First structurally characterised metal complex of a 2H-benzimidazole derivative. Copper mediated synthesis of 2,2-dimethyl-2H-benzimidazole from 1,2-phenylenediamine and acetone
Hati, Sanchita; Patra, Goutam K.; Naskar, Jnan P.; Drew, Michael G. B.; Datta, Dipankar; New Journal of Chemistry 25 (2001) 218–; doi:10.1039/b007410l

data_7051039
_publ_section_title
;
 First structurally characterised metal complex of a 2H-benzimidazole
 derivative. Copper mediated synthesis of 2,2-dimethyl-2H-benzimidazole
 from 1,2-phenylenediamine and acetone
;
_journal_issue                   2
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              218
_journal_paper_doi               10.1039/b007410l
_journal_volume                  25
_journal_year                    2001
_chemical_formula_sum            'C45 H40 Cl Cu N2 O4 P2'
_chemical_formula_weight         833.72
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 123.777(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   39.72(4)
_cell_length_b                   10.198(13)
_cell_length_c                   24.59(3)
_cell_measurement_reflns_used    all
_cell_measurement_temperature    293(2)
_cell_volume                     8279(17)
_computing_cell_refinement       XDS
_computing_data_collection       'XDS (Kabsch, 1991)'
_computing_data_reduction        XDS
_computing_molecular_graphics    PLATON(Spek,1994)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Marresearch Image Plate'
_diffrn_measurement_method
'95 frames at 2^o intervals, counting time 2 min.'
_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  0.0289
_diffrn_reflns_av_sigmaI/netI    0.0406
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            12812
_diffrn_reflns_theta_max         26.08
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.714
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.338
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3456
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.20
_refine_diff_density_max         1.055
_refine_diff_density_min         -0.760
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     498
_refine_ls_number_reflns         7360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0907
_refine_ls_R_factor_gt           0.0599
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+12.1347P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1591
_refine_ls_wR_factor_ref         0.1775
_reflns_number_gt                5304
_reflns_number_total             7360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b007410l.txt
_cod_data_source_block           4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0979P)^2^+12.1347P] 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^)+(0.0979P)^2^+12.1347P] 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        8280(16)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7051039