Interplay of Axial Ligation, Hydrogen Bonding, Self-Assembly, and Conformational Landscapes in High-Spin Ni(II) Porphyrins
Barkigia, Kathleen M.; Renner, Mark W.; Senge, Mathias O.; Fajer, Jack; The Journal of Physical Chemistry B 108 (2004) 2173–; doi:10.1021/jp036398d

data_1506813
_publ_section_title
;
 Interplay of Axial Ligation, Hydrogen Bonding, Self-Assembly, and
 Conformational Landscapes in High-Spin Ni(II) Porphyrins
;
_journal_issue                   7
_journal_name_full               'The Journal of Physical Chemistry B'
_journal_page_first              2173
_journal_paper_doi               10.1021/jp036398d
_journal_volume                  108
_journal_year                    2004
_chemical_compound_source        'methylene chloride/pentane'
_chemical_formula_structural
'C36 H40 N8 Ni O8, 2(Se N2 C6 H4), (Se N2 C6 H4)'
_chemical_formula_sum            'C54 H52 N14 Ni O8 Se3'
_chemical_formula_weight         1320.69
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 105.10(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.917(2)
_cell_length_b                   23.658(2)
_cell_length_c                   12.853(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25
_cell_measurement_theta_min      17
_cell_volume                     5553.6(9)
_computing_cell_refinement       CAD4_(Enraf-Nonius,_1977)
_computing_data_collection       CAD4_(Enraf-Nonius,_1977)
_computing_data_reduction        'XCAD4VAX provided with SHELXTL Version 5'
_computing_molecular_graphics    'SHELXTL Version 5, other in-house programs'
_computing_publication_material  'CIFTAB supplied with SHELXL-93'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \q/2\q
_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  0.0429
_diffrn_reflns_av_sigmaI/netI    0.0455
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            8627
_diffrn_reflns_theta_max         60.12
_diffrn_reflns_theta_min         2.42
_diffrn_standards_decay_%        0.46
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.313
_exptl_absorpt_correction_T_max  0.4457
_exptl_absorpt_correction_T_min  0.1854
_exptl_absorpt_correction_type   semiempirical
_exptl_absorpt_process_details
;
 The data were processed first with an analytical absorption correction   The
 semiempirical treatment (SHELXTL-Version 5 (1994)) gives slightly better 
 results with a lower residual density around Se1.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.580
_exptl_crystal_density_meas      'not applicable'
_exptl_crystal_density_method    'not applicable'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672.
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_refine_diff_density_max         3.075
_refine_diff_density_min         -1.272
_refine_diff_density_rms         0.173
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.045
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     767
_refine_ls_number_reflns         8199
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.051
_refine_ls_restrained_S_obs      1.117
_refine_ls_R_factor_all          0.1418
_refine_ls_R_factor_gt           0.1017
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2339P)^2^+5.2373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_obs         0.2822
_refine_ls_wR_factor_ref         0.3293
_reflns_number_gt                5469
_reflns_number_total             8200
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp036398dsi20030812_092352.cif
_cod_data_source_block           4
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1506813