A Neutral Cluster Cage with a Tetrahedral [Pd12IIL6] Framework: Crystal Structures and Host‒Guest Studies
Gupta, Arvind K.; Yadav, Ashok; Srivastava, Anant Kumar; Ramya, Kormathmadam Raghupathy; Paithankar, Harshad; Nandi, Shyamapada; Chugh, Jeetender; Boomishankar, Ramamoorthy; Inorganic chemistry  (2015) 150317143949001–; doi:10.1021/ic502798r

data_4342695
_publ_section_title
;
 A Neutral Cluster Cage with a Tetrahedral [Pd12IIL6] Framework: Crystal
 Structures and Host--Guest Studies
;
_journal_name_full               'Inorganic chemistry'
_journal_page_first              150317143949001
_journal_paper_doi               10.1021/ic502798r
_journal_year                    2015
_chemical_formula_moiety         'C48 H84 N12 O28 P4 Pd12, (C7H8), (C2H6SO)'
_chemical_formula_sum            'C57 H98 N12 O29 P4 Pd12 S'
_chemical_formula_weight         2848.21
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 108.407(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.4768(11)
_cell_length_b                   28.3891(14)
_cell_length_c                   17.6626(8)
_cell_measurement_reflns_used    5651
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.10
_cell_measurement_theta_min      2.30
_cell_volume                     10218.0(9)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.973
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0930
_diffrn_reflns_av_unetI/netI     0.0882
_diffrn_reflns_Laue_measured_fraction_full 0.951
_diffrn_reflns_Laue_measured_fraction_max 0.973
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            72749
_diffrn_reflns_point_group_measured_fraction_full 0.951
_diffrn_reflns_point_group_measured_fraction_max 0.973
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.027
_diffrn_reflns_theta_min         4.079
_exptl_absorpt_coefficient_mu    2.207
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6635
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.851
_exptl_crystal_description       prism
_exptl_crystal_F_000             5536
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_platon_squeeze_details
;
;
_refine_diff_density_max         1.925
_refine_diff_density_min         -1.064
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1003
_refine_ls_number_reflns         17570
_refine_ls_number_restraints     38
_refine_ls_restrained_S_all      0.974
_refine_ls_R_factor_all          0.0722
_refine_ls_R_factor_gt           0.0452
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0427P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0980
_refine_ls_wR_factor_ref         0.1058
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12149
_reflns_number_total             17570
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            2_Toluene.cif
_cod_data_source_block           Toluene_outside_cage
_cod_depositor_comments
;
 Updating space group information.

 Antanas Vaitkus,
 2018-06-07
;
_cod_database_code               4342695
_shelx_refln_list_code           4
_shelx_f_calc_maximum            1194.85
_shelx_f_squared_multiplier      1.000