Probing the reactivity of a 2,2′-bipyridyl-3,3′-bis-imine ligand by X-ray crystallography
Wang, Jian; Hayward, John J.; Gumbau-Brisa, Roger; Wallis, John D.; Stoeckli-Evans, Helen; Pilkington, Melanie; CrystEngComm 17 (2015) 1159–; doi:10.1039/C4CE01952K

data_7219047
_publ_section_title
;
 Probing the reactivity of a 2,2&#x2032;-bipyridyl-3,3&#x2032;-bis-imine
 ligand by X-ray crystallography
;
_journal_issue                   5
_journal_name_full               CrystEngComm
_journal_page_first              1159
_journal_paper_doi               10.1039/C4CE01952K
_journal_volume                  17
_journal_year                    2015
_chemical_formula_moiety         'C32 H16 F12 N6 O5 Zn'
_chemical_formula_sum            'C32 H16 F12 N6 O5 Zn'
_chemical_formula_weight         857.88
_chemical_name_systematic
; 
[5-(2'-Pyridinoyl)-6-(pyrid-2-yl)-5H-dipyrido[3,2-d:2',3'-f][1,3]diazepine]
complex with Zn(hfac)2
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_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_creation_method           SHELXL-97
_audit_update_record
;
2013-11-14 deposited with the CCDC.
2014-12-09 downloaded from the CCDC.
;
_cell_angle_alpha                80.759(10)
_cell_angle_beta                 80.757(10)
_cell_angle_gamma                84.987(10)
_cell_formula_units_Z            2
_cell_length_a                   9.5227(8)
_cell_length_b                   12.9131(11)
_cell_length_c                   13.7732(11)
_cell_measurement_reflns_used    7409
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.00
_cell_volume                     1646.7(2)
_computing_cell_refinement       'CELL (Stoe, 2000)'
_computing_data_collection       'EXPOSE (Stoe, 2000)'
_computing_data_reduction        'INTEGRATE (Stoe, 2000)'
_computing_molecular_graphics    'PLATON (Spek, 2003)'
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 0.81\%A
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'STOE IPDS'
_diffrn_measurement_method       'phi oscillation'
_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  0.0498
_diffrn_reflns_av_sigmaI/netI    0.0828
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            10520
_diffrn_reflns_theta_full        25.95
_diffrn_reflns_theta_max         25.95
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.867
_exptl_absorpt_correction_T_max  0.836
_exptl_absorpt_correction_T_min  0.725
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'MULscanABS in PLATON; Spek, 2003)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.730
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             856
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.708
_refine_diff_density_min         -0.849
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     505
_refine_ls_number_reflns         5992
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.0831
_refine_ls_R_factor_gt           0.0465
_refine_ls_shift/su_max          <0.001
_refine_ls_shift/su_mean         <0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0766P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1089
_refine_ls_wR_factor_ref         0.1291
_reflns_number_gt                3851
_reflns_number_total             5992
_reflns_threshold_expression     I>2sigma(I)
_cod_data_source_file            c4ce01952k2.cif
_cod_data_source_block           mel-7jw
_cod_depositor_comments
'Adding full bibliography for 7219043--7219047.cif.'
_cod_database_code               7219047