Reactions of Nickel(II) 2-Aza-5,10,15,20-tetraphenyl-21- carbaporphyrin with Methyl Iodide. The First Structural Characterization of a Paramagnetic Organometallic Nickel(II) Complex
Piotr J. Chmielewski; Lechosław Latos-Grażyński; Tadeusz Głowiak; Journal of the American Chemical Society 118 (1996) 5690–5701; doi:10.1021/ja9527028

data_4117152
_publ_section_title
;
 Reactions of Nickel(II) 2-Aza-5,10,15,20-tetraphenyl-21- carbaporphyrin
 with Methyl Iodide. The First Structural Characterization of a
 Paramagnetic Organometallic Nickel(II) Complex
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              5690
_journal_page_last               5701
_journal_paper_doi               10.1021/ja9527028
_journal_volume                  118
_journal_year                    1996
_chemical_formula_sum            'C52 H39 I N4 Ni'
_chemical_formula_weight         905.48
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 93.20(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.946(3)
_cell_length_b                   23.519(5)
_cell_length_c                   13.945(3)
_cell_measurement_temperature    293(2)
_cell_volume                     4239.3(16)
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_sigmaI/netI    0.0394
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3427
_diffrn_reflns_theta_max         64.96
_diffrn_reflns_theta_min         3.69
_exptl_absorpt_coefficient_mu    6.685
_exptl_crystal_density_diffrn    1.419
_exptl_crystal_F_000             1840
_refine_diff_density_max         1.159
_refine_diff_density_min         -0.761
_refine_diff_density_rms         0.095
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.080
_refine_ls_goodness_of_fit_obs   1.080
_refine_ls_matrix_type           full
_refine_ls_number_parameters     502
_refine_ls_number_reflns         3257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.080
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0562
_refine_ls_R_factor_obs          0.0562
_refine_ls_shift/esd_max         0.013
_refine_ls_shift/esd_mean        0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+26.8356P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1440
_refine_ls_wR_factor_obs         0.1440
_reflns_number_observed          3257
_reflns_number_total             3257
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9527028_2.cif
_cod_data_source_block           IMe2CPNi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+26.8356P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0757P)^2^+26.8356P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4117152