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_4117151
_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            'C46 H32 Cl2 N4 Ni'
_chemical_formula_weight         770.37
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 115.00(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.055(3)
_cell_length_b                   15.795(3)
_cell_length_c                   17.069(3)
_cell_measurement_temperature    293(2)
_cell_volume                     3678.6(15)
_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  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0429
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            3762
_diffrn_reflns_theta_max         74.98
_diffrn_reflns_theta_min         3.24
_exptl_absorpt_coefficient_mu    2.402
_exptl_crystal_density_diffrn    1.391
_exptl_crystal_F_000             1592
_refine_diff_density_max         0.656
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.0008(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_all   1.047
_refine_ls_goodness_of_fit_obs   1.048
_refine_ls_matrix_type           full
_refine_ls_number_parameters     476
_refine_ls_number_reflns         3622
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_restrained_S_obs      1.048
_refine_ls_R_factor_all          0.0692
_refine_ls_R_factor_obs          0.0691
_refine_ls_shift/esd_max         -0.051
_refine_ls_shift/esd_mean        0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+12.4798P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1850
_refine_ls_wR_factor_obs         0.1849
_reflns_number_observed          3619
_reflns_number_total             3622
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9527028_1.cif
_cod_data_source_block           MeCPNi
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.1101P)^2^+12.4798P] 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^)+(0.1101P)^2^+12.4798P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3678.6(12)
_cod_database_code               4117151