Vanadium, Molybdenum, and Sodium Triethanolamine Complexes Derived from an Assembly System Containing Tetrathiometalate and Triethanolamine
Yihui Chen; Qiutian Liu; Yuheng Deng; Hongping Zhu; Changneng Chen; Hongjun Fan; Daizheng Liao; Enqing Gao; Inorganic Chemistry 40 (2001) 3725–3733; doi:10.1021/ic010126c

data_4319983
_publ_section_references
;
 1.Enraf-Nonius (1977). CAD4 Operations Manual. Enraf-Nonius, Delft, The
   Netherlands.
 2.Cromer,D.T. & Waber,J.T.(1974). International Tables for X-ray
   Crystallography, Vol.IV, Tables 2.2A,2.3.1. Birmingham:Kynoch Press.
   (Present distributor Kluwer Academic Publisher, Dordrecht.)
 3.Fair,C.K.(1990). MolEN. An Interactive Intelligent System for Crystal
   Structure Analysis. Enraf-Nonius, Delft,The Netherland.
 4.North,A.C.T. & Phillips,D.C.(1968). Acta Cryst., A24, 351-359.
;
_publ_section_title
;
 Vanadium, Molybdenum, and Sodium Triethanolamine Complexes Derived from
 an Assembly System Containing Tetrathiometalate and Triethanolamine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3725
_journal_page_last               3733
_journal_paper_doi               10.1021/ic010126c
_journal_volume                  40
_journal_year                    2001
_chemical_formula_moiety         '[NaV6O6{N(CH2CH2O)2(CH2CH2OH)}6]2.S6.2CH3OH'
_chemical_formula_sum            'C37 H82 N6 Na O25 S3 V6'
_chemical_formula_weight         1435.92
_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_type_scat_source
'International Tables for X-Ray Crystallography Vol.IV '
_audit_creation_method           from_GCIF_by_our_laboratory
_cell_angle_alpha                73.94(2)
_cell_angle_beta                 80.29(2)
_cell_angle_gamma                72.75(2)
_cell_formula_units_Z            2
_cell_length_a                   14.374(3)
_cell_length_b                   14.486(3)
_cell_length_c                   15.152(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293
_cell_measurement_theta_max      15
_cell_measurement_theta_min      14
_cell_volume                     2882.5(11)
_computing_cell_refinement       'CAD4 (Enraf-Nonius)'
_computing_data_collection       'CAD4 (Enraf-Nonius)'
_computing_data_reduction        'Lorentz-Polarization (MolEN)'
_computing_molecular_graphics    'ORTEP (1989)'
_computing_publication_material  GCIF_by_Our_laboratory
_computing_structure_refinement  'Full Matrix Least Squares-LSFM (MolEN)'
_computing_structure_solution    'Direct Method (MolEN)'
_diffrn_measurement_device       'Enraf Nonius CAD4'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.024
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11303
_diffrn_reflns_theta_max         26.0
_diffrn_standards_decay_%        5.8
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.09
_exptl_absorpt_correction_T_max  0.999
_exptl_absorpt_correction_T_min  0.839
_exptl_absorpt_correction_type   Empirical_\y
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.62
_exptl_crystal_density_meas      ?
_exptl_crystal_description       prism
_exptl_crystal_size_max          0.55
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         1.42
_refine_diff_density_min         -0.09
_refine_ls_goodness_of_fit_obs   1.57
_refine_ls_hydrogen_treatment
;
H atoms were added in geom for C=20
atoms except for O atoms that ought to be located, but not refined
;
_refine_ls_number_parameters     760
_refine_ls_number_reflns         8194
_refine_ls_R_factor_obs          .0487
_refine_ls_shift/esd_max         0.0094
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     w=1/(\s^2^(F))
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         .0691
_reflns_number_observed          8194
_reflns_number_total             11303
_reflns_observed_criterion       refl_observed_if_I_>3.0_sigma(I)
_cod_data_source_file            ic010126c_1.cif
_cod_data_source_block           gcif.out
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from
2010-06-29.

'_geom_angle_publ_flag' value 'Yes' changed to 'yes'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (419
times).

'_geom_bond_publ_flag' value 'Yes' changed to 'yes'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29 (123 times).

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'No' 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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'w=1/(\s^2^(F))' was changed to
'calc'. New tag '_refine_ls_weighting_details' was created. The value
of the new tag was set to 'w=1/(\s^2^(F))'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 

2024-02-02
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_weight         2871.85
_cod_original_formula_units_Z            1
_cod_original_cell_volume        2882.4(1)
_cod_original_formula_sum        'V12 S6 Na2 O50 N12 C74 H164'
_cod_database_code               4319983
_f(000)                          1486