Facile Synthesis of Rhodium(III) Porphyrin Silyls by Silicon−Hydrogen Bond Activation with Rhodium(III) Porphyrin Halides and Methyls
Zhang, Lirong; Chan, Kin Shing; Organometallics 25 (2006) 4822–; doi:10.1021/om0604472

data_4074167
_publ_section_title
;
 Facile Synthesis of Rhodium(III) Porphyrin Silyls by
 Silicon&#x2212;Hydrogen Bond Activation with Rhodium(III) Porphyrin
 Halides and Methyls
;
_journal_issue                   20
_journal_name_full               Organometallics
_journal_page_first              4822
_journal_paper_doi               10.1021/om0604472
_journal_volume                  25
_journal_year                    2006
_chemical_formula_sum            'C64 H65 N4 O Rh Si'
_chemical_formula_weight         1037.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           80
_symmetry_space_group_name_Hall  'I 4bw'
_symmetry_space_group_name_H-M   'I 41'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.4903(14)
_cell_length_b                   28.4903(14)
_cell_length_c                   14.7397(16)
_cell_measurement_temperature    293(2)
_cell_volume                     11964.2(15)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.1000
_diffrn_reflns_av_sigmaI/netI    0.1245
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            33010
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.01
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_T_max  0.9661
_exptl_absorpt_correction_T_min  0.9031
_exptl_crystal_density_diffrn    1.152
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             4352
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.911
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.133
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.29(8)
_refine_ls_extinction_coef       0.00112(19)
_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   1.034
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     642
_refine_ls_number_reflns         10378
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.034
_refine_ls_R_factor_all          0.1901
_refine_ls_R_factor_gt           0.0888
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1777P)^2^+8.3503P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2210
_refine_ls_wR_factor_ref         0.3125
_reflns_number_gt                5217
_reflns_number_total             10378
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om0604472si20060522_025042.cif
_cod_data_source_block           p
_cod_database_code               4074167