Metalloporphycenes: Synthesis and Characterization of (Pentamethylcyclopentadienyl)ruthenium Sitting-Atop and π-Complexes
Luciano Cuesta; Elizabeth Karnas; Vincent M. Lynch; Ping Chen; Jing Shen; Karl M. Kadish; Kei Ohkubo; Shunichi Fukuzumi; Jonathan L. Sessler; Journal of the American Chemical Society 131 (2009) 13538–13547; doi:10.1021/ja905284d

data_4105044
_publ_section_title
;
 Metalloporphycenes: Synthesis and Characterization of
 (Pentamethylcyclopentadienyl)ruthenium Sitting-Atop and \p-Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              13538
_journal_page_last               13547
_journal_paper_doi               10.1021/ja905284d
_journal_volume                  131
_journal_year                    2009
_chemical_formula_moiety         'C32 H36 N4, C10 H15, Ru, P F6'
_chemical_formula_sum            'C42 H51 F6 N4 P Ru'
_chemical_formula_weight         857.91
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 90.525(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.737(2)
_cell_length_b                   25.642(2)
_cell_length_c                   13.8213(12)
_cell_measurement_reflns_used    6739
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.0
_cell_measurement_theta_min      1.0
_cell_volume                     7703.4(11)
_computing_cell_refinement       'Collect software, Nonius B.V. 1998'
_computing_data_collection       'Collect software, Nonius B.V. 1998'
_computing_data_reduction
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_solution
;

SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., 
Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R.
;
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.587
_diffrn_measured_fraction_theta_max 0.587
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71070
_diffrn_reflns_av_R_equivalents  0.0000
_diffrn_reflns_av_sigmaI/netI    0.2394
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            11835
_diffrn_reflns_theta_full        24.99
_diffrn_reflns_theta_max         24.99
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.514
_exptl_absorpt_correction_T_max  1.04
_exptl_absorpt_correction_T_min  0.62
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_exptl_crystal_density_diffrn    1.479
_exptl_crystal_F_000             3552
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.947
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.232
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     992
_refine_ls_number_reflns         11835
_refine_ls_number_restraints     648
_refine_ls_restrained_S_all      1.216
_refine_ls_R_factor_all          0.2232
_refine_ls_R_factor_gt           0.1020
_refine_ls_shift/su_max          0.054
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0320P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.2088
_reflns_number_gt                6025
_reflns_number_total             11835
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905284d_si_004.cif
_cod_data_source_block           lc136p
_cod_database_code               4105044