Cyclopentadiene Alkylation and Nickel Complexes with Tri-, Tetra-, or Pentaisopropylcyclopentadienide or an Even Bulkier Lithium Alkylcyclopentadienide
Weismann, Daniel; Saurenz, Dirk; Boese, Roland; Bläser, Dieter; Wolmershäuser, Gotthelf; Sun, Yu; Sitzmann, Helmut; Organometallics 30 (2011) 6351–; doi:10.1021/om200372j

data_4064863
_publ_section_title
;
 Cyclopentadiene Alkylation and Nickel Complexes with Tri-, Tetra-, or
 Pentaisopropylcyclopentadienide or an Even Bulkier Lithium
 Alkylcyclopentadienide
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              6351
_journal_paper_doi               10.1021/om200372j
_journal_volume                  30
_journal_year                    2011
_chemical_formula_sum            'C42 H67 Ni2 O2'
_chemical_formula_weight         721.38
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                74.631(10)
_cell_angle_beta                 87.691(10)
_cell_angle_gamma                76.631(10)
_cell_formula_units_Z            2
_cell_length_a                   10.0100(9)
_cell_length_b                   12.6008(11)
_cell_length_c                   17.1516(15)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      2.05
_cell_volume                     2029.0(3)
_computing_cell_refinement       'Stoe IPDS V2.63'
_computing_data_collection       'Stoe IPDS V2.63'
_computing_data_reduction        'Stoe IPDS V2.63'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Giacovazzo et al., 1993)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_diffrn_measurement_device       'Stoe IPDS'
_diffrn_measurement_method       'Phi- Rotation'
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0505
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            29318
_diffrn_reflns_theta_full        26.02
_diffrn_reflns_theta_max         26.02
_diffrn_reflns_theta_min         2.61
_exptl_absorpt_coefficient_mu    0.959
_exptl_absorpt_correction_T_max  0.89363
_exptl_absorpt_correction_T_min  0.73021
_exptl_absorpt_correction_type   'analytical (ABST/PLATON 98)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.181
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent plate'
_exptl_crystal_F_000             782
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.32
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.551
_refine_diff_density_min         -0.389
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.882
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     443
_refine_ls_number_reflns         7483
_refine_ls_number_restraints     24
_refine_ls_restrained_S_all      0.882
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0401
_refine_ls_shift/su_max          0.032
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0937
_refine_ls_wR_factor_ref         0.1032
_reflns_number_gt                4792
_reflns_number_total             7483
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om200372j_si_004.cif
_cod_data_source_block           2008
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
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_values 1715 2011-07-08 13:25:40Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0600P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               4064863