Homoleptic Permethylpentalene Complexes: "Double Metallocenes" of the First-Row Transition Metals
Andrew E. Ashley; Robert T. Cooper; Gregory G. Wildgoose; Jennifer C. Green; Dermot O'Hare; Journal of the American Chemical Society 130 (2008) 15662–15677; doi:10.1021/ja8057138

data_4108680
_publ_contact_author_address
;
Chemistry Research Laboratory,
University of Oxford,
Mansfield Road, 
Oxford OX1 3TA. UK.
;
_publ_contact_author_email       dermot.ohare@chem.ox.ac.uk
_publ_contact_author_name        'Dermot O'Hare'
_publ_section_title
;
 Homoleptic Permethylpentalene Complexes: "Double Metallocenes" of the
 First-Row Transition Metals
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              15662
_journal_page_last               15677
_journal_paper_doi               10.1021/ja8057138
_journal_volume                  130
_journal_year                    2008
_chemical_formula_moiety         'C28 H36 Ni2'
_chemical_formula_sum            'C28 H36 Ni2'
_chemical_formula_weight         490.01
_chemical_name_systematic        Bis(permethylpentalene)dinickel(II)
_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'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_audit_creation_date             07-12-17
_audit_creation_method           CRYSTALS_ver_12.85
_cell_angle_alpha                90
_cell_angle_beta                 108.6695(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.6285(3)
_cell_length_b                   12.3192(4)
_cell_length_c                   10.2589(4)
_cell_measurement_reflns_used    2292
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1152.83(7)
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_collection       'COLLECT (Nonius, 1997-2001).'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.976
_diffrn_measurement_device       'Nonius KappaCCD'
_diffrn_measurement_device_type  Area
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.041
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            7694
_diffrn_reflns_theta_full        25.826
_diffrn_reflns_theta_max         27.474
_diffrn_reflns_theta_min         5.249
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.645
_exptl_absorpt_correction_T_max  0.93
_exptl_absorpt_correction_T_min  0.88
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.412
_exptl_crystal_description       block
_exptl_crystal_F_000             520
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.27
_refine_diff_density_min         -0.31
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.9948
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     136
_refine_ls_number_reflns         1831
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0554
_refine_ls_R_factor_gt           0.0346
_refine_ls_shift/su_max          0.000881
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[\s^2^(F^2^) + ( 0.02P)^2^ + 1.08P] 
 ,where P=(max(Fo^2^,0) + 2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0769
_refine_ls_wR_factor_gt          0.0665
_refine_ls_wR_factor_ref         0.0638
_reflns_limit_h_max              11
_reflns_limit_h_min              -12
_reflns_limit_k_max              15
_reflns_limit_k_min              0
_reflns_limit_l_max              13
_reflns_limit_l_min              0
_reflns_number_gt                1968
_reflns_number_total             2576
_reflns_threshold_expression     I>2.0\s(I)
_oxford_diffrn_Wilson_B_factor   1.59
_oxford_diffrn_Wilson_scale      9.75
_oxford_refine_ls_r_factor_ref   0.0307
_oxford_refine_ls_scale          0.3110(3)
_oxford_reflns_number_all        2576
_oxford_reflns_threshold_expression_ref I>3.0\s(I)
_cod_data_source_file            ja8057138_si_002_1.cif
_cod_data_source_block           5
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               4108680