Hydrothermal synthesis and crystal structures of two novel hybrid open-frameworks and a two-dimensional network based on tungsten(vi) oxides
Yan, Bangbo; Xu, Yan; Goh, Ngoh K.; Chia, Lian S.; Chemical Communications  (2000) 2169–; doi:10.1039/b005303l

data_7111050
_publ_contact_author
;  Bangbo Yan
  Division of Chemistry, School of Science, National Institute of Education
  Nanyang Technological University
  Singapore 259756
  Fax: 65-4698928 
  email: yanbangbo@hotmail.com
;
_publ_section_title
;
 Hydrothermal synthesis and crystal structures of two novel hybrid
 open-frameworks and a two-dimensional network based on tungsten(vi)
 oxides
;
_journal_issue                   21
_journal_name_full               'Chemical Communications'
_journal_page_first              2169
_journal_paper_doi               10.1039/b005303l
_journal_year                    2000
_chemical_formula_sum            'C2.5 H2 N0.5 O1.5 W0.5'
_chemical_formula_weight         154.97
_space_group_IT_number           64
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2ac 2'
_symmetry_space_group_name_H-M   'C m c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             'Thu Sept 7 08:57:58 2000'
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   7.4733(15)
_cell_length_b                   7.3927(15)
_cell_length_c                   22.570(4)
_cell_measurement_reflns_used    33
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.65
_cell_measurement_theta_min      3.63
_cell_volume                     1246.9(4)
_computing_cell_refinement       'Bruker XSCANS'
_computing_data_collection       'Bruker XSCANS'
_computing_data_reduction        'Bruker SHELXTL'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.973
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '2\q/\w scans'
_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  0.0913
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            2482
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         25.01
_diffrn_reflns_theta_min         3.98
_diffrn_standards_decay_%        43.98
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    18.462
_exptl_absorpt_correction_T_max  0.7906
_exptl_absorpt_correction_T_min  0.2375
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            YELLOW
_exptl_crystal_density_diffrn    3.302
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.262
_refine_diff_density_min         -1.378
_refine_diff_density_rms         0.297
_refine_ls_extinction_coef       0.00094(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     81
_refine_ls_number_reflns         581
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0445
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.361
_refine_ls_shift/su_mean         0.005
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0496P)^2^+5.5404P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0776
_refine_ls_wR_factor_ref         0.0811
_reflns_number_gt                501
_reflns_number_total             581
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005303lsup1.cif
_cod_data_source_block           2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_sg_symbol_H-M      Cmca
_cod_original_formula_sum        'C2.50 H2 N0.50 O1.50 W0.50'
_cod_database_code               7111050