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_4339262
_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 H72 N8 Ni1 O12, 2(C1 H2 Cl2)'
_chemical_formula_sum            'C92 H76 Cl4 N8 Ni O12'
_chemical_formula_weight         1686.12
_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_conform_dict_location     ftp://ftp.iucr.org/pub/cif_core.dic
_audit_conform_dict_name         cif_core.dic
_audit_conform_dict_version      2.3
_audit_creation_date             2006-10-24T10:51:33-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                77.743(5)
_cell_angle_beta                 75.776(4)
_cell_angle_gamma                70.863(5)
_cell_formula_units_Z            2
_cell_length_a                   12.6081(12)
_cell_length_b                   14.1098(14)
_cell_length_c                   24.181(2)
_cell_measurement_reflns_used    7866
_cell_measurement_temperature    102(2)
_cell_measurement_theta_max      27.66
_cell_measurement_theta_min      2.23
_cell_measurement_wavelength     0.71073
_cell_volume                     3898.4(6)
_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      102(2)
_diffrn_detector                 'CCD plate'
_diffrn_measured_fraction_theta_full 0.984
_diffrn_measured_fraction_theta_max 0.984
_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  0.0632
_diffrn_reflns_av_unetI/netI     0.0645
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            79733
_diffrn_reflns_theta_full        27.66
_diffrn_reflns_theta_max         27.66
_diffrn_reflns_theta_min         2.23
_exptl_absorpt_coefficient_mu    0.458
_exptl_absorpt_correction_T_max  0.925
_exptl_absorpt_correction_T_min  0.803
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.436
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1752
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.902
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.04
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1054
_refine_ls_number_reflns         17912
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.04
_refine_ls_R_factor_all          0.0842
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0630P)^2^+3.3767P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1246
_refine_ls_wR_factor_ref         0.1409
_reflns_number_gt                12650
_reflns_number_total             17912
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0703272-file001.cif
_cod_data_source_block           1Ni
_cod_original_cell_volume        3898.5(6)
_cod_database_code               4339262