Porpholactams and chlorolactams: Replacement of a b,b'-double bond in meso-tetraphenyl-porphyrin and -chlorin by a lactam moiety
Joshua Akhigbe; John Haskoor; Matthias Zeller; Christian Bruckner; Chem.Commun. 47 (2011) 8599–; doi:10.1039/c1cc12955d

data_7106707
_publ_section_title
;
 Porpholactams and chlorolactams: Replacement of a b,b'-double bond in
 meso-tetraphenyl-porphyrin and -chlorin by a lactam moiety
;
_journal_name_full               Chem.Commun.
_journal_page_first              8599
_journal_paper_doi               10.1039/c1cc12955d
_journal_volume                  47
_journal_year                    2011
_chemical_formula_moiety         'C43 H30 N6 O, 0.37(H2 O)'
_chemical_formula_sum            'C43 H30.74 N6 O1.37'
_chemical_formula_weight         653.34
_chemical_name_systematic
;
?
;
_space_group_IT_number           2
_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                76.707(4)
_cell_angle_beta                 78.360(4)
_cell_angle_gamma                65.649(4)
_cell_formula_units_Z            2
_cell_length_a                   11.737(4)
_cell_length_b                   12.257(4)
_cell_length_c                   13.154(4)
_cell_measurement_reflns_used    2668
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      29.93
_cell_measurement_theta_min      2.35
_cell_volume                     1665.5(9)
_computing_cell_refinement       'Apex2 v2009.7-0'
_computing_data_collection       'Apex2 v2009.7-0 (Bruker, 2009)'
_computing_data_reduction        'Apex2 v2009.7-0'
_computing_molecular_graphics    'SHELXTL 6.14'
_computing_publication_material  'SHELXTL 6.14'
_computing_structure_refinement  'SHELXTL 6.14'
_computing_structure_solution
'SHELXTL 6.14 (Bruker, 2000-2003; Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker AXS SMART APEX CCD diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0781
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_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            12566
_diffrn_reflns_theta_full        25.03
_diffrn_reflns_theta_max         25.03
_diffrn_reflns_theta_min         1.60
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.081
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.5694
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex2 v2009.7-0 (Bruker, 2009)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             683.1
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.09
_refine_diff_density_max         0.825
_refine_diff_density_min         -0.402
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       0.016(3)
_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_ref   1.049
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     516
_refine_ls_number_reflns         5846
_refine_ls_number_restraints     85
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.1432
_refine_ls_R_factor_gt           0.0861
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0944P)^2^+3.7220P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2284
_refine_ls_wR_factor_ref         0.2608
_reflns_number_gt                3393
_reflns_number_total             5846
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            c1cc12955d.txt
_cod_data_source_block           10mz481_0m
_cod_original_cell_volume        1665.6(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7106707