Bis(piperazinium) Pentakis(trioxomolybdo)bis(phenylphosphonate) Dihydrate
Harrison, William T. A.; Dussack, Laurie L.; Jacobson, Allan J.; Acta Crystallographica Section C 53 (1997) 856–859; doi:10.1107/S0108270197002989

data_2006343
_publ_contact_author
;
William T. A. Harrison,
Department of Chemistry,
University of Western Australia,
Nedlands, WA  6907
Australia
;
_publ_section_title
;
 Bis(piperazinium) Pentakis(trioxomolybdo)bis(phenylphosphonate)
 Dihydrate
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              856
_journal_page_last               859
_journal_paper_doi               10.1107/S0108270197002989
_journal_volume                  53
_journal_year                    1997
_chemical_formula_iupac
'(C4 H12 N2)2 [Mo5 O15 (C6 H5 O3 P)2] , 2H2 O'
_chemical_formula_moiety         ' C20 H38 Mo5 P2 O23 N4 '
_chemical_formula_sum            'C20 H38 Mo5 N4 O23 P2'
_chemical_formula_weight         1244.20
_chemical_melting_point          'Decomposes before melting'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_method           CRYSTALS
_cell_angle_alpha                90.000
_cell_angle_beta                 95.70(3)
_cell_angle_gamma                90.000
_cell_formula_units_Z            4
_cell_length_a                   13.133(4)
_cell_length_b                   18.932(6)
_cell_length_c                   14.646(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    298
_cell_measurement_theta_max      11.6
_cell_measurement_theta_min      6.3
_cell_volume                     3623(3)
_computing_cell_refinement       'CAD-4 software'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'RC85 (Baird, 1985)'
_computing_molecular_graphics    'CAMERON (Watkin, Prout & Pearce, 1996)'
_computing_publication_material  CRYSTALS
_computing_structure_refinement
'CRYSTALS (Watkin, Prout, Carruthers & Betteridge, 1996)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1985)'
_diffrn_ambient_temperature      298
_diffrn_measurement_device       '  Enraf-Nonius CAD4 '
_diffrn_measurement_method       2\q/\w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.013
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5006
_diffrn_reflns_theta_max         22.5
_diffrn_reflns_theta_min         0.5
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.87
_exptl_absorpt_correction_T_max  0.57
_exptl_absorpt_correction_T_min  0.53
_exptl_absorpt_correction_type
;
\y scans  (North, Phillips & Matthews, 1968)
;
_exptl_crystal_colour            ' colorless '
_exptl_crystal_density_diffrn    2.27
_exptl_crystal_density_meas      ?
_exptl_crystal_description       ' faceted lump '
_exptl_crystal_F_000             2440
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.62
_refine_diff_density_min         -0.41
_refine_ls_extinction_coef       20.7(13)
_refine_ls_extinction_method     'Larson (1970)'
_refine_ls_goodness_of_fit_obs   1.84
_refine_ls_hydrogen_treatment
;
H atoms refined by riding on their appropriate N or C atoms.
H atoms associated with O31 and O32 (water molecules) not located.
;
_refine_ls_matrix_type           full
_refine_ls_number_parameters     489
_refine_ls_number_reflns         4307
_refine_ls_R_factor_all          0.022
_refine_ls_R_factor_obs          .022
_refine_ls_shift/esd_max         0.006
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
1/\s~2~(F)
;
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_all         0.035
_refine_ls_wR_factor_obs         .035
_reflns_number_observed          4307
_reflns_number_total             4621
_reflns_observed_criterion       'I > 0'
_cod_data_source_file            ta1124.cif
_cod_data_source_block           mophen
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_calc_flag' value 'CALC' changed to 'calc'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (34 times).

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from
2010-06-29.

'_atom_site_calc_flag' value 'CALC' changed to 'calc'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29 (34
times).

Automatic conversion script
Id: cif_fix_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'Not measured ' 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 
;
_cod_original_cell_volume        3623(4)
_cod_original_sg_symbol_H-M      'P 21/a'
_cod_original_formula_sum        ' C20 H38 Mo5 P2 O23 N4 '
_cod_database_code               2006343
_cod_database_fobs_code          2006343