Stability-inducing strain: application to the synthesis of alkyl-BIAN ligands (alkyl-BIAN = bis(alkyl)acenaphthenequinonediimine)
Ragaini, Fabio; Gasperini, Michela; Parma, Paolo; Gallo, Emma; Casati, Nicola; Macchi, Piero; New Journal of Chemistry 30 (2006) 1046–; doi:10.1039/b602257j

data_7052266
_publ_section_title
;
 Stability-inducing strain: application to the synthesis of alkyl-BIAN
 ligands (alkyl-BIAN = bis(alkyl)acenaphthenequinonediimine)
;
_journal_issue                   7
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              1046
_journal_paper_doi               10.1039/b602257j
_journal_volume                  30
_journal_year                    2006
_chemical_formula_sum            'C33 H38 Br2 Cl2 N2 Ni'
_chemical_formula_weight         752.08
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2005-07-18T16:19:44-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                103.925(2)
_cell_angle_beta                 108.377(2)
_cell_angle_gamma                108.885(2)
_cell_formula_units_Z            2
_cell_length_a                   11.3215(10)
_cell_length_b                   11.7432(11)
_cell_length_c                   13.7576(12)
_cell_measurement_temperature    150(2)
_cell_volume                     1518.0(2)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0662
_diffrn_reflns_av_unetI/netI     0.0725
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13979
_diffrn_reflns_theta_full        23.28
_diffrn_reflns_theta_max         23.28
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    3.474
_exptl_absorpt_correction_T_max  0.6449
_exptl_absorpt_correction_T_min  0.6421
_exptl_absorpt_correction_type   sphere
_exptl_absorpt_process_details
;
Interpolation using Int.Tab. Vol. C (1992) p. 523,Tab. 6.3.3.3
for values of muR in the range 0-2.5, and Int.Tab. Vol.II (1959)
p.302; Table 5.3.6 B for muR in the range 2.6-10.0.
The interpolation procedure of C.W.Dwiggins Jr (Acta Cryst.(1975)
A31,146-148) is used with some modification.
;
_exptl_crystal_density_diffrn    1.645
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             764
_refine_diff_density_max         0.725
_refine_diff_density_min         -0.932
_refine_diff_density_rms         0.122
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     361
_refine_ls_number_reflns         4360
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.022
_refine_ls_R_factor_all          0.0855
_refine_ls_R_factor_gt           0.0469
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0492P)^2^+6.6412P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.108
_refine_ls_wR_factor_ref         0.1243
_reflns_number_gt                3001
_reflns_number_total             4360
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b602257j.txt
_cod_data_source_block           fr11
_cod_database_code               7052266