A 3-Fold-Symmetric Ligand Based on 2-Hydroxypyridine: Regulation of Ligand Binding by Hydrogen Bonding.
Moore, Cameron M.; Quist, David A.; Kampf, Jeff W.; Szymczak, Nathaniel K.; Inorganic chemistry 53 (2014) 3278–; doi:10.1021/ic5003594

data_4337843
_publ_section_title
;
 A 3-Fold-Symmetric Ligand Based on 2-Hydroxypyridine: Regulation of
 Ligand Binding by Hydrogen Bonding.
;
_journal_issue                   7
_journal_name_full               'Inorganic chemistry'
_journal_page_first              3278
_journal_paper_doi               10.1021/ic5003594
_journal_volume                  53
_journal_year                    2014
_chemical_formula_moiety         '2(C18 H18 N4 O3), C H4 O'
_chemical_formula_sum            'C37 H40 N8 O7'
_chemical_formula_weight         708.77
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.267(6)
_cell_angle_beta                 104.955(7)
_cell_angle_gamma                101.462(7)
_cell_formula_units_Z            1
_cell_length_a                   8.8840(2)
_cell_length_b                   8.9889(2)
_cell_length_c                   11.4219(8)
_cell_measurement_temperature    85
_cell_volume                     862.15(8)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      85
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0198
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6202
_diffrn_reflns_theta_full        68.23
_diffrn_reflns_theta_max         68.23
_diffrn_reflns_theta_min         4.01
_exptl_absorpt_coefficient_mu    0.796
_exptl_absorpt_correction_T_max  0.9246
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Jacobson, R. (1998) Private communication'
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             374
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.597
_refine_diff_density_min         -0.415
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.103(4)
_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   1.181
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     255
_refine_ls_number_reflns         3101
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.181
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0699P)^2^+0.3837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1272
_refine_ls_wR_factor_ref         0.1276
_reflns_number_gt                3059
_reflns_number_total             3101
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic5003594_si_002.cif
_cod_data_source_block           p-1
_cod_depositor_comments
'Adding full bibliography for 4337842--4337844.cif.'
_cod_original_cell_volume        862.14(7)
_cod_database_code               4337843