Synthesis and Characterization of Transition Metal Complexes of Dimeric N-Confused Porphyrin Linked by an o-Xylene Fragment
Piotr J. Chmielewski; Inorganic Chemistry 48 (2009) 432–445; doi:10.1021/ic800591n

data_4301179
_publ_section_title
;
Synthesis and Characterization of Transition Metal Complexes of Dimeric
N-Confused Porphyrin Linked by an o-Xylene Fragment
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              432
_journal_page_last               445
_journal_paper_doi               10.1021/ic800591n
_journal_volume                  48
_journal_year                    2009
_chemical_formula_sum            'C118 H113 N8 Ni O'
_chemical_formula_weight         1717.87
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.856(13)
_cell_angle_beta                 107.447(13)
_cell_angle_gamma                98.818(15)
_cell_formula_units_Z            2
_cell_length_a                   17.007(3)
_cell_length_b                   18.130(3)
_cell_length_c                   18.797(2)
_cell_measurement_temperature    100(2)
_cell_volume                     5141.1(16)
_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, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_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  0.0456
_diffrn_reflns_av_sigmaI/netI    0.0639
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            39282
_diffrn_reflns_theta_full        60.00
_diffrn_reflns_theta_max         60.00
_diffrn_reflns_theta_min         4.15
_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.110
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1826
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.712
_refine_diff_density_min         -0.374
_refine_diff_density_rms         0.115
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.054
_refine_ls_hydrogen_treatment    refxyz
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1181
_refine_ls_number_reflns         14517
_refine_ls_number_restraints     66
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.1266
_refine_ls_R_factor_gt           0.0980
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2682
_refine_ls_wR_factor_ref         0.2845
_reflns_number_gt                9390
_reflns_number_total             14517
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic800591n-file001.cif
_cod_data_source_block           swi4dc
_cod_original_cell_volume        5141.1(15)
_cod_database_code               4301179