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_4318628
_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            'C100 H106 N4 P2 Ru'
_chemical_formula_weight         1526.90
_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                71.554(2)
_cell_angle_beta                 73.964(2)
_cell_angle_gamma                73.214(2)
_cell_formula_units_Z            1
_cell_length_a                   11.1136(5)
_cell_length_b                   12.4931(5)
_cell_length_c                   16.7167(7)
_cell_measurement_reflns_used    10146
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      25.03
_cell_measurement_theta_min      2.91
_cell_volume                     2063.81(15)
_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  0.0316
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            11339
_diffrn_reflns_theta_full        25.02
_diffrn_reflns_theta_max         25.02
_diffrn_reflns_theta_min         3.52
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.279
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.229
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             808
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.321
_refine_diff_density_min         -0.421
_refine_diff_density_rms         0.075
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.200
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     494
_refine_ls_number_reflns         7184
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.200
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_gt           0.0551
_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^)+(0.0000P)^2^+5.6321P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1312
_refine_ls_wR_factor_ref         0.1356
_reflns_number_gt                6175
_reflns_number_total             7184
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025727y_1.cif
_cod_data_source_block           js0018
_cod_database_code               4318628