Unusual Aryl-Porphyrin Rotational Barriers in Peripherally Crowded Porphyrins
Craig J. Medforth; Raid E. Haddad; Cinzia M. Muzzi; Neal R. Dooley; Laurent Jaquinod; David C. Shyr; Daniel J. Nurco; Marilyn M. Olmstead; Kevin M. Smith; Jian-Guo Ma; John A. Shelnutt; Inorganic Chemistry 42 (2003) 2227–2241; doi:10.1021/ic010958a

data_4313416
_publ_section_title
;
 Unusual Aryl-Porphyrin Rotational Barriers in Peripherally Crowded
 Porphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2227
_journal_page_last               2241
_journal_paper_doi               10.1021/ic010958a
_journal_volume                  42
_journal_year                    2003
_chemical_formula_moiety         'C52 H32 N4 Ni S2'
_chemical_formula_sum            'C52 H32 N4 Ni S2'
_chemical_formula_weight         835.68
_chemical_name_common
;
Ni(II) di-(3-thienyl)tetraphenylporphyrin
;
_chemical_name_systematic
;
Ni(II) 5,10,15,20-tetraphenyl-2,3-bis(3-thienyl)porphyrin
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.8080(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   24.2800(10)
_cell_length_b                   15.3387(6)
_cell_length_c                   10.7881(4)
_cell_measurement_reflns_used    5216
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.5
_cell_measurement_theta_min      2.3
_cell_volume                     3865.8(3)
_computing_cell_refinement       'Bruker, SAINT'
_computing_data_collection       'Bruker, SMART'
_computing_data_reduction        'Bruker, SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 0.83
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.042
_diffrn_reflns_av_sigmaI/netI    0.033
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            27265
_diffrn_reflns_theta_full        31.51
_diffrn_reflns_theta_max         31.5
_diffrn_reflns_theta_min         1.6
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_count
;
Measured at the beginning and end of the data collection.
;
_diffrn_standards_number         '50 frames'
_exptl_absorpt_coefficient_mu    0.66
_exptl_absorpt_correction_T_max  0.937
_exptl_absorpt_correction_T_min  0.744
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS 2.0 (Sheldrick, 2000)
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.434
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelepiped
_exptl_crystal_F_000             1725
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.855
_refine_diff_density_min         -1.139
_refine_diff_density_rms         0.096
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6283
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0728
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0876P)^2^+5.9187P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1453
_refine_ls_wR_factor_ref         0.1572
_reflns_number_gt                4729
_reflns_number_total             6283
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic010958a_2.cif
_cod_data_source_block           djn156v'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4313416