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_4334564
_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_moiety         'C40 H56 Cl2 In2 N4 O12 P4'
_chemical_formula_sum            'C40 H56 Cl2 In2 N4 O12 P4'
_chemical_formula_weight         1209.31
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 105.909(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.1925(18)
_cell_length_b                   10.6948(16)
_cell_length_c                   19.807(3)
_cell_measurement_reflns_used    2664
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.95
_cell_measurement_theta_min      2.18
_cell_volume                     2483.8(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 0.996
_diffrn_measured_fraction_theta_max 0.996
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0548
_diffrn_reflns_av_sigmaI/netI    0.0620
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13455
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.18
_exptl_absorpt_coefficient_mu    1.225
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.746626
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.617
_exptl_crystal_description       block
_exptl_crystal_F_000             1224
_exptl_crystal_size_max          0.14
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.179
_refine_diff_density_min         -0.804
_refine_diff_density_rms         0.233
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.145
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     300
_refine_ls_number_reflns         4861
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.145
_refine_ls_R_factor_all          0.0616
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0649P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1341
_reflns_number_gt                3804
_reflns_number_total             4861
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic3022485_si_001_1.cif
_cod_data_source_block           complex_1
_cod_database_code               4334564