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_4076041
_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         'C41 H29 Fe N4 P Ru, 0.725(C H2 Cl2)'
_chemical_formula_sum            'C41.725 H30.45 Cl1.45 Fe N4 P Ru'
_chemical_formula_weight         827.18
_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'
_cell_angle_alpha                90.00000
_cell_angle_beta                 101.885(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   16.3170(10)
_cell_length_b                   10.2710(8)
_cell_length_c                   21.581(2)
_cell_measurement_reflns_used    7359
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      31.3
_cell_measurement_theta_min      2.4
_cell_volume                     3539.3(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 PIG'
_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  .058
_diffrn_reflns_av_sigmaI/netI    .063
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            73303
_diffrn_reflns_theta_full        32.2
_diffrn_reflns_theta_max         32.2
_diffrn_reflns_theta_min         1.93
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.029
_exptl_absorpt_correction_T_max  1
_exptl_absorpt_correction_T_min  .83
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.552
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       bar
_exptl_crystal_F_000             1673.8
_exptl_crystal_size_max          .48
_exptl_crystal_size_mid          .22
_exptl_crystal_size_min          .18
_refine_diff_density_max         1.422
_refine_diff_density_min         -.44
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.036
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           atomblock
_refine_ls_number_constraints    0
_refine_ls_number_parameters     479
_refine_ls_number_reflns         9678
_refine_ls_number_restraints     6
_refine_ls_R_factor_all          .062
_refine_ls_R_factor_gt           .042
_refine_ls_shift/su_max          .049
_refine_ls_shift/su_mean         .003
_refine_ls_structure_factor_coef F
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .06
_refine_ls_wR_factor_ref         .054
_reflns_d_resolution_high        .667
_reflns_d_resolution_low         10.537
_reflns_Friedel_coverage         0
_reflns_limit_h_max              24
_reflns_limit_h_min              0
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              31
_reflns_limit_l_min              -32
_reflns_number_gt                9678
_reflns_number_total             12512
_reflns_threshold_expression     'F    > 4.00 sig(F   )'
_cod_data_source_file            om050483lsi20050611_121017.cif
_cod_data_source_block           br959
_cod_original_sg_symbol_Hall     -p_2ybc
_cod_original_sg_symbol_H-M      P_1_21/c_1
_cod_original_formula_sum        'C41.725 H30.45 Cl1.45 Fe1 N4 P1 Ru1'
_cod_database_code               4076041