Do Sitting-Atop Metalloporphyrin Complexes Exist? Observation of N-H—π Bonding in Arene Solvates of a Diprotonated Porphyrin Dication
J. Luis Gárate-Morales; Fook S. Tham; Christopher A. Reed; Inorganic Chemistry 46 (2007) 1514–1516; doi:10.1021/ic062213g

data_4307720
_publ_section_title
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Do Sitting-Atop Metalloporphyrin Complexes Exist? Observation of
N-H---\p Bonding in Arene Solvates of a Diprotonated Porphyrin
Dication
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1514
_journal_page_last               1516
_journal_paper_doi               10.1021/ic062213g
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C71 H66 B22 Cl22 N4 Zn0.05'
_chemical_formula_weight         1995.94
_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                87.025(2)
_cell_angle_beta                 82.280(2)
_cell_angle_gamma                87.631(2)
_cell_formula_units_Z            2
_cell_length_a                   14.5120(15)
_cell_length_b                   15.8141(17)
_cell_length_c                   19.710(2)
_cell_measurement_reflns_used    5558
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.97
_cell_measurement_theta_min      2.36
_cell_volume                     4473.6(8)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0945
_diffrn_reflns_av_sigmaI/netI    0.0846
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            78972
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         1.62
_exptl_absorpt_coefficient_mu    0.727
_exptl_absorpt_correction_T_max  0.9928
_exptl_absorpt_correction_T_min  0.6557
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.482
_exptl_crystal_density_meas      0
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'thin needle frag'
_exptl_crystal_F_000             2011
_exptl_crystal_size_max          0.63
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.697
_refine_diff_density_min         -0.463
_refine_diff_density_rms         0.097
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1113
_refine_ls_number_reflns         18293
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1106
_refine_ls_R_factor_gt           0.0513
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0528P)^2^+5.4865P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1109
_refine_ls_wR_factor_ref         0.1340
_reflns_number_gt                11252
_reflns_number_total             18293
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic062213gsi20061120_091837.cif
_cod_data_source_block           cr221_0m
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
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_cod_original_cell_volume        4473.5(8)
_cod_database_code               4307720