Synthesis and Structures of [In4(4,4'-bipy)3(HPO4)4(H2PO4)4].4H2O and In4(4,4'-bipy)3(HPO4)4(H2PO4)4, Indium Phosphates with a Pillared Layer Structure
Kwang-Hwa Lii; Yuh-Feng Huang; Inorganic Chemistry 38 (1999) 1348–1350; doi:10.1021/ic9715106

data_4321817
_publ_section_title
;
 Synthesis and Structures of [In4(4,4'-bipy)3(HPO4)4(H2PO4)4].4H2O and
 In4(4,4'-bipy)3(HPO4)4(H2PO4)4, Indium Phosphates with a Pillared Layer
 Structure
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1348
_journal_page_last               1350
_journal_paper_doi               10.1021/ic9715106
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C30 H44 In4 N6 O36 P8'
_chemical_formula_weight         1771.75
_chemical_name_common            '[In4(4,4'-bipy)3(HPO4)4(H2PO4)4].4H2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                110.116(1)
_cell_angle_beta                 100.445(1)
_cell_angle_gamma                104.339(1)
_cell_formula_units_Z            1
_cell_length_a                   10.5429(4)
_cell_length_b                   11.6345(5)
_cell_length_c                   11.7303(5)
_cell_measurement_reflns_used    5375
_cell_measurement_temperature    296
_cell_volume                     1251.58(9)
_computing_molecular_graphics    'ATOMS, SHELXTL version 5'
_computing_structure_refinement  'SHELXTL version 5'
_computing_structure_solution    'SHELXTL version 5'
_diffrn_ambient_temperature      296
_diffrn_measurement_device       '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  0.0520
_diffrn_reflns_av_sigmaI/netI    0.0881
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            12334
_diffrn_reflns_theta_max         28.37
_diffrn_reflns_theta_min         1.93
_exptl_absorpt_coefficient_mu    2.194
_exptl_absorpt_correction_T_max  0.915
_exptl_absorpt_correction_T_min  0.761
_exptl_crystal_colour            tan
_exptl_crystal_density_diffrn    2.351
_exptl_crystal_description       tabular
_exptl_crystal_F_000             870
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.09
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.160
_refine_diff_density_min         -0.990
_refine_diff_density_rms         0.204
_refine_ls_extinction_coef       0.0024(3)
_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   1.048
_refine_ls_goodness_of_fit_obs   1.119
_refine_ls_matrix_type           full
_refine_ls_number_parameters     383
_refine_ls_number_reflns         5678
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_restrained_S_obs      1.119
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_obs          0.0517
_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^)+(0.0426P)^2^+3.6157P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1163
_refine_ls_wR_factor_obs         0.1034
_reflns_number_observed          4045
_reflns_number_total             5678
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9715106_1.cif
_cod_data_source_block           C30H44In4N6O36P8
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0426P)^2^+3.6157P] 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^)+(0.0426P)^2^+3.6157P] 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        1251.58(15)
_cod_database_code               4321817