Synthesis of and Evidence for Electronic Communication within Heteromultimetallic Tetrakis(NCN-pincer metal)-(Metallo)porphyrin Hybrids
Bart M. J. M. Suijkerbuijk; Duncan M. Tooke; Martin Lutz; Anthony L. Spek; Leonardus W. Jenneskens; Gerard van Koten; Robertus J. M. Klein Gebbink; Journal of Organic Chemistry 75 (2010) 1534–1549; doi:10.1021/jo902402g

data_4025260
_publ_contact_author_address
; Bijvoet Center for Biomolecular Research
  Crystal and Structural Chemistry
  Utrecht University
  Padualaan 8
  3584 CH Utrecht
  The Netherlands
;
_publ_contact_author_email       m.lutz@uu.nl
_publ_contact_author_fax         '[+31] 30 2533940'
_publ_contact_author_name        'Martin Lutz'
_publ_contact_author_phone       '[+31] 30 2533902'
_publ_section_title
;
 Synthesis of and Evidence for Electronic Communication within
 Heteromultimetallic Tetrakis(NCN-pincer metal)-(Metallo)porphyrin Hybrids
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              1534
_journal_page_last               1549
_journal_paper_doi               10.1021/jo902402g
_journal_volume                  75
_journal_year                    2010
_chemical_formula_moiety         'C68 H80 Br4 N12 Ni'
_chemical_formula_sum            'C68 H80 Br4 N12 Ni'
_chemical_formula_weight         1443.79
_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                 126.1130(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.4380(10)
_cell_length_b                   9.8494(10)
_cell_length_c                   29.2457(10)
_cell_measurement_reflns_used    28
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      13.749
_cell_measurement_theta_min      4.444
_cell_volume                     8246.6(9)
_computing_cell_refinement       DIRAX
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        'EvalCCD and SADABS'
_computing_molecular_graphics    PLATON
_computing_publication_material  PLATON
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1217
_diffrn_reflns_av_sigmaI/netI    0.0656
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            77763
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.72
_exptl_absorpt_coefficient_mu    2.214
_exptl_absorpt_correction_T_max  0.96
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red-orange
_exptl_crystal_density_diffrn    1.163
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2960
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.984
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     393
_refine_ls_number_reflns         5378
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1117
_refine_ls_R_factor_gt           0.0647
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+32.1646P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1303
_refine_ls_wR_factor_ref         0.1463
_reflns_number_gt                3835
_reflns_number_total             5378
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo902402g_si_002_2.cif
_cod_data_source_block           s3073a
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4025260