Hydrothermal assembly and structural characterisation of one- and two-dimensional organic/inorganic hybrid materials constructed from diphosphopentamolybdate(VI) clusters and {Cu(en)}2+ complex groups
Lu, Jianjiang; Xu, Yan; Goh, Ngoh K.; Chia, Lian S.; Chemical Communications  (1998) 2733–; doi:10.1039/a807617k

data_7110378
_publ_section_title
;
 Hydrothermal assembly and structural characterisation of one- and
 two-dimensional organic/inorganic hybrid materials constructed from
 diphosphopentamolybdate(VI) clusters and {Cu(en)}2+ complex groups
;
_journal_issue                   24
_journal_name_full               'Chemical Communications'
_journal_page_first              2733
_journal_paper_doi               10.1039/a807617k
_journal_year                    1998
_chemical_formula_sum            'C4 H20 Cu Mo2.5 N4 O13 P'
_chemical_formula_weight         666.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           73
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_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            16
_cell_length_a                   11.478(4)
_cell_length_b                   39.171(8)
_cell_length_c                   15.226(6)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      12.54
_cell_measurement_theta_min      4.93
_cell_volume                     6846(4)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296(2)
_diffrn_measurement_device       'Siemens 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  0.0310
_diffrn_reflns_av_sigmaI/netI    0.0298
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -46
_diffrn_reflns_limit_l_max       1
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            6556
_diffrn_reflns_theta_max         25.10
_diffrn_reflns_theta_min         2.08
_diffrn_standards_decay_%        3.43
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.190
_exptl_absorpt_correction_T_max  0.9874
_exptl_absorpt_correction_T_min  0.4740
_exptl_absorpt_correction_type   'Semi-empirical from psi-scan'
_exptl_crystal_colour            'DARK_BLUE         '
_exptl_crystal_density_diffrn    2.587
_exptl_crystal_F_000             5200
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.451
_refine_diff_density_min         -0.523
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.00053(2)
_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   1.109
_refine_ls_goodness_of_fit_obs   1.123
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3006
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.252
_refine_ls_restrained_S_obs      1.123
_refine_ls_R_factor_all          0.0288
_refine_ls_R_factor_obs          0.0246
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+18.9322P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0694
_refine_ls_wR_factor_obs         0.0603
_reflns_number_observed          2813
_reflns_number_total             3035
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            807617ksup1.cif
_cod_data_source_block           3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0248P)^2^+18.9322P] 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^)+(0.0248P)^2^+18.9322P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        6845.4(38)
_cod_original_formula_sum        'C4 H20 Cu Mo2.50 N4 O13 P'
_cod_database_code               7110378