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_4313415
_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_compound_source        synthetic
_chemical_formula_sum            'C78.46 H43.92 Cl7.71 N4 Ni S8'
_chemical_formula_weight         1638.8
_chemical_name_common
;
Ni(II) octa-(3-thienyl)tetraphenylporphyrin
;
_chemical_name_systematic
;
Ni(II) 5,10,15,20-tetraphenyl-2,3,7,8,12,13-17,18-octakis(3-
thienyl)porphyrin
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            24
_cell_length_a                   23.1924(15)
_cell_length_b                   23.1924(15)
_cell_length_c                   82.412(7)
_cell_measurement_reflns_used    47
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      29.7
_cell_measurement_theta_min      4.3
_cell_volume                     44328(6)
_computing_cell_refinement       'Siemens P3'
_computing_data_collection       'Siemens P3'
_computing_data_reduction        'Siemens XDISK'
_computing_molecular_graphics    'Bruker XP'
_computing_publication_material  'Bruker XCIF'
_computing_structure_refinement  'SHELXTL V. 5.03 (Sheldrick, 1994)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\q - 2\q scans'
_diffrn_radiation_monochromator  'nickel filter'
_diffrn_radiation_source         'Bruker rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.032
_diffrn_reflns_av_sigmaI/netI    0.0659
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       88
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            14433
_diffrn_reflns_theta_full        55.99
_diffrn_reflns_theta_max         55.99
_diffrn_reflns_theta_min         2.14
_diffrn_standards_decay_%        2.0
_diffrn_standards_interval_count 198
_diffrn_standards_number         2
_exptl_absorpt_coefficient_mu    5.314
_exptl_absorpt_correction_T_max  0.54
_exptl_absorpt_correction_T_min  0.24
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
XABS2, S. R. Parkin, B. Moezzi, and H. Hope, J. Appl. Crystallogr., 
1995,
28, 53.
;
_exptl_crystal_colour            'dark purple'
_exptl_crystal_density_diffrn    1.454
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             19897
_exptl_crystal_size_max          0.34
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.791
_refine_diff_density_min         -1.049
_refine_diff_density_rms         0.128
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     749
_refine_ls_number_reflns         14428
_refine_ls_number_restraints     23
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.1724
_refine_ls_R_factor_gt           0.1256
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1567P)^2^+978.0757P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3086
_refine_ls_wR_factor_ref         0.3495
_reflns_number_gt                9524
_reflns_number_total             14428
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010958a_1.cif
_cod_data_source_block           101xj
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        44328.5(54)
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4313415