Synthesis and Structures of 9-Nickelafluorenyllithium Complexes
Buchalski, Piotr; Grabowska, Ilona; Kamińska, Elżbieta; Suwińska, Kinga; Organometallics 27 (2008) 2346–; doi:10.1021/om701275u

data_4071117
_publ_section_title
;
 Synthesis and Structures of 9-Nickelafluorenyllithium Complexes
;
_journal_issue                   10
_journal_name_full               Organometallics
_journal_page_first              2346
_journal_paper_doi               10.1021/om701275u
_journal_volume                  27
_journal_year                    2008
_chemical_formula_sum            'C31 H48 Li Ni O7'
_chemical_formula_weight         598.34
_chemical_name_common            Pw16
_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                 98.85(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   31.21(3)
_cell_length_b                   11.851(7)
_cell_length_c                   17.44(2)
_cell_measurement_reflns_used    10253
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      23.257
_cell_measurement_theta_min      2.910
_cell_volume                     6374(10)
_computing_cell_refinement       'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_data_collection
'Collect data collection software (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo and Scalepak (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'ORTEP-3 (Johnson & Burnet, 1996)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 9.1
_diffrn_measured_fraction_theta_full 0.959
_diffrn_measured_fraction_theta_max 0.959
_diffrn_measurement_device_type  KappaCCD
_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  0.115
_diffrn_reflns_av_sigmaI/netI    0.1847
_diffrn_reflns_limit_h_max       36
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            47962
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.92
_exptl_absorpt_coefficient_mu    0.651
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9087
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'deep red'
_exptl_crystal_density_diffrn    1.247
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             2568
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.699
_refine_diff_density_min         -0.825
_refine_diff_density_rms         0.106
_refine_ls_extinction_coef       0.00138(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.935
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     735
_refine_ls_number_reflns         10745
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.935
_refine_ls_R_factor_all          0.1719
_refine_ls_R_factor_gt           0.0618
_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^)+(0.0785P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1328
_refine_ls_wR_factor_ref         0.1746
_reflns_number_gt                4692
_reflns_number_total             10745
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            om701275u-file003.cif
_cod_data_source_block           compound_(2)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4071117