \\sim Ba1-H2WB
 with sigma of 0.02
3.a Free rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB)
3.b Aromatic/amide H refined with riding coordinates:
 C3(H3), C5(H5), C4(H4)
;
_shelx_res_checksum              28148
_shelx_hkl_checksum              46565
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 21.208
_oxdiff_exptl_absorpt_empirical_full_min 0.508