Molecular Indium(III) Phosphonates Possessing Ring and Cage Structures. Synthesis and Structural Characterization of [In2(t-BuPO3H)4(phen)2Cl2] and [In3(C5H9PO3)2(C5H9PO3H)4(phen)3].NO3.3.5H2O
Vadapalli Chandrasekhar; Joydeb Goura; Andrew Duthie; Inorganic Chemistry 52 (2013) 4819–4824; doi:10.1021/ic3022485

data_4334565
_publ_section_title
;
 Molecular Indium(III) Phosphonates Possessing Ring and Cage Structures.
 Synthesis and Structural Characterization of [In2(t-BuPO3H)4(phen)2Cl2]
 and [In3(C5H9PO3)2(C5H9PO3H)4(phen)3].NO3.3.5H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4819
_journal_page_last               4824
_journal_paper_doi               10.1021/ic3022485
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C66 H89 In3 N7 O24.5 P6'
_chemical_formula_weight         1902.73
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                90.000(5)
_cell_angle_beta                 94.303(5)
_cell_angle_gamma                90.000(5)
_cell_formula_units_Z            8
_cell_length_a                   17.854(5)
_cell_length_b                   40.106(5)
_cell_length_c                   21.363(5)
_cell_measurement_reflns_used    3835
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      17.77
_cell_measurement_theta_min      2.24
_cell_volume                     15254(6)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.1176
_diffrn_reflns_av_sigmaI/netI    0.1473
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            83100
_diffrn_reflns_theta_full        25.50
_diffrn_reflns_theta_max         25.50
_diffrn_reflns_theta_min         1.90
_exptl_absorpt_coefficient_mu    1.106
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.447321
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.657
_exptl_crystal_description       block
_exptl_crystal_F_000             7736
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         1.528
_refine_diff_density_min         -0.780
_refine_diff_density_rms         0.152
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1806
_refine_ls_number_reflns         28355
_refine_ls_number_restraints     14
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1735
_refine_ls_R_factor_gt           0.0880
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1103P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1993
_refine_ls_wR_factor_ref         0.2520
_reflns_number_gt                13996
_reflns_number_total             28355
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3022485_si_001_2.cif
_cod_data_source_block           complex_2
_cod_database_code               4334565