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_1506810
_publ_contact_author
;
 K.M. Barkigia (regarding the crystallographic data and cif)
 Materials Science Dept.
 Bldg. 555
 Brookhaven National Laboratory
 Upton, NY 11973 USA
;
_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        '2-methyl imidazole, pentane'
_chemical_formula_structural     'C36 H40 N6 Ni O8, 2(C3 H4 N2), 1(C4 H6 N2)'
_chemical_formula_sum            'C46 H54 N14 Ni O8'
_chemical_formula_weight         989.74
_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
_cell_angle_alpha                91.87(1)
_cell_angle_beta                 96.19(1)
_cell_angle_gamma                110.94(1)
_cell_formula_units_Z            2
_cell_length_a                   13.181(2)
_cell_length_b                   13.563(1)
_cell_length_c                   14.545(2)
_cell_measurement_reflns_used    15487
_cell_measurement_temperature    145(2)
_cell_measurement_theta_max      31.07
_cell_measurement_theta_min      1.87
_cell_volume                     2407.3(6)
_computing_cell_refinement       Scalepack/Denzo
_computing_data_collection
; The software provided with the MAR345 detector was used to run the
  instrument.
;
_computing_data_reduction        Denzo
_computing_molecular_graphics    'SHELXTL-Version 5'
_computing_publication_material  'CIFTAB provided with SHELXS-86'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al.)'
_diffrn_ambient_temperature      145(2)
_diffrn_measurement_device       'MAR345 image plate detector'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'X-rays from beamline X7B at the NSLS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.9398
_diffrn_reflns_av_R_equivalents  0.043
_diffrn_reflns_av_sigmaI/netI    0.0527
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15482
_diffrn_reflns_theta_max         31.07
_diffrn_reflns_theta_min         1.87
_diffrn_standards_decay_%        'not applicable'
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.471
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.365
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1040.
_exptl_crystal_size_max          0.085
_exptl_crystal_size_mid          0.045
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.277
_refine_diff_density_min         -0.296
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.063
_refine_ls_goodness_of_fit_ref   1.105
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     612
_refine_ls_number_reflns         3781
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0498
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1323
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                3151
_reflns_number_total             3783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp036398dsi20030812_092352.cif
_cod_data_source_block           1
_cod_original_cell_volume        2407.3(5)
_cod_database_code               1506810
_refine_ls_weighting_scheme_details
'calc w=1/[\s^2^(Fo^2^)+(0.0302P)^2^+10.5695P] where P=(Fo^2^+2Fc^2^)/3'