Synthesis of Novel Organic-Inorganic Hybrid Compounds: Lanthanide Phosphites Incorporating a Squarate Ligand
Chih-Min Wang; Kwang-Hwa Lii; Inorganic Chemistry 48 (2009) 6335–6337; doi:10.1021/ic9006394

data_4302721
_publ_contact_author
;
Kwang-Hwa Lii
Department of Chemistry
National Central University
Jhongli, Taiwan 320
;
_publ_contact_author_email
;
liikh@cc.ncu.edu.tw
;
_publ_section_title
;
Synthesis of Novel Organic-Inorganic Hybrid Compounds: Lanthanide
Phosphites Incorporating a Squarate Ligand
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6335
_journal_page_last               6337
_journal_paper_doi               10.1021/ic9006394
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[Gd(H2O)(C4O4)0.5(HPO3)]'
_chemical_formula_sum            'C2 H3 Gd O6 P'
_chemical_formula_weight         311.26
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           12
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2y'
_symmetry_space_group_name_H-M   'C 1 2/m 1'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 104.70(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   15.392(3)
_cell_length_b                   10.196(2)
_cell_length_c                   8.1580(16)
_cell_measurement_temperature    293(2)
_cell_volume                     1238.4(5)
_computing_cell_refinement       'Bruker X8 Apex II'
_computing_data_collection       'Bruker X8 Apex II'
_computing_data_reduction        'Bruker X8 Apex II'
_computing_molecular_graphics    Diamond
_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  'CCD area detector'
_diffrn_measurement_method       'omega scan'
_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  0.0649
_diffrn_reflns_av_sigmaI/netI    0.0311
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            13667
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         2.42
_exptl_absorpt_coefficient_mu    10.937
_exptl_absorpt_correction_T_max  0.953
_exptl_absorpt_correction_T_min  0.705
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS program'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    3.339
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.013
_refine_diff_density_min         -1.043
_refine_diff_density_rms         0.236
_refine_ls_extinction_coef       0.00045(7)
_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   1.106
_refine_ls_matrix_type           full
_refine_ls_number_parameters     98
_refine_ls_number_reflns         1498
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_R_factor_all          0.0232
_refine_ls_R_factor_gt           0.0198
_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^)+(0.0203P)^2^+1.6928P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0461
_refine_ls_wR_factor_ref         0.0470
_reflns_number_gt                1322
_reflns_number_total             1498
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic9006394_si_001_2.cif
_cod_data_source_block           GdPO3
_cod_original_cell_volume        1238.4(4)
_cod_original_sg_symbol_H-M      'C 2/m'
_cod_database_code               4302721