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_7003018
_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         'C45 H74 Co P3'
_chemical_formula_sum            'C45 H74 Co P3'
_chemical_formula_weight         766.88
_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                 106.466(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   19.466(3)
_cell_length_b                   14.368(3)
_cell_length_c                   16.471(3)
_cell_measurement_reflns_used    3327
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      23.64
_cell_measurement_theta_min      2.84
_cell_volume                     4417.8(14)
_computing_cell_refinement       'Bruker SMART APEX II'
_computing_data_collection       'Bruker SMART APEX II'
_computing_data_reduction        'Bruker SMART APEX II'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_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 APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_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  0.1086
_diffrn_reflns_av_sigmaI/netI    0.1009
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            24439
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         25.25
_diffrn_reflns_theta_min         2.60
_exptl_absorpt_coefficient_mu    0.525
_exptl_absorpt_correction_T_max  0.9742
_exptl_absorpt_correction_T_min  0.9445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2007/4 (Sheldrick, 2007)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.153
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1664
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.976
_refine_diff_density_min         -0.604
_refine_diff_density_rms         0.089
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.982
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         7991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.982
_refine_ls_R_factor_all          0.1078
_refine_ls_R_factor_gt           0.0585
_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^)+(0.0843P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1421
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                5097
_reflns_number_total             7991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b904647j.txt
_cod_data_source_block           cbn21fmi
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        4417.7(13)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               7003018