Synthesis and metalation of a chiral, pyridine-strapped, cyclic bis(benzimidazole) ligand.
Fekner, Tomasz; Gallucci, Judith; Chan, Michael K.; Organic letters 6 (2004) 989–992; doi:10.1021/ol049954a

data_1507130
_publ_section_title
;
 Synthesis and metalation of a chiral, pyridine-strapped, cyclic
 bis(benzimidazole) ligand.
;
_journal_issue                   6
_journal_name_full               'Organic letters'
_journal_page_first              989
_journal_page_last               992
_journal_paper_doi               10.1021/ol049954a
_journal_volume                  6
_journal_year                    2004
_chemical_formula_sum            'C39 H39 B2 Cu F8 N7 O2'
_chemical_formula_weight         874.93
_chemical_name_systematic
;
?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-93
_cell_angle_alpha                90.00
_cell_angle_beta                 106.12(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.595(1)
_cell_length_b                   16.922(2)
_cell_length_c                   19.919(3)
_cell_measurement_temperature    150(2)
_cell_volume                     3754.7(8)
_computing_cell_refinement       'DENZO (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1999)'
_computing_data_reduction        'DENZO (Otwinowski & Minor, 1997)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_measurement_device       'Nonius Kappa CCD'
_diffrn_measurement_method       'phi and omega 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  0.038
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            55721
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.13
_exptl_absorpt_coefficient_mu    0.669
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       'rectangular plate'
_exptl_crystal_F_000             1796
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.021
_refine_diff_density_min         -0.732
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.026
_refine_ls_goodness_of_fit_obs   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     538
_refine_ls_number_reflns         6608
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.045
_refine_ls_restrained_S_obs      1.067
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_obs          0.0515
_refine_ls_shift/esd_max         -0.092
_refine_ls_shift/esd_mean        0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+9.5759P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1367
_refine_ls_wR_factor_obs         0.1252
_reflns_number_observed          5432
_reflns_number_total             6608
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ol049954asi20040107_031436.cif
_cod_data_source_block           compound_12
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+9.5759P] 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^)+(0.0594P)^2^+9.5759P] 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        3754.7(7)
_cod_original_sg_symbol_H-M      'P 2(1)/c'
_cod_database_code               1507130