Diastereoselective methylation of bis(N-confused porphyrinatonickel(II)): access to configurationally stable chiral bis(porphyrinoid) and non-symmetric dimers.
Chmielewski, Piotr J.; Maciołek, Justyna; Chemical communications (Cambridge, England) 48 (2012) 428–430; doi:10.1039/c1cc14536c

data_7112550
_publ_section_title
;
 Diastereoselective methylation of bis(N-confused porphyrinatonickel(II)):
 access to configurationally stable chiral bis(porphyrinoid) and
 non-symmetric dimers.
;
_journal_issue                   3
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              428
_journal_page_last               430
_journal_paper_doi               10.1039/c1cc14536c
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C100 H78 Cl4 N8 Ni2'
_chemical_formula_weight         1650.92
_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-97
_cell_angle_alpha                100.664(2)
_cell_angle_beta                 102.767(2)
_cell_angle_gamma                111.139(2)
_cell_formula_units_Z            2
_cell_length_a                   13.3922(3)
_cell_length_b                   15.4736(3)
_cell_length_c                   23.0929(4)
_cell_measurement_reflns_used    24989
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      38.5154
_cell_measurement_theta_min      4.7138
_cell_volume                     4164.63(18)
_computing_cell_refinement
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_collection
;
CrysAlis CCD, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_data_reduction
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.33.48 (release 15-09-2009 CrysAlis171 .NET)
(compiled Sep 15 2009,11:49:04)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.957
_diffrn_measurement_device_type  'Xcalibur with Onyx CCD'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.1401
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       40
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            94045
_diffrn_reflns_theta_full        27.00
_diffrn_reflns_theta_max         38.59
_diffrn_reflns_theta_min         4.73
_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.317
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1716
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_platon_squeeze_details
;
;
_refine_diff_density_max         1.476
_refine_diff_density_min         -1.575
_refine_diff_density_rms         0.099
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.834
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1035
_refine_ls_number_reflns         45163
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.834
_refine_ls_R_factor_all          0.1137
_refine_ls_R_factor_gt           0.0516
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0749P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1362
_refine_ls_wR_factor_ref         0.1460
_reflns_number_gt                21181
_reflns_number_total             45163
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c1cc14536c.txt
_cod_data_source_block           chni3
_cod_depositor_comments
;

2018-03-14
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C200 H156 Cl8 N16 Ni4'
_cod_original_formula_weight         3301.85
_cod_original_formula_units_Z            1
_cod_original_cell_volume        4164.62(18)
_cod_database_code               7112550