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_7101480
_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         'C38 H24 N4 Ni O'
_chemical_formula_sum            'C38 H24 N4 Ni O'
_chemical_formula_weight         611.32
_chemical_melting_point          ?
_chemical_name_common
(5-Hydroxy-10,15,20-triphenylporphyrinato)nickel(ii)
_chemical_name_systematic
;
(5-Hydroxy-10,15,20-triphenylporphyrinato)nickel(II)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                69.02(3)
_cell_angle_beta                 77.92(3)
_cell_angle_gamma                85.14(3)
_cell_formula_units_Z            2
_cell_length_a                   9.6815(19)
_cell_length_b                   12.028(2)
_cell_length_c                   12.986(3)
_cell_measurement_reflns_used    3868
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      50.575
_cell_measurement_theta_min      4.925
_cell_volume                     1380.6(6)
_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
_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 1.000
_diffrn_measured_fraction_theta_max 0.978
_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  0.0624
_diffrn_reflns_av_sigmaI/netI    0.0647
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            15377
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.51
_diffrn_reflns_theta_min         1.71
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.744
_exptl_absorpt_correction_T_max  0.9853
_exptl_absorpt_correction_T_min  0.8077
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'program SADABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.471
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       parallelpiped
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.02
_exptl_crystal_size_min          0.01
_refine_diff_density_max         1.624
_refine_diff_density_min         -0.710
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         5050
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.052
_refine_ls_R_factor_all          0.0862
_refine_ls_R_factor_gt           0.0573
_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^)+(0.1112P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1464
_refine_ls_wR_factor_ref         0.1690
_reflns_number_gt                3718
_reflns_number_total             5050
_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               7101480