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_1506812
_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(N2 C3 H4), 1(C H2 Cl2)'
_chemical_formula_sum            'C43 H50 Cl2 N12 Ni O8'
_chemical_formula_weight         992.56
_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                107.75(1)
_cell_angle_beta                 104.22(1)
_cell_angle_gamma                106.73(2)
_cell_formula_units_Z            2
_cell_length_a                   12.795(2)
_cell_length_b                   13.686(2)
_cell_length_c                   15.496(2)
_cell_measurement_reflns_used    22251
_cell_measurement_temperature    107(2)
_cell_measurement_theta_max      31.03
_cell_measurement_theta_min      2.36
_cell_volume                     2303.7(7)
_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 and other inhouse programs'
_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      107(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     0.93910
_diffrn_reflns_av_R_equivalents  0.046
_diffrn_reflns_av_sigmaI/netI    0.051
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            22251
_diffrn_reflns_theta_max         31.03
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        'not applicable'
_diffrn_standards_interval_count none
_diffrn_standards_interval_time  none
_diffrn_standards_number         none
_exptl_absorpt_coefficient_mu    0.603
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.431
_exptl_crystal_description       'thin plate'
_exptl_crystal_F_000             1036
_exptl_crystal_size_max          0.158
_exptl_crystal_size_mid          0.023
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.537
_refine_diff_density_min         -0.467
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.082
_refine_ls_goodness_of_fit_ref   1.137
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     315
_refine_ls_number_reflns         3054
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0881
_refine_ls_R_factor_gt           0.0716
_refine_ls_shift/esd_mean        0.001
_refine_ls_shift/su_max          0.006
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0842P)^2^+15.6538P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1997
_refine_ls_wR_factor_ref         0.1809
_reflns_number_gt                2513
_reflns_number_total             3055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jp036398dsi20030812_092352.cif
_cod_data_source_block           3
_cod_original_cell_volume        2303.7(6)
_cod_database_code               1506812