Systematic Evaluation of Molecular Recognition Phenomena. 3. Selective Diphosphate Binding to Isomeric Hexaazamacrocyclic Ligands Containing Xylylic Spacers
Carmen Anda; Antoni Llobet; Arthur E. Martell; Bruno Donnadieu; Teodor Parella; Inorganic Chemistry 42 (2003) 8545–8550; doi:10.1021/ic034205v

data_4312656
_publ_contact_author             'Prof Antoni Llobet'
_publ_contact_author_address
;
Departament de Quimica
Universitat de Girona
17071 Girona, Spain
;
_publ_contact_author_email       ' Antoni.llobet@udg.es '
_publ_section_title
;
 Systematic Evaluation of Molecular Recognition Phenomena. 3. Selective
 Diphosphate Binding to Isomeric Hexaazamacrocyclic Ligands Containing
 Xylylic Spacers
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              8545
_journal_page_last               8550
_journal_paper_doi               10.1021/ic034205v
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C30 H59 Br6 N6 O1.5'
_chemical_formula_weight         1007.28
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 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                 110.064(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.4653(4)
_cell_length_b                   30.519(3)
_cell_length_c                   10.7740(7)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      52.0
_cell_measurement_theta_min      2.15
_cell_volume                     2305.7(3)
_computing_cell_refinement       'Stoe IPDS software (Stoe, 1996)'
_computing_data_collection       'Stoe IPDS software (Stoe, 1996)'
_computing_data_reduction        'XRED (Stoe, 1.08, 1996)'
_computing_molecular_graphics    'ORTEP3 for Windows (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al, 1992)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.974
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       \f
_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  0.0299
_diffrn_reflns_av_sigmaI/netI    0.0230
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            13298
_diffrn_reflns_theta_full        23.26
_diffrn_reflns_theta_max         23.26
_diffrn_reflns_theta_min         2.84
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time  'every frame'
_diffrn_standards_number         200
_exptl_absorpt_coefficient_mu    5.252
_exptl_absorpt_correction_T_max  0.7693
_exptl_absorpt_correction_T_min  0.3502
_exptl_absorpt_correction_type   semi-empirical
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.448
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1002
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.879
_refine_diff_density_min         -0.566
_refine_diff_density_rms         0.096
_refine_ls_extinction_coef       0.0011(6)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         3281
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.100
_refine_ls_R_factor_all          0.0556
_refine_ls_R_factor_gt           0.0450
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+8.3341P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1175
_refine_ls_wR_factor_ref         0.1223
_reflns_number_gt                2708
_reflns_number_total             3281
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic034205vsi20030929_064743.cif
_cod_data_source_block           (H6P3)Br6
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_original_formula_sum        'C30 H59 Br6 N6 O1.50'
_cod_database_code               4312656
_computing_corr_abs              DIFABS