Phosphine and Phosphonite Complexes of a Ruthenium(II) Porphyrin. 1. Synthesis, Structure, and Solution State Studies
Eugen Stulz; Michael Maue; Neil Feeder; Simon J. Teat; Yiu-Fai Ng; Andrew D. Bond; Scott L. Darling; Jeremy K. M. Sanders; Inorganic Chemistry 41 (2002) 5255–5268; doi:10.1021/ic025727y

data_4318631
_publ_section_title
;
 Phosphine and Phosphonite Complexes of a Ruthenium(II) Porphyrin. 1.
 Synthesis, Structure, and Solution State Studies
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5255
_journal_page_last               5268
_journal_paper_doi               10.1021/ic025727y
_journal_volume                  41
_journal_year                    2002
_chemical_formula_sum            'C84 H106 N4 O4 P2 Ru'
_chemical_formula_weight         1398.74
_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                87.309(2)
_cell_angle_beta                 77.381(2)
_cell_angle_gamma                84.103(2)
_cell_formula_units_Z            1
_cell_length_a                   9.8043(2)
_cell_length_b                   10.7826(3)
_cell_length_c                   18.6293(6)
_cell_measurement_reflns_used    12351
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      27.48
_cell_measurement_theta_min      1.02
_cell_volume                     1911.06(9)
_computing_cell_refinement       'HKL Scalepack (Otwinowski & Minor 1997)'
_computing_data_collection       'Collect (Nonius B.V. 1998)'
_computing_data_reduction
;

HKL Denzo and Scalepack (Otwinowski & Minor 1997)

;
_computing_publication_material  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick 1997)'
_computing_structure_solution    'SIR-92 (Altomare et al. 1994)'
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Nonius Kappa CCD'
_diffrn_measurement_method       'Thin slice \w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0605
_diffrn_reflns_av_sigmaI/netI    0.0612
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            21731
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         3.58
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.298
_exptl_absorpt_correction_T_max  0.948
_exptl_absorpt_correction_T_min  0.808
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sortav Blessing (1995)'
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.215
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             744
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.647
_refine_diff_density_min         -1.187
_refine_diff_density_rms         0.155
_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     450
_refine_ls_number_reflns         8637
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0703
_refine_ls_R_factor_gt           0.0536
_refine_ls_shift/su_max          0.019
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0728P)^2^+1.7947P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1347
_refine_ls_wR_factor_ref         0.1485
_reflns_number_gt                7160
_reflns_number_total             8637
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025727y_4.cif
_cod_data_source_block           js0020
_cod_database_code               4318631