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_4318630
_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_moiety         'C108 H106 N4 P2 Ru, 4(C H Cl3)'
_chemical_formula_sum            'C112 H110 Cl12 N4 P2 Ru'
_chemical_formula_weight         2100.45
_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                87.730(2)
_cell_angle_beta                 83.010(2)
_cell_angle_gamma                67.105(2)
_cell_formula_units_Z            1
_cell_length_a                   13.8041(7)
_cell_length_b                   13.8388(8)
_cell_length_c                   14.7719(8)
_cell_measurement_reflns_used    20080
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.18
_cell_measurement_theta_min      3.04
_cell_volume                     2580.2(2)
_computing_cell_refinement       'Bruker SAINT (Bruker AXS, 1994)'
_computing_data_collection       'Bruker SMART (Bruker AXS, 1994)'
_computing_data_reduction        'Bruker SAINT (Bruker AXS, 1994)'
_computing_molecular_graphics    'XP (Sheldrick, 1996)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 8.192
_diffrn_measured_fraction_theta_full 0.856
_diffrn_measured_fraction_theta_max 0.856
_diffrn_measurement_device_type  'Bruker SMART CCD'
_diffrn_measurement_method       'Thin slice \w-scans'
_diffrn_radiation_monochromator  'Silicon 111'
_diffrn_radiation_source         'Daresbury SRS, Station 9.8'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.6923
_diffrn_reflns_av_R_equivalents  0.0258
_diffrn_reflns_av_sigmaI/netI    0.0430
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            25065
_diffrn_reflns_theta_full        29.44
_diffrn_reflns_theta_max         29.44
_diffrn_reflns_theta_min         1.73
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.544
_exptl_absorpt_correction_T_max  0.9681
_exptl_absorpt_correction_T_min  0.9578
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;

Correction applied by SADABS - note that the transmission factors are

not real since they include corrections for beam decay and possibly

crystal decay (the two cannot be distinguished).

The numbers listed in the CIF are those calculated by SHELXL.

;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.352
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1088
_exptl_crystal_size_max          0.08
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.021
_refine_diff_density_min         -1.402
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     604
_refine_ls_number_reflns         13243
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0514
_refine_ls_shift/su_max          0.024
_refine_ls_shift/su_mean         0.002
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0869P)^2^+1.3889P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1333
_refine_ls_wR_factor_ref         0.1365
_reflns_number_gt                11428
_reflns_number_total             13243
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025727y_3.cif
_cod_data_source_block           js0007
_cod_database_code               4318630