Hydrothermal assembly and crystal structures of three novel open frameworks based on molybdenum(vi) oxides
Xu, Yan; Lu, Jianjiang; Goh, Ngoh K.; Journal of Materials Chemistry 9 (1999) 1599–; doi:10.1039/a901592b

data_7213043
_publ_section_title
;
 Hydrothermal assembly and crystal structures of three novel open
 frameworks based on molybdenum(vi) oxides
;
_journal_issue                   7
_journal_name_full               'Journal of Materials Chemistry'
_journal_page_first              1599
_journal_paper_doi               10.1039/a901592b
_journal_volume                  9
_journal_year                    1999
_chemical_formula_sum            'C H Mo0.5 N0.5 O1.5'
_chemical_formula_weight         91.99
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           23
_symmetry_space_group_name_Hall  'I 2 2'
_symmetry_space_group_name_H-M   'I 2 2 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   5.2702(15)
_cell_length_b                   5.2674(7)
_cell_length_c                   14.2310(11)
_cell_measurement_reflns_used    18
_cell_measurement_temperature    297(2)
_cell_measurement_theta_max      12.67
_cell_measurement_theta_min      5.47
_cell_volume                     395.06(13)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      297(2)
_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  0.0159
_diffrn_reflns_av_sigmaI/netI    0.0253
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       6
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            438
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.86
_diffrn_standards_decay_%        4.36
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.181
_exptl_absorpt_correction_T_max  0.9911
_exptl_absorpt_correction_T_min  0.8009
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            LIGHT-COLOURED
_exptl_crystal_density_diffrn    3.093
_exptl_crystal_description       PLATE
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.406
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.100
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.06(16)
_refine_ls_extinction_coef       0.0301(15)
_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_all   1.194
_refine_ls_goodness_of_fit_obs   1.201
_refine_ls_matrix_type           full
_refine_ls_number_parameters     35
_refine_ls_number_reflns         374
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_restrained_S_obs      1.201
_refine_ls_R_factor_all          0.0179
_refine_ls_R_factor_obs          0.0169
_refine_ls_shift/esd_max         0.157
_refine_ls_shift/esd_mean        0.025
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.2956P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0433
_refine_ls_wR_factor_obs         0.0414
_reflns_number_observed          361
_reflns_number_total             375
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            901592bsup1.cif
_cod_data_source_block           1
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0154P)^2^+0.2956P] where P=(Fo^2^+2Fc^2^)/3' 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^(Fo^2^)+(0.0154P)^2^+0.2956P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C H Mo0.50 N0.50 O1.50'
_cod_database_code               7213043