Syntheses, structures and redox properties of some complexes containing the Os(dppe)Cp* fragment, including [{Os(dppe)Cp*}2(mu-C triple bondCC triple bond C)].
Bruce, Michael I.; Costuas, Karine; Davin, Thomas; Halet, Jean-François; Kramarczuk, Kathy A.; Low, Paul J.; Nicholson, Brian K.; Perkins, Gary J.; Roberts, Rachel L.; Skelton, Brian W.; Smith, Mark E.; White, Allan H.; Dalton transactions (Cambridge, England : 2003)  (2007) 5387–5399; doi:10.1039/b712104k

data_7006298
_publ_section_title
;
 Syntheses, structures and redox properties of some complexes
 containing the Os(dppe)Cp* fragment, including [{Os(dppe)Cp*}2(mu-C
 triple bondCC triple bond C)].
;
_journal_issue                   46
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5387
_journal_page_last               5399
_journal_paper_doi               10.1039/b712104k
_journal_year                    2007
_chemical_formula_moiety         'C38 H41 Os P2, F6 P, C H4 O'
_chemical_formula_sum            'C39 H45 F6 O Os P3'
_chemical_formula_weight         926.90
_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                 103.300(2)
_cell_angle_gamma                90.00000
_cell_formula_units_Z            4
_cell_length_a                   11.7240(10)
_cell_length_b                   17.360(2)
_cell_length_c                   18.500(2)
_cell_measurement_reflns_used    7325
_cell_measurement_temperature    150
_cell_measurement_theta_max      36.2
_cell_measurement_theta_min      2.6
_cell_volume                     3664.3(7)
_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
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_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  .054
_diffrn_reflns_av_sigmaI/netI    .103
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            76389
_diffrn_reflns_theta_full        37.5
_diffrn_reflns_theta_max         37.5
_diffrn_reflns_theta_min         1.63
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    3.673
_exptl_absorpt_correction_T_max  .70
_exptl_absorpt_correction_T_min  .46
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS; Sheldrick, 1996
;
_exptl_crystal_colour            pale_yellow
_exptl_crystal_density_diffrn    1.68
_exptl_crystal_description       prism
_exptl_crystal_F_000             1848
_exptl_crystal_size_max          .35
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .13
_refine_diff_density_max         2.559
_refine_diff_density_min         -1.813
_refine_ls_goodness_of_fit_all   .98
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     615
_refine_ls_number_reflns         13371
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          .069
_refine_ls_R_factor_gt           .035
_refine_ls_shift/su_max          .019
_refine_ls_shift/su_mean         .0005
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details
;
w=1/(sig^2(F) + .0003F^2)
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         .04
_refine_ls_wR_factor_ref         .035
_reflns_d_resolution_high        .583
_reflns_d_resolution_low         12.466
_reflns_Friedel_coverage         0
_reflns_limit_h_max              20
_reflns_limit_h_min              0
_reflns_limit_k_max              29
_reflns_limit_k_min              0
_reflns_limit_l_max              30
_reflns_limit_l_min              -31
_reflns_number_gt                13371
_reflns_number_total             19252
_reflns_threshold_expression     'F > 4.00 sig(F )'
_cod_data_source_file            b712104k.txt
_cod_data_source_block           br778
_cod_original_sg_symbol_Hall     -p_2yn
_cod_original_sg_symbol_H-M      P_1_21/n_1
_cod_original_formula_sum        'C39 H45 F6 O1 Os1 P3'
_cod_database_code               7006298