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_4332606
_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         'C62 H34 F20 N4 P2 Ru'
_chemical_formula_sum            'C62 H34 F20 N4 P2 Ru'
_chemical_formula_weight         1377.94
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 92.99(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.103(2)
_cell_length_b                   11.570(2)
_cell_length_c                   21.840(4)
_cell_measurement_reflns_used    0
_cell_measurement_temperature    301(2)
_cell_measurement_theta_max      0
_cell_measurement_theta_min      0
_cell_volume                     2801.8(9)
_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 (Sheldrick, 1997)'
_diffrn_ambient_temperature      301(2)
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_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  0.0462
_diffrn_reflns_av_sigmaI/netI    0.0692
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            19781
_diffrn_reflns_theta_full        25.63
_diffrn_reflns_theta_max         25.63
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.450
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark brown'
_exptl_crystal_density_diffrn    1.633
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1376
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.452
_refine_diff_density_min         -0.356
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     411
_refine_ls_number_reflns         5198
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0364
_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^)+(0.0393P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0960
_refine_ls_wR_factor_ref         0.1026
_reflns_number_gt                3658
_reflns_number_total             5198
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060553wsup1.cif
_cod_data_source_block           complex_1c
_cod_original_cell_volume        2801.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4332606