Preparation of η(2)-complexes of fullerenes by reduction. Crystal structure and optical properties of {Ni(dppp)·(η(2)-C(70))}·(C(6)H(4)Cl(2))(0.5).
Konarev, Dmitri V.; Simonov, Sergey V.; Khasanov, Salavat S.; Lyubovskaya, Rimma N.; Dalton transactions (Cambridge, England : 2003) 40 (2011) 9176–9179; doi:10.1039/c1dt10839e

data_7016552
_publ_section_title
;
 Preparation of \h(2)-complexes of fullerenes by reduction. Crystal
 structure and optical properties of
 {Ni(dppp)&#x00B7;(\h(2)-C(70))}&#x00B7;(C(6)H(4)Cl(2))(0.5).
;
_journal_issue                   36
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9176
_journal_page_last               9179
_journal_paper_doi               10.1039/c1dt10839e
_journal_volume                  40
_journal_year                    2011
_chemical_formula_moiety         'C70, C27 H26 Ni P2, 0.5(C6 H4 Cl2)'
_chemical_formula_sum            'C100 H28 Cl Ni P2'
_chemical_formula_weight         1385.32
_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                100.191(4)
_cell_angle_beta                 97.361(4)
_cell_angle_gamma                97.999(4)
_cell_formula_units_Z            2
_cell_length_a                   10.5609(6)
_cell_length_b                   14.0596(7)
_cell_length_c                   19.888(1)
_cell_measurement_reflns_used    16023
_cell_measurement_temperature    130(1)
_cell_measurement_theta_max      31.1926
_cell_measurement_theta_min      1.4892
_cell_volume                     2842.6(3)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution
;
SIR 2004 : An improved tool for crystal structure determination and refinement
Burla, M.C., Camalli, M., Carrozzini, B., Cascarano, G.L., Giacovazzo,
C., Polidori, G. & Spagna, R. (2003). J. Appl. Cryst., 36, 1103
;
_diffrn_ambient_temperature      130(1)
_diffrn_detector_area_resol_mean 10.4752
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.860
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0534
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            33893
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         31.26
_diffrn_reflns_theta_min         1.49
_exptl_absorpt_coefficient_mu    0.509
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69388
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.34.46 (release 25-11-2010 CrysAlis171 .NET)
(compiled Nov 25 2010,17:55:46)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.619
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       pike
_exptl_crystal_F_000             1406
_exptl_crystal_size_max          0.17
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.12
_refine_diff_density_max         0.875
_refine_diff_density_min         -0.963
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     926
_refine_ls_number_reflns         15949
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0700
_refine_ls_R_factor_gt           0.0558
_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^)+(0.0802P)^2^+2.3791P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1431
_refine_ls_wR_factor_ref         0.1530
_reflns_number_gt                13129
_reflns_number_total             15949
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            c1dt10839e.txt
_cod_data_source_block           C70_Ni(dppp)_(DCB)_130K
_cod_database_code               7016552