Influence of Bulky N-Substituents on the Formation of Lanthanide Triple Helical Complexes with a Ligand Derived from Bis(benzimidazole)pyridine: Structural and Thermodynamic Evidence
Gilles Muller; Jean-Claude G. Bünzli; Kurt J. Schenk; Claude Piguet; Gérard Hopfgartner; Inorganic Chemistry 40 (2001) 2642–2651; doi:10.1021/ic001289o

data_4319754
_publ_section_title
;
 Influence of Bulky N-Substituents on the Formation of Lanthanide Triple
 Helical Complexes with a Ligand Derived from Bis(benzimidazole)pyridine:
 Structural and Thermodynamic Evidence
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2642
_journal_page_last               2651
_journal_paper_doi               10.1021/ic001289o
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C29 H33 N5'
_chemical_formula_weight         451.60
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.71(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.435(3)
_cell_length_b                   11.973(2)
_cell_length_c                   16.352(3)
_cell_measurement_temperature    293(2)
_cell_volume                     2555.4(9)
_computing_cell_refinement       KM4CCD
_computing_data_collection       KM4CCD
_computing_data_reduction        KM4CCD
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0408
_diffrn_reflns_av_sigmaI/netI    0.0373
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18681
_diffrn_reflns_theta_full        20.81
_diffrn_reflns_theta_max         20.81
_diffrn_reflns_theta_min         3.08
_exptl_absorpt_coefficient_mu    0.071
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.174
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             968
_refine_diff_density_max         0.208
_refine_diff_density_min         -0.153
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -1(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     621
_refine_ls_number_reflns         5308
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.118
_refine_ls_R_factor_all          0.0752
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.2746P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0903
_refine_ls_wR_factor_ref         0.1134
_reflns_number_gt                3679
_reflns_number_total             5308
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic001289o_1.cif
_cod_data_source_block           Ligand_II
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.2746P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0565P)^2^+0.2746P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        2555.5(9)
_cod_database_code               4319754