A ternary complex of aqua(18-crown-6)bis(<i>o</i>-nitrophenolato)barium(II), the triaqua(18-crown-6)(<i>o</i>-nitrophenolato)barium(II) cation and the <i>o</i>-nitrophenolate anion
Chantrapromma, Suchada; Usman, Anwar; .; Fun, Hoong-Kun; .; Acta Crystallographica Section C 58 (2002) m531–m533; doi:10.1107/S0108270102016451

data_2013007
_publ_section_title
;
 A ternary complex of
 aqua(18-crown-6)bis(<i>o</i>-nitrophenolato)barium(II), the
 triaqua(18-crown-6)(<i>o</i>-nitrophenolato)barium(II) cation and the
 <i>o</i>-nitrophenolate anion
;
_journal_issue                   11
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m531
_journal_page_last               m533
_journal_paper_doi               10.1107/S0108270102016451
_journal_volume                  58
_journal_year                    2002
_chemical_formula_iupac
;
[Ba (C12 H24 O6) (C6 H4 N O3) (H2 O)3] (C6 H4 N O3) [Ba (C12 H24 O6) (C6 H4 N
O3)2 (H2 O)]
;
_chemical_formula_moiety
'C18 H34 Ba N O12 + , C6 H4 N O3 - , C24 H34 Ba N2 O13'
_chemical_formula_sum            'C48 H72 Ba2 N4 O28'
_chemical_formula_weight         1427.78
_chemical_name_systematic
;
triaqua(1,4,7,10,13,16-hexaoxacyclooctadecane-\k^6^O)(2-nitrophenolato-
\kO)barium(II)--2-nitrophenolate--aqua(1,4,7,10,13,16-
hexaoxacyclooctadecane-\k^6^O)bis(2-nitrophenolato-\k^2^O,O')barium(II)
(1/1/1)
;
_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           SHELXL97
_cell_angle_alpha                97.9362(2)
_cell_angle_beta                 109.7546(7)
_cell_angle_gamma                108.8642(7)
_cell_formula_units_Z            2
_cell_length_a                   13.7492(3)
_cell_length_b                   14.9672(3)
_cell_length_c                   16.8669(3)
_cell_measurement_reflns_used    7466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.33
_cell_measurement_theta_min      2.52
_cell_volume                     2969.64(11)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        SAINT
_computing_molecular_graphics    SHELXTL
_computing_publication_material
'SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990)'
_computing_structure_refinement  SHELXTL
_computing_structure_solution    'SHELXTL (Sheldrick, 1997)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 8.33
_diffrn_measured_fraction_theta_full 0.915
_diffrn_measured_fraction_theta_max 0.915
_diffrn_measurement_device_type  'Siemens SMART CCD area-detector'
_diffrn_measurement_method       \w
_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  0.081
_diffrn_reflns_av_sigmaI/netI    0.147
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            17916
_diffrn_reflns_theta_full        28.26
_diffrn_reflns_theta_max         28.26
_diffrn_reflns_theta_min         2.52
_diffrn_standards_decay_%        negligible
_diffrn_standards_interval_count none
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.407
_exptl_absorpt_correction_T_max  0.766
_exptl_absorpt_correction_T_min  0.729
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   '(SADABS; Sheldrick, 1996)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.597
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1448
_exptl_crystal_size_max          0.24
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         2.47
_refine_diff_density_min         -2.90
_refine_ls_extinction_coef       0.0175(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXTL (Sheldrick, 1997)'
_refine_ls_goodness_of_fit_ref   0.964
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     692
_refine_ls_number_reflns         13455
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.075
_refine_ls_R_factor_gt           0.063
_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/[\s^2^(Fo^2^)+(0.0328P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.164
_refine_ls_wR_factor_ref         0.171
_reflns_number_gt                10337
_reflns_number_total             13455
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            av1117.cif
_cod_data_source_block           I
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        2969.60(10)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               2013007
_cod_database_fobs_code          2013007