New palladium catalysed reactions of bromoporphyrins: synthesis and crystal structures of nickel(II) complexes of primary 5-aminoporphyrin, 5,5'-bis(porphyrinyl) secondary amine, and 5-hydroxyporphyrin
Louisa J. Esdaile; D.P.Arnold; M.Senge; Chemical Communications  (2006) –; doi:10.1039/b608365j

data_7101479
_publ_section_title
;
New palladium catalysed reactions of bromoporphyrins:
synthesis and crystal structures of nickel(II) complexes of primary
5-aminoporphyrin, 5,5'-bis(porphyrinyl) secondary amine, and
5-hydroxyporphyrin
;
_journal_issue                   40
_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/b608365j
_journal_year                    2006
_chemical_formula_moiety         'C76 H47 N9 Ni2'
_chemical_formula_sum            'C76 H47 N9 Ni2'
_chemical_formula_weight         1203.65
_chemical_melting_point          ?
_chemical_name_common
Bis((10,15,20-triphenylporphyrinato-5-yl)nickel(ii))amine
_chemical_name_systematic
;
Bis[(10,15,20-triphenylporphyrinato-5-yl)nickel(II)]amine
;
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                101.5380(10)
_cell_angle_beta                 99.8540(10)
_cell_angle_gamma                95.8160(10)
_cell_formula_units_Z            2
_cell_length_a                   12.4790(9)
_cell_length_b                   14.1516(9)
_cell_length_c                   16.1406(11)
_cell_measurement_reflns_used    3073
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      44.332
_cell_measurement_theta_min      4.773
_cell_volume                     2724.3(3)
_computing_cell_refinement       'SAINT v7.12 (Bruke, 2005)'
_computing_data_collection       'Apex2 v1.0-27 (Bruker, 2005'
_computing_data_reduction        SAINT
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL; Platon (Spek, 2003)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker SMART APex2'
_diffrn_measurement_method       \w
_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  0.0790
_diffrn_reflns_av_sigmaI/netI    0.1172
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            27815
_diffrn_reflns_theta_full        26.12
_diffrn_reflns_theta_max         26.12
_diffrn_reflns_theta_min         1.67
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.750
_exptl_absorpt_correction_T_max  0.98
_exptl_absorpt_correction_T_min  0.94
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.467
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1244
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.676
_refine_diff_density_min         -0.379
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.965
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10802
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.965
_refine_ls_R_factor_all          0.1354
_refine_ls_R_factor_gt           0.0566
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0691P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1178
_refine_ls_wR_factor_ref         0.1489
_reflns_number_gt                5743
_reflns_number_total             10802
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b608365j.txt
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'n/d' was changed to '?' - the value
is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'n/d' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7101479