Synthesis of N-confused tetraphenylporphyrin rhodium complexes having versatile metal oxidation states.
Srinivasan, Alagar; Toganoh, Motoki; Niino, Teppei; Osuka, Atsuhiro; Furuta, Hiroyuki; Inorganic chemistry 47 (2008) 11305–11313; doi:10.1021/ic061093+

data_4338703
_publ_section_title
;
 Synthesis of N-confused tetraphenylporphyrin rhodium complexes having
 versatile metal oxidation states.
;
_journal_issue                   23
_journal_name_full               'Inorganic chemistry'
_journal_page_first              11305
_journal_page_last               11313
_journal_paper_doi               10.1021/ic061093+
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C44 H28 I2 N4 Rh, C2 H6 O'
_chemical_formula_sum            'C46 H34 I2 N4 O Rh'
_chemical_formula_weight         1015.48
_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_method           SHELXL-97
_cell_angle_alpha                64.512(2)
_cell_angle_beta                 86.478(5)
_cell_angle_gamma                66.596(4)
_cell_formula_units_Z            1
_cell_length_a                   9.1089(7)
_cell_length_b                   11.3145(12)
_cell_length_c                   11.7172(12)
_cell_measurement_temperature    123(2)
_cell_volume                     991.61(17)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0272
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7554
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.19
_exptl_absorpt_coefficient_mu    2.028
_exptl_absorpt_correction_T_max  0.8546
_exptl_absorpt_correction_T_min  0.6311
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
; 
    Higashi, T. (1995). Program for Absorption Correction.
    Rigaku Corporation, Tokyo, Japan. 
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.701
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             497
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.543
_refine_diff_density_min         -0.700
_refine_diff_density_rms         0.132
_refine_ls_extinction_coef       0.0092(9)
_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   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     260
_refine_ls_number_reflns         3788
_refine_ls_number_restraints     349
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0409
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+3.6222P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0947
_refine_ls_wR_factor_ref         0.0974
_reflns_number_gt                3523
_reflns_number_total             3788
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061093%2B_si_002.cif
_cod_data_source_block           Rh(NCTPP)I2
_cod_original_cell_volume        991.61(16)
_cod_database_code               4338703