Synthesis and reactivity of tetrakis(imino)pyracene (TIP) ligands; bifunctional analogues of the BIAN ligand class.
Vasudevan, Kalyan V; Findlater, Michael; Cowley, Alan H; Chemical communications (Cambridge, England)  (2008) 1918–1919; doi:10.1039/b719251g

data_7103078
_publ_section_title
;
 Synthesis and reactivity of tetrakis(imino)pyracene (TIP) ligands;
 bifunctional analogues of the BIAN ligand class.
;
_journal_issue                   16
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              1918
_journal_page_last               1919
_journal_paper_doi               10.1039/b719251g
_journal_year                    2008
_chemical_formula_moiety         'C31 H36 Br Cu N2, C4 H8 O'
_chemical_formula_sum            'C35 H44 Br Cu N2 O'
_chemical_formula_weight         652.17
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
manual editing of the .cif file
created by SHELXTL Ver. 6.10
;
_cell_angle_alpha                90.00
_cell_angle_beta                 106.77(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.719(3)
_cell_length_b                   13.400(3)
_cell_length_c                   19.628(4)
_cell_measurement_temperature    153(2)
_cell_volume                     3454.9(12)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;
SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C.,
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scan
_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  0.0683
_diffrn_reflns_av_sigmaI/netI    0.0928
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            22151
_diffrn_reflns_theta_full        27.41
_diffrn_reflns_theta_max         27.41
_diffrn_reflns_theta_min         1.87
_exptl_absorpt_coefficient_mu    1.816
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            Black-Green
_exptl_crystal_density_diffrn    1.254
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          .15
_exptl_crystal_size_mid          .10
_exptl_crystal_size_min          .10
_refine_diff_density_max         3.207
_refine_diff_density_min         -0.736
_refine_diff_density_rms         0.279
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     369
_refine_ls_number_reflns         7850
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.1318
_refine_ls_R_factor_gt           0.0678
_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^)+(0.1349P)^2^+3.2961P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2037
_refine_ls_wR_factor_ref         0.2403
_reflns_number_gt                4596
_reflns_number_total             7850
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b719251g.txt
_cod_data_source_block           ccdkvkv059a
_cod_original_sg_symbol_Hall     -p2ybc
_cod_original_sg_symbol_H-M      p21/c
_cod_database_code               7103078