Spectroscopic, Structural, and Theoretical Studies of Halide Complexes with a Urea-Based Tripodal Receptor
Avijit Pramanik; Douglas R. Powell; Bryan M. Wong; Md. Alamgir Hossain; Inorganic Chemistry 51 (2012) 4274–4284; doi:10.1021/ic202747q

data_4328829
_publ_section_title
;
 Spectroscopic, Structural, and Theoretical Studies of Halide Complexes
 with a Urea-Based Tripodal Receptor
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4274
_journal_page_last               4284
_journal_paper_doi               10.1021/ic202747q
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '2(C30 H31 N10 O3), Si F6, 6.35(H2 O)'
_chemical_formula_sum            'C60 H74.7 F6 N20 O12.35 Si'
_chemical_formula_weight         1415.79
_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                 96.061(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   15.4907(14)
_cell_length_b                   11.5343(11)
_cell_length_c                   19.4685(17)
_cell_measurement_reflns_used    8580
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.85
_cell_measurement_theta_min      2.21
_cell_volume                     3459.1(5)
_computing_cell_refinement       'Bruker SAINT, 2007'
_computing_data_collection       'Bruker SMART, 2007'
_computing_data_reduction        'Bruker SAINT, 2007'
_computing_molecular_graphics    'SHELXTL (Sheldrick, 2008)'
_computing_publication_material  'SHELXTL (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXTL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXTL (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'CCD Bruker APEX'
_diffrn_measurement_method       '\f and \w 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  0.0650
_diffrn_reflns_av_sigmaI/netI    0.0668
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            35178
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.32
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.124
_exptl_absorpt_correction_T_max  0.9780
_exptl_absorpt_correction_T_min  0.9531
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2001)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.359
_exptl_crystal_description       prism
_exptl_crystal_F_000             1483
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.370
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.003
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     480
_refine_ls_number_reflns         8552
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0954
_refine_ls_R_factor_gt           0.0600
_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^)+(0.0700P)^2^+1.8000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1408
_refine_ls_wR_factor_ref         0.1581
_reflns_number_gt                5882
_reflns_number_total             8552
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            ic202747q_si_005.cif
_cod_data_source_block           10073
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C60 H74.70 F6 N20 O12.35 Si'
_cod_database_code               4328829