Synthesis, crystal structure and magnetic properties of a novel mixed-valence copper phosphonate: Na2Cu15(hedp)6(OH)2(H2O) (hedp = 1-hydroxyethylidenediphosphonate) ‡
Zheng, Li-Min; Duan, Chun-Ying; Ye, Xiang-Rong; Zhang, Li-Yi; Wang, Cheng; Xin, Xin-Quan; Journal of the Chemical Society, Dalton Transactions  (1998) 905–; doi:10.1039/a706601e

data_7028028
_publ_section_title
;
 Synthesis, crystal structure and magnetic properties of a novel
 mixed-valence copper phosphonate: Na2Cu15(hedp)6(OH)2(H2O)
 (hedp&#x2005;=&#x2005;1-hydroxyethylidenediphosphonate)&#x200A;&#x2021;
;
_journal_issue                   6
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              905
_journal_paper_doi               10.1039/a706601e
_journal_year                    1998
_chemical_formula_sum            'C12 H28 Cu15 Na2 O45 P12'
_chemical_formula_weight         2263.28
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -3'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   11.720(20)
_cell_length_b                   11.720(2)
_cell_length_c                   9.5309(10)
_cell_measurement_reflns_used    11
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      8.83
_cell_measurement_theta_min      4.74
_cell_volume                     1133.8(19)
_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  'Siemens SHELXTL'
_computing_structure_solution    'Siemens SHELXTL'
_diffrn_ambient_temperature      293(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  0.0476
_diffrn_reflns_av_sigmaI/netI    0.1160
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            1938
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.01
_diffrn_standards_decay_%        5.18
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    7.451
_exptl_absorpt_correction_T_max  0.8801
_exptl_absorpt_correction_T_min  0.3416
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    3.315
_exptl_crystal_description       hexagon
_exptl_crystal_F_000             1097
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.906
_refine_diff_density_min         -1.287
_refine_diff_density_rms         0.234
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.069
_refine_ls_goodness_of_fit_obs   1.288
_refine_ls_matrix_type           full
_refine_ls_number_parameters     132
_refine_ls_number_reflns         1308
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.230
_refine_ls_restrained_S_obs      1.288
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_obs          0.0565
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0550P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1659
_refine_ls_wR_factor_obs         0.1384
_reflns_number_observed          840
_reflns_number_total             1320
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            e706601sup1.cif
_cod_data_source_block           zlm2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Trigonal' changed to 'trigonal'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0400P)^2^+0.0550P] 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^)+(0.0400P)^2^+0.0550P] 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        1133.7(19)
_cod_original_sg_symbol_H-M      'P-3   '
_cod_database_code               7028028