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_4025259
_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
'C73 H85 Br1.84 Cl2.16 N13 Pd4 Zn, 3(C7 H8), 2(C H CL3)'
_chemical_formula_sum            'C96 H111 Br1.84 Cl8.16 N13 Pd4 Zn'
_chemical_formula_weight         2374.25
_chemical_name_systematic
; 
 ? 
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                111.226(3)
_cell_angle_beta                 95.283(3)
_cell_angle_gamma                101.042(3)
_cell_formula_units_Z            2
_cell_length_a                   15.126(3)
_cell_length_b                   19.255(4)
_cell_length_c                   20.943(5)
_cell_measurement_temperature    150(2)
_cell_volume                     5493(2)
_computing_cell_refinement       EvalCCD-Postref
_computing_data_collection       'Nonius COLLECT'
_computing_data_reduction        'EvalCCD, Sadabs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'DIRDIF-99 (Beurskens et al., 1999)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0329
_diffrn_reflns_av_sigmaI/netI    0.0341
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            125122
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    1.772
_exptl_absorpt_correction_T_max  0.73
_exptl_absorpt_correction_T_min  0.61
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2390
_exptl_crystal_size_max          0.39
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.545
_refine_diff_density_min         -1.416
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.141
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1129
_refine_ls_number_reflns         25199
_refine_ls_number_restraints     175
_refine_ls_restrained_S_all      1.223
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0408
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0669P)^2^+2.7741P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1150
_refine_ls_wR_factor_ref         0.1230
_reflns_number_gt                18881
_reflns_number_total             25199
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            jo902402g_si_002_1.cif
_cod_data_source_block           s2960a
_cod_database_code               4025259