One-Pot Synthesis of Metal Primary Phosphine Complexes from OPCl2R or PCl2R. Isolation and Characterization of Primary Alkylphosphine Complexes of a Metalloporphyrin
Huang, Jie-Sheng; Yu, Guang-Ao; Xie, Jin; Zhu, Nianyong; Che, Chi-Ming; Inorganic Chemistry 45 (2006) 5724–5726; doi:10.1021/ic060553w

data_4332607
_publ_section_title
;
 One-Pot Synthesis of Metal Primary Phosphine Complexes from OPCl2R or
 PCl2R. Isolation and Characterization of Primary Alkylphosphine Complexes
 of a Metalloporphyrin
;
_journal_issue                   15
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5724
_journal_page_last               5726
_journal_paper_doi               10.1021/ic060553w
_journal_volume                  45
_journal_year                    2006
_chemical_formula_moiety         'C78 H94 N4 P2 Ru'
_chemical_formula_sum            'C78 H94 N4 P2 Ru'
_chemical_formula_weight         1250.58
_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                78.01(3)
_cell_angle_beta                 78.97(3)
_cell_angle_gamma                72.70(3)
_cell_formula_units_Z            1
_cell_length_a                   11.194(2)
_cell_length_b                   11.597(2)
_cell_length_c                   14.722(3)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     1767.6(7)
_computing_cell_refinement       scalepack
_computing_data_collection       marcontrol
_computing_data_reduction        Denzo
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.906
_diffrn_measured_fraction_theta_max 0.906
_diffrn_measurement_device_type  'marresearch IPDS mar300'
_diffrn_measurement_method       oscillation
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0284
_diffrn_reflns_av_sigmaI/netI    0.0593
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            13161
_diffrn_reflns_theta_full        25.49
_diffrn_reflns_theta_max         25.49
_diffrn_reflns_theta_min         2.16
_exptl_absorpt_coefficient_mu    0.311
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             664
_exptl_crystal_size_max          0.6
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.522
_refine_diff_density_min         -0.375
_refine_diff_density_rms         0.078
_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     370
_refine_ls_number_reflns         5955
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0465
_refine_ls_R_factor_gt           0.0403
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0796P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1170
_refine_ls_wR_factor_ref         0.1200
_reflns_number_gt                5207
_reflns_number_total             5955
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060553wsup2.cif
_cod_data_source_block           complex_2a
_cod_original_cell_volume        1767.6(6)
_cod_database_code               4332607