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_4064865
_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            'C30 H42 Br N Ni'
_chemical_formula_weight         555.27
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           9
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 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                 100.440(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            16
_cell_length_a                   17.5710(6)
_cell_length_b                   17.2638(8)
_cell_length_c                   37.9120(25)
_cell_measurement_reflns_used    5581
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      62.8726
_cell_measurement_theta_min      3.6191
_cell_volume                     11309.9(10)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 16.1399
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type
'Goniometer Xcalibur, detector: Sapphire3 (Gemini ultra Cu)'
_diffrn_measurement_method       '\w and \p scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'Enhance Ultra (Cu) X-ray Source'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0846
_diffrn_reflns_av_sigmaI/netI    0.0852
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -43
_diffrn_reflns_number            55373
_diffrn_reflns_theta_full        63.25
_diffrn_reflns_theta_max         63.25
_diffrn_reflns_theta_min         3.62
_exptl_absorpt_coefficient_mu    2.753
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.64007
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET)
(compiled Feb 27 2009,15:38:38)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.304
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       'transparent block'
_exptl_crystal_F_000             4672
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.04
_refine_diff_density_max         1.936
_refine_diff_density_min         -0.561
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.79(2)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.945
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1230
_refine_ls_number_reflns         16507
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.944
_refine_ls_R_factor_all          0.0812
_refine_ls_R_factor_gt           0.0529
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0727P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1278
_refine_ls_wR_factor_ref         0.1387
_reflns_number_gt                11290
_reflns_number_total             16507
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om200372j_si_006.cif
_cod_data_source_block           09174o
_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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_sg_symbol_H-M      'C c'
_cod_database_code               4064865