Synthesis, crystal structure and 71Ga MAS NMR spectroscopy of a novel gallium phosphatooxalate: [Ga5(OH)2(C10H9N2)(C2O4)(PO4)4]·2H2O
Chen, Ching-Yeh; Chu, Peter P.; Lii, Kwang-Hwa; Lii, Kwang-Hwa; Chemical Communications  (1999) 1473–; doi:10.1039/a903213d

data_7115201
_publ_section_title
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 Synthesis, crystal structure and 71Ga MAS NMR spectroscopy of a novel
 gallium phosphatooxalate: [Ga5(OH)2(C10H9N2)(C2O4)(PO4)4]&#x00B7;2H2O
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_journal_issue                   16
_journal_name_full               'Chemical Communications'
_journal_page_first              1473
_journal_paper_doi               10.1039/a903213d
_journal_year                    1999
_chemical_formula_moiety         '[Ga5(OH)2(C10H9N2)(C2O4)(PO4)4].2H2O'
_chemical_formula_sum            'C12 H15 Ga5 N2 O24 P4'
_chemical_formula_weight         1043.74
_chemical_name_systematic
; 
 ? 
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_space_group_IT_number           15
_symmetry_cell_setting           1
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 90.8670(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.3430(2)
_cell_length_b                   15.9372(4)
_cell_length_c                   9.1019(2)
_cell_measurement_reflns_used    3782
_cell_measurement_temperature    293(2)
_cell_volume                     2660.51(9)
_computing_molecular_graphics    ATOMS
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.911
_diffrn_measured_fraction_theta_max 0.911
_diffrn_measurement_device_type  'Siemens Smart CCD'
_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  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0636
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            7595
_diffrn_reflns_theta_full        27.95
_diffrn_reflns_theta_max         27.95
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    5.353
_exptl_absorpt_correction_T_max  0.942
_exptl_absorpt_correction_T_min  0.826
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    2.606
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2032
_exptl_crystal_size_max          0.135
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.009
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.970
_refine_diff_density_rms         0.170
_refine_ls_extinction_coef       0.00099(11)
_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   1.072
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     240
_refine_ls_number_reflns         2902
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_R_factor_all          0.0682
_refine_ls_R_factor_gt           0.0410
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0313P)^2^+12.5437P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0806
_refine_ls_wR_factor_ref         0.0921
_reflns_number_gt                2187
_reflns_number_total             2902
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            903213d.txt
_cod_data_source_block           Ga5
_cod_depositor_comments
;
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 
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_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7115201