Metalloporphines: Dimers and Trimers.
Jentzen, Walter; Shelnutt, John A.; Scheidt, W. Robert; Inorganic chemistry 55 (2016) 6294–6299; doi:10.1021/acs.inorgchem.6b00956

data_4348101
_publ_section_title
;
 Metalloporphines: Dimers and Trimers.
;
_journal_issue                   12
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6294
_journal_page_last               6299
_journal_paper_doi               10.1021/acs.inorgchem.6b00956
_journal_volume                  55
_journal_year                    2016
_chemical_formula_moiety         'C20 H12 N4 Zn'
_chemical_formula_sum            'C20 H12 N4 Zn'
_chemical_formula_weight         373.71
_chemical_name_common            zinc(II)porphine
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                99.853(9)
_cell_angle_beta                 93.007(4)
_cell_angle_gamma                97.742(5)
_cell_formula_units_Z            5
_cell_length_a                   10.0359(10)
_cell_length_b                   12.5467(8)
_cell_length_c                   14.8377(7)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    130(2)
_cell_measurement_theta_max      20.48
_cell_measurement_theta_min      2.36
_cell_volume                     1818.5(2)
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      130(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.884
_diffrn_measurement_device_type  'Enraf-Nonius FAST area-detector'
_diffrn_measurement_method       'ellipsoid-mask fitting'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0543
_diffrn_reflns_av_unetI/netI     0.0477
_diffrn_reflns_Laue_measured_fraction_full 0.986
_diffrn_reflns_Laue_measured_fraction_max 0.884
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            17939
_diffrn_reflns_point_group_measured_fraction_full 0.986
_diffrn_reflns_point_group_measured_fraction_max 0.884
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.802
_diffrn_reflns_theta_min         2.359
_diffrn_source                   'rotating anode'
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8759
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details   DIfABS
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       plate-like
_exptl_crystal_F_000             950
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.486
_refine_diff_density_min         -0.729
_refine_diff_density_rms         0.105
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     565
_refine_ls_number_reflns         9195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0516
_refine_ls_R_factor_gt           0.0383
_refine_ls_shift/su_max          0.010
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0467P)^2^+1.5375P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0908
_refine_ls_wR_factor_ref         0.0967
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7648
_reflns_number_total             9195
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b00956_si_002.cif
_cod_data_source_block           ZnP-1
_cod_database_code               4348101
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.728
_shelx_estimated_absorpt_t_max   0.849
_exptl_absorpt_special_details
; Diffraction data were measured with an Enraf-Nonius FAST area detector to 59.6  
 deg in 2 theta.  With the hardware and software supplied for the
 diffractometer, the data collection process  provides substantial redundancy 
 but not necessarily completion up to the limiting resolution.  At a resolution
 of 0.83 \%A (52 deg in 2 theta) essentially full coverage of data 
were met. Successful and suitable refinement of the structure supports this. 
  
;
_shelx_res_checksum              85421
_shelx_hkl_checksum              87661