Organometallic Chemistry of Azuliporphyrins: Synthesis, Spectroscopy, Electrochemistry, and Structural Characterization of Nickel(II), Palladium(II), and Platinum(II) Complexes of Azuliporphyrins
Timothy D. Lash; Denise A. Colby; Shelley R. Graham; Gregory M. Ferrence; Lisa F. Szczepura; Inorganic Chemistry 42 (2003) 7326–7338; doi:10.1021/ic030166b

data_4312365
_publ_contact_author             'Ferrence, Gregory M.'
_publ_section_title
;
 Organometallic Chemistry of Azuliporphyrins: Synthesis, Spectroscopy,
 Electrochemistry, and Structural Characterization of Nickel(II),
 Palladium(II), and Platinum(II) Complexes of Azuliporphyrins
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7326
_journal_page_last               7338
_journal_paper_doi               10.1021/ic030166b
_journal_volume                  42
_journal_year                    2003
_chemical_compound_source        'Lash Laboratory'
_chemical_formula_moiety         'C44 H35 N3 Ni1'
_chemical_formula_structural     'C44 H35 N3 Ni1'
_chemical_formula_sum            'C44 H35 N3 Ni'
_chemical_formula_weight         664.46
_chemical_melting_point_gt       573
_chemical_name_systematic
;
  8,17-diethyl-7,18-dimethyl-12,13-diphenylazuliporphyrinatonickel(II)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2001-06-11T21:10:21-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 96.166(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   31.028(2)
_cell_length_b                   8.8409(6)
_cell_length_c                   11.7434(8)
_cell_measurement_reflns_used    6648
_cell_measurement_temperature    193(2)
_cell_measurement_theta_max      26.383
_cell_measurement_theta_min      2.396
_cell_measurement_wavelength     0.71073
_cell_volume                     3202.8(4)
_computing_cell_refinement       'Brucker SMART (Brucker Analyt. Sys., 1997)'
_computing_data_collection       'Brucker SMART (Brucker Analyt. Sys., 1997)'
_computing_data_reduction        'Brucker SAINT (Brucker Analyt. Sys., 1997)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR-92 (Altomare, G., et.al, 1993)'
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_orient_matrix_type       X=UB
_diffrn_orient_matrix_UB_11      0.0027586
_diffrn_orient_matrix_UB_12      -0.1100194
_diffrn_orient_matrix_UB_13      -0.0176115
_diffrn_orient_matrix_UB_21      0.0012010
_diffrn_orient_matrix_UB_22      -0.0241557
_diffrn_orient_matrix_UB_23      0.0834709
_diffrn_orient_matrix_UB_31      -0.0322761
_diffrn_orient_matrix_UB_32      -0.0103019
_diffrn_orient_matrix_UB_33      -0.0076387
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_limit_h_max       38
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            14860
_diffrn_reflns_theta_full        26.41
_diffrn_reflns_theta_max         26.41
_diffrn_reflns_theta_min         1.8
_exptl_absorpt_coefficient_mu    0.644
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             1392
_exptl_crystal_preparation       'diffusion of hexanes into CH2Cl2'
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     433
_refine_ls_number_reflns         6534
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.082
_refine_ls_R_factor_gt           0.0519
_refine_ls_shift/su_max          0.006
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.2780P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1161
_refine_ls_wR_factor_ref         0.1286
_reflns_number_gt                4718
_reflns_number_total             6534
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030166b.cif
_cod_data_source_block           isu0104
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' tag was changed to
'_chemical_melting_point_gt' since the value was specified 'more
than' ('>') a certain temperature. The value '>573 K' was changed to
'573' - it should be numeric and without a unit designator.

Automatic conversion script
Id: cif_fix_values 1569 2011-02-09 13:29:24Z adriana 
;
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4312365