Synthesis, Structure, and Redox Properties of N-Confused Bis(porphyrinatonickel(II)) Linked byo-Xylene
Piotr J. Chmielewski; Inorganic Chemistry 46 (2007) 1617–1626; doi:10.1021/ic061793e

data_4307266
_publ_section_title
;
Synthesis, Structure, and Redox Properties of N-Confused
Bis(porphyrinatonickel(II)) Linked byo-Xylene
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1617
_journal_page_last               1626
_journal_paper_doi               10.1021/ic061793e
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety
'C104 H78 N8 Ni2, 0.5(C6 H14), 2(C H2 Cl2), 0.5(C6)'
_chemical_formula_sum            'C112 H89 Cl4 N8 Ni2'
_chemical_formula_weight         1806.13
_chemical_name_systematic
; 
 1,2-bis(21'-(5',10',15',20'-tetratolyl-2'-aza-
21'-carbaporphyrinatonickel(II)-methyl)benzene
;
_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
_cell_angle_alpha                77.43(3)
_cell_angle_beta                 75.31(3)
_cell_angle_gamma                66.20(3)
_cell_formula_units_Z            2
_cell_length_a                   16.455(3)
_cell_length_b                   16.776(3)
_cell_length_c                   18.400(4)
_cell_measurement_temperature    100(2)
_cell_volume                     4457.1(19)
_computing_cell_refinement
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_data_collection
'CrysAlis CCD (Oxford Diffraction, 1995-2003)'
_computing_data_reduction
'CrysAlis RED (Oxford Diffraction, 1995-2003)'
_computing_molecular_graphics    'XP (Bruker, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.927
_diffrn_measured_fraction_theta_max 0.927
_diffrn_measurement_device_type  'Xcalibur PX \k-geometry diffractometer'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0812
_diffrn_reflns_av_sigmaI/netI    0.1236
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            24566
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         3.54
_exptl_absorpt_coefficient_mu    2.064
_exptl_absorpt_correction_T_max  0.85601
_exptl_absorpt_correction_T_min  0.81744
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   'CrysAlis, Oxford Diffraction'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.346
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1882
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.756
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.011
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1111
_refine_ls_number_reflns         12274
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.012
_refine_ls_R_factor_all          0.1378
_refine_ls_R_factor_gt           0.0903
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1514P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2308
_refine_ls_wR_factor_ref         0.2732
_reflns_number_gt                6502
_reflns_number_total             12274
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061793esi20060921_063209.cif
_cod_data_source_block           chm2abs
_cod_original_cell_volume        4457.1(18)
_cod_database_code               4307266