Cationic nickel porphyrinoids with unexpected reactivity
Wicht, Richard; Bahnmüller, Stefanie; Brandhorst, Kai; Schweyen, Peter; Bröring, Martin; Chem. Sci. 7 (2016) 583–; doi:10.1039/C5SC03663A

data_1540747
_publ_section_title
;
 Cationic nickel porphyrinoids with unexpected reactivity
;
_journal_issue                   1
_journal_name_full               'Chem. Sci.'
_journal_page_first              583
_journal_paper_doi               10.1039/C5SC03663A
_journal_volume                  7
_journal_year                    2016
_chemical_formula_moiety
;
 C72 H92 N8 Ni2, 2(B F4), 3.657(C H Cl3)
;
_chemical_formula_sum            'C75.66 H95.66 B2 Cl10.97 F8 N8 Ni2'
_chemical_formula_weight         1797.07
_chemical_name_systematic
;
 ?
;
_chemical_properties_physical    Moisture-sensitive
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_audit_update_record
;
2015-03-30 deposited with the CCDC.
2015-10-16 downloaded from the CCDC.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 104.352(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.0884(11)
_cell_length_b                   31.4527(15)
_cell_length_c                   18.2241(14)
_cell_measurement_reflns_used    18138
_cell_measurement_temperature    100.0(3)
_cell_measurement_theta_max      75.2300
_cell_measurement_theta_min      3.6610
_cell_volume                     8378.7(10)
_computing_cell_refinement
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_collection
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_data_reduction
;
 CrysAlisPro, Oxford Diffraction Ltd.,
 Version 1.171.34.40 (release 27-08-2010 CrysAlis171 .NET)
 (compiled Aug 27 2010,11:50:40)
;
_computing_molecular_graphics
;
 ORTEP3 for Windows (L. J. Farrugia, J. Appl. Crystallogr. 1997, 30, 565.)
;
_computing_publication_material
;
 WinGX v1.70.01 (L. J. Farrugia, J. Appl. Cryst., 1999, 32, 837-838.)
;
_computing_structure_refinement
;
 SHELXL-97 (G. M. Sheldrick, Acta Cryst. (2008). A64, 122-122)'
;
_computing_structure_solution
;
 SHELXS-97 (G. M. Sheldrick, Z. Dauter, K. S, Wilson, H. Hope, 
 L. C. Sieker, Acta Cryst. (1993), D49, 18)
;
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10.3543
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Diffraction, Xcalibur, Atlas, Nova'
_diffrn_measurement_method       \w-scan
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Nova (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0904
_diffrn_reflns_av_sigmaI/netI    0.0576
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            95426
_diffrn_reflns_theta_full        74.99
_diffrn_reflns_theta_max         74.99
_diffrn_reflns_theta_min         3.33
_exptl_absorpt_coefficient_mu    4.311
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.62546
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 CrysAlisPro, Agilent Technologies,
 Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET)
 (compiled Feb  1 2013,16:14:44)
 Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.426
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             3720.4
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: chloroform, n-hexane'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.564
_refine_diff_density_min         -0.602
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1039
_refine_ls_number_reflns         17132
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.028
_refine_ls_R_factor_all          0.0946
_refine_ls_R_factor_gt           0.0660
_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^)+(0.0934P)^2^+8.0765P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1650
_refine_ls_wR_factor_ref         0.1844
_reflns_number_gt                12109
_reflns_number_total             17132
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c5sc03663a2.cif
_cod_data_source_block           rw100bb_(sb)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               1540747