Hydrothermal Synthesis and Characterization of New Pillared Layered Ethylenediphosphonates of Molybdenum(VI), A2[Mo2O5(O3PCH2CH2PO3)] (A = NH4, Tl, Cs, Rb) and K(H3O)[Mo2O5(O3PCH2CH2PO3)]
K. Prabhakara Rao; Vidyavathy Balraj; M. P. Minimol; K. Vidyasagar; Inorganic Chemistry 43 (2004) 4610–4614; doi:10.1021/ic035081p

data_4311315
_publ_section_title
;
 Hydrothermal Synthesis and Characterization of New Pillared Layered
 Ethylenediphosphonates of Molybdenum(VI), A2[Mo2O5(O3PCH2CH2PO3)] (A =
 NH4, Tl, Cs, Rb) and K(H3O)[Mo2O5(O3PCH2CH2PO3)]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4610
_journal_page_last               4614
_journal_paper_doi               10.1021/ic035081p
_journal_volume                  43
_journal_year                    2004
_chemical_formula_sum            'C2 H7 K Mo2 O12 P2'
_chemical_formula_weight         516.00
_chemical_name_systematic
; 
 ? 
;
_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_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   25.625(11)
_cell_length_b                   10.007(2)
_cell_length_c                   9.5119(11)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15
_cell_measurement_theta_min      10
_cell_volume                     2439.1(12)
_computing_cell_refinement       'cad 4 program'
_computing_data_collection       'cad4 program'
_computing_data_reduction        'xcad4 (wingx)'
_computing_molecular_graphics    ortep
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'cad4 diffractometer'
_diffrn_measurement_method       'omega twotheta'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0343
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            1102
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         3.06
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  '1 hour'
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    2.718
_exptl_absorpt_correction_T_max  0.9807
_exptl_absorpt_correction_T_min  0.8215
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    2.810
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       flake
_exptl_crystal_F_000             1984
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.075
_refine_diff_density_max         0.735
_refine_diff_density_min         -1.153
_refine_diff_density_rms         0.163
_refine_ls_extinction_coef       0.00112(9)
_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   1.103
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1102
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0347
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+41.8629P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0811
_refine_ls_wR_factor_ref         0.0859
_reflns_number_gt                920
_reflns_number_total             1102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035081psi20030912_063629_2.cif
_cod_data_source_block           K(H3O)[Mo2O5(O3PCH2CH2PO3)]
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'psi_scan' changed to 'psi-scan'
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:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0294P)^2^+41.8629P] 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^)+(0.0294P)^2^+41.8629P] 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        C2H7KMo2O12P2
_cod_database_code               4311315