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_1506811
_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(C4 H6 N2), (C4 H6 N2)'
_chemical_formula_sum            'C48 H58 N14 Ni O8'
_chemical_formula_weight         1017.79
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 103.05(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.351(2)
_cell_length_b                   22.677(2)
_cell_length_c                   15.373(2)
_cell_measurement_reflns_used    77945
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.70
_cell_measurement_theta_min      3.74
_cell_volume                     4873.7(10)
_computing_cell_refinement       Scalepack/Denzo
_computing_data_collection
;
 The data collection is described by J.M. Skinner, J.W. Pflugrath, and R.M.
 Sweet in Proc. of SHARE 80 Winter 1993 Meeting, 1993.
;
_computing_data_reduction        Denzo
_computing_molecular_graphics    'SHELXTL-Version 5'
_computing_publication_material  'CIFTAB provided with SHELXS-96'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SIR92 (Altomare et al.)'
_diffrn_ambient_temperature      100(2)
_diffrn_measurement_device       'Brandeis B1 CCD detector'
_diffrn_measurement_method       rotation
_diffrn_radiation_monochromator  Si(111)
_diffrn_radiation_source         'X-rays from beamline X12C at the NSLS'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.91000
_diffrn_reflns_av_R_equivalents  0.049
_diffrn_reflns_av_sigmaI/netI    0.0422
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            8440
_diffrn_reflns_theta_max         33.70
_diffrn_reflns_theta_min         3.74
_diffrn_standards_decay_%        'not applicable'
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.467
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.387
_exptl_crystal_description       thin
_exptl_crystal_F_000             2144.
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.136
_refine_diff_density_min         -0.664
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.070
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         8438
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.072
_refine_ls_restrained_S_obs      1.102
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0578
_refine_ls_shift/esd_mean        0.000
_refine_ls_shift/su_max          0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0824P)^2^+8.3033P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1627
_refine_ls_wR_factor_ref         0.1566
_reflns_number_gt                7480
_reflns_number_total             8440
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp036398dsi20030812_092352.cif
_cod_data_source_block           2
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               1506811