Seven-coordinate anion complex with a tren-based urea: Binding discrepancy of hydrogen sulfate in solid and solution states
Pramanik, Avijit; Thompson, Bethtrice; Hayes, Trina; Tucker, Kimberly; Powell, Douglas R.; Bonnesen, Peter V.; Ellis, Erick D.; Lee, Ken S.; Yu, Hongtao; Hossain, Md. Alamgir; Organic & Biomolecular Chemistry 9 (2011) 4444–; doi:10.1039/c1ob05052d

data_7151849
_publ_section_title
;
 Seven-coordinate anion complex with a tren-based urea: Binding
 discrepancy of hydrogen sulfate in solid and solution states
;
_journal_issue                   12
_journal_name_full               'Organic &amp; Biomolecular Chemistry'
_journal_page_first              4444
_journal_paper_doi               10.1039/c1ob05052d
_journal_volume                  9
_journal_year                    2011
_chemical_formula_moiety         'C30 H31 N10 O3, H O4 S'
_chemical_formula_sum            'C30 H32 N10 O7 S'
_chemical_formula_weight         676.72
_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                 103.912(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.696(2)
_cell_length_b                   12.411(2)
_cell_length_c                   20.491(4)
_cell_measurement_reflns_used    6532
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.35
_cell_measurement_theta_min      2.33
_cell_volume                     3134.1(9)
_computing_cell_refinement       'Bruker SAINT, 1998'
_computing_data_collection       'Bruker SMART, 1998'
_computing_data_reduction        'Bruker SAINT, 1998'
_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 1.000
_diffrn_measured_fraction_theta_max 0.999
_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  0.0716
_diffrn_reflns_av_sigmaI/netI    0.0865
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            29878
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.38
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    0.169
_exptl_absorpt_correction_T_max  0.9639
_exptl_absorpt_correction_T_min  0.9265
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2007)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_size_max          0.46
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.22
_refine_diff_density_max         0.303
_refine_diff_density_min         -0.419
_refine_diff_density_rms         0.066
_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     457
_refine_ls_number_reflns         7849
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.1064
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1188
_refine_ls_wR_factor_ref         0.1367
_reflns_number_gt                5058
_reflns_number_total             7849
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1ob05052d.txt
_cod_data_source_block           10054
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               7151849