Syntheses, Structures, Some Reactions, and Electrochemical Oxidation of Ferrocenylethynyl Complexes of Iron, Ruthenium, and Osmium
Bruce, Michael I.; Low, Paul J.; Hartl, František; Humphrey, Paul A.; de Montigny, Frédéric; Jevric, Martyn; Lapinte, Claude; Perkins, Gary J.; Roberts, Rachel L.; Skelton, Brian W.; White, Allan H.; Organometallics 24 (2005) 5241–; doi:10.1021/om050483l

data_4076042
_publ_section_title
;
 Syntheses, Structures, Some Reactions, and Electrochemical Oxidation of
 Ferrocenylethynyl Complexes of Iron, Ruthenium, and Osmium
;
_journal_issue                   22
_journal_name_full               Organometallics
_journal_page_first              5241
_journal_paper_doi               10.1021/om050483l
_journal_volume                  24
_journal_year                    2005
_chemical_formula_moiety         'C49 H38 Fe1 N4 P2 Ru, C H2 Cl2'
_chemical_formula_sum            'C50 H40 Cl2 Fe N4 P2 Ru'
_chemical_formula_weight         986.67
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90.00000
_cell_angle_beta                 96.774(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   8.9587(6)
_cell_length_b                   19.2810(10)
_cell_length_c                   25.191(2)
_cell_measurement_reflns_used    8192
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      24.5
_cell_measurement_theta_min      1.33
_cell_volume                     4320.9(5)
_computing_cell_refinement       'Siemens SAINT (Siemens, 1995)'
_computing_data_collection       'Siemens SMART (Siemens, 1995)'
_computing_data_reduction        'xtal ADDREF SORTRF'
_computing_molecular_graphics    xtal
_computing_publication_material  'xtal BONDLA CIFIO'
_computing_structure_refinement  'xtal CRYLSQ'
_computing_structure_solution    xtal
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type
;
Bruker SMART CCD diffractometer
;
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_detector       'CCD area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     .71073
_diffrn_reflns_av_R_equivalents  .043
_diffrn_reflns_av_sigmaI/netI    .087
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            89959
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         1.33
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    .924
_exptl_absorpt_correction_T_max  .83
_exptl_absorpt_correction_T_min  .72
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.517
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       slab
_exptl_crystal_F_000             2008
_exptl_crystal_size_max          .26
_exptl_crystal_size_mid          .24
_exptl_crystal_size_min          .13
_refine_diff_density_max         1.607
_refine_diff_density_min         -1.744
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.02
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     541
_refine_ls_number_reflns         16335
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .073
_refine_ls_R_factor_gt           .044
_refine_ls_shift/su_max          .03
_refine_ls_shift/su_mean         .008
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .075
_refine_ls_wR_factor_ref         .067
_reflns_d_resolution_high        .583
_reflns_d_resolution_low         15.225
_reflns_Friedel_coverage         0
_reflns_limit_h_max              15
_reflns_limit_h_min              0
_reflns_limit_k_max              32
_reflns_limit_k_min              0
_reflns_limit_l_max              42
_reflns_limit_l_min              -43
_reflns_number_gt                16335
_reflns_number_total             22790
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            om050483lsi20050611_121017.cif
_cod_data_source_block           br875
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C50 H40 Cl2 Fe1 N4 P2 Ru1'
_cod_database_code               4076042