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_4318629
_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           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 102.44(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.920(5)
_cell_length_b                   20.254(5)
_cell_length_c                   18.366(5)
_cell_measurement_reflns_used    7233
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      28.37
_cell_measurement_theta_min      2.21
_cell_volume                     8326(4)
_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 0.994
_diffrn_measured_fraction_theta_max 0.994
_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     0.6929
_diffrn_reflns_av_R_equivalents  0.2070
_diffrn_reflns_av_sigmaI/netI    0.1489
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            13361
_diffrn_reflns_theta_full        20.27
_diffrn_reflns_theta_max         20.27
_diffrn_reflns_theta_min         3.55
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.276
_exptl_absorpt_correction_T_max  0.9945
_exptl_absorpt_correction_T_min  0.9836
_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            orange
_exptl_crystal_density_diffrn    1.218
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3232
_exptl_crystal_size_max          0.06
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         7.736
_refine_diff_density_min         -7.001
_refine_diff_density_rms         0.293
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.822
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         4335
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.822
_refine_ls_R_factor_all          0.2451
_refine_ls_R_factor_gt           0.2036
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4681
_refine_ls_wR_factor_ref         0.5064
_reflns_number_gt                2856
_reflns_number_total             4335
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic025727y_2.cif
_cod_data_source_block           js0016
_cod_database_code               4318629