Structural and coordination studies of "pearl oysterlike" porphyrins.
Halime, Zakaria; Lachkar, Mohammed; Roisnel, Thierry; Richard, Philippe; Boitrel, Bernard; Inorganic chemistry 46 (2007) 6338–6346; doi:10.1021/ic0703272

data_4339263
_publ_section_title
;
 Structural and coordination studies of &quot;pearl oysterlike&quot;
 porphyrins.
;
_journal_issue                   16
_journal_name_full               'Inorganic chemistry'
_journal_page_first              6338
_journal_page_last               6346
_journal_paper_doi               10.1021/ic0703272
_journal_volume                  46
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C90 H64 N8 O12 Pb1'
_chemical_formula_sum            'C90 H64 N8 O12 Pb'
_chemical_formula_weight         1656.68
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_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_date             2007-02-08T12:25:05-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                64.844(4)
_cell_angle_beta                 73.031(4)
_cell_angle_gamma                69.642(4)
_cell_formula_units_Z            2
_cell_length_a                   13.1804(11)
_cell_length_b                   17.0677(14)
_cell_length_c                   20.0012(15)
_cell_measurement_reflns_used    3484
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.45
_cell_measurement_theta_min      2.58
_cell_measurement_wavelength     0.71073
_cell_volume                     3763.0(5)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'SIR97 (Altomare et al., 1999)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device_type  'APEXII, Bruker-AXS'
_diffrn_measurement_method       'CCD rotation images, thin slices'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0905
_diffrn_reflns_av_unetI/netI     0.1677
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            42042
_diffrn_reflns_theta_full        27.48
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         3.05
_exptl_absorpt_coefficient_mu    2.313
_exptl_absorpt_correction_T_max  0.966
_exptl_absorpt_correction_T_min  0.686
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.462
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1676
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.662
_refine_diff_density_min         -1.523
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.962
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1010
_refine_ls_number_reflns         17055
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.962
_refine_ls_R_factor_all          0.121
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0594P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1233
_refine_ls_wR_factor_ref         0.1394
_reflns_number_gt                10601
_reflns_number_total             17055
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0703272-file001.cif
_cod_data_source_block           1Pb
_cod_database_code               4339263