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_4105042
_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, Cu, Ru, P F6, C H2 Cl2'
_chemical_formula_sum            'C43 H53 Cl2 Cu F6 N4 P Ru'
_chemical_formula_weight         1006.37
_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                73.990(3)
_cell_angle_beta                 77.861(3)
_cell_angle_gamma                82.878(3)
_cell_formula_units_Z            2
_cell_length_a                   10.2466(7)
_cell_length_b                   12.5796(10)
_cell_length_c                   17.5498(15)
_cell_measurement_reflns_used    7101
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.0
_cell_volume                     2120.5(3)
_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 0.980
_diffrn_measured_fraction_theta_max 0.980
_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     0.71069
_diffrn_reflns_av_R_equivalents  0.0396
_diffrn_reflns_av_sigmaI/netI    0.1092
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            14990
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.81
_exptl_absorpt_coefficient_mu    1.085
_exptl_absorpt_correction_T_max  0.926
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
DENZO and Scalepack (Otwinoski and Minor, 1997)
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.576
_exptl_crystal_description       needles
_exptl_crystal_F_000             1030
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.861
_refine_diff_density_min         -0.829
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     548
_refine_ls_number_reflns         9552
_refine_ls_number_restraints     64
_refine_ls_restrained_S_all      1.046
_refine_ls_R_factor_all          0.1099
_refine_ls_R_factor_gt           0.0565
_refine_ls_shift/su_max          0.015
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0309P)^2^+2.9225P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0987
_refine_ls_wR_factor_ref         0.1178
_reflns_number_gt                6337
_reflns_number_total             9552
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja905284d_si_002.cif
_cod_data_source_block           lc164
_cod_database_code               4105042