Reduction of terphenyl iron(ii) or cobalt(ii) halides in the presence of trimethylphosphine: an unusual triple dehydrogenation of an alkyl group
Ni, Chengbao; Ellis, Bobby D.; Stich, Troy A.; Fettinger, James C.; Long, Gary J.; Britt, R. David; Power, Philip P.; Dalton Transactions  (2009) 5401–5405; doi:10.1039/b904647j

data_7003019
_publ_section_title
;
 Reduction of terphenyl iron(ii) or cobalt(ii) halides in the presence
 of trimethylphosphine: an unusual triple dehydrogenation of an alkyl
 group
;
_journal_issue                   27
_journal_name_full               'Dalton Transactions'
_journal_page_first              5401
_journal_page_last               5405
_journal_paper_doi               10.1039/b904647j
_journal_year                    2009
_chemical_formula_moiety         'C39 H62 Co P3'
_chemical_formula_sum            'C39 H62 Co P3'
_chemical_formula_weight         682.73
_chemical_name_systematic
;
?
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   23.347(5)
_cell_length_b                   12.992(3)
_cell_length_c                   26.446(5)
_cell_measurement_reflns_used    8041
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      27.39
_cell_measurement_theta_min      2.81
_cell_volume                     8022(3)
_computing_cell_refinement       'SAINT (7.46A) (Bruker, 2006)'
_computing_data_collection       'Apex2 (2.1-4) (Bruker, 2007)'
_computing_data_reduction        'SAINT (7.46A) (Bruker, 2006)'
_computing_molecular_graphics    'SHELXTL 5.1, XP (Sheldrick, 1994)'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEXII CCD'
_diffrn_measurement_method       '\w and \f'
_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  0.0435
_diffrn_reflns_av_sigmaI/netI    0.0199
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            98145
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.81
_exptl_absorpt_coefficient_mu    0.571
_exptl_absorpt_correction_T_max  0.9557
_exptl_absorpt_correction_T_min  0.8895
_exptl_absorpt_correction_type   'Empirical, SADabs (multi-scan)'
_exptl_absorpt_process_details   'SADABS 2007/3 (Sheldrick, 2007)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.131
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_platon_squeeze_details
;
;
_refine_diff_density_max         0.474
_refine_diff_density_min         -0.260
_refine_diff_density_rms         0.048
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.052
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     414
_refine_ls_number_reflns         9193
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.054
_refine_ls_R_factor_all          0.0405
_refine_ls_R_factor_gt           0.0293
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0352P)^2^+3.8133P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0715
_refine_ls_wR_factor_ref         0.0774
_reflns_number_gt                7608
_reflns_number_total             9193
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904647j.txt
_cod_data_source_block           final
_cod_original_cell_volume        8021(3)
_cod_database_code               7003019