“Chiral-at-Metal” Hemilabile Nickel Complexes with a Latent d10-ML2Configuration: Receiving Substrates with Open Arms
Linden, Anthony; Llovera, Ligia; Herrera, Julio; Dorta, Reto; Agrifoglio, Giuseppe; Dorta, Romano; Organometallics 31 (2012) 6162–; doi:10.1021/om300484z

data_4079096
_publ_section_title
;
 &#x201C;Chiral-at-Metal&#x201D; Hemilabile Nickel Complexes with a Latent
 d10-ML2Configuration: Receiving Substrates with Open Arms
;
_journal_issue                   17
_journal_name_full               Organometallics
_journal_page_first              6162
_journal_paper_doi               10.1021/om300484z
_journal_volume                  31
_journal_year                    2012
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C68 H44 N2 Ni O4 P2, 2(C4 H8 O)'
_chemical_formula_sum            'C76 H60 N2 Ni O6 P2'
_chemical_formula_weight         1217.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_Int_Tables_number      146
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             10-06-24
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            9
_cell_length_a                   37.5195(6)
_cell_length_b                   37.5195(6)
_cell_length_c                   13.4940(2)
_cell_measurement_reflns_used    41902
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      27.6
_cell_measurement_theta_min      3.2
_cell_volume                     16450.7(4)
_computing_cell_refinement
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_collection
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_data_reduction
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
;
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2003)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      160(1)
_diffrn_detector                 'Atlas CCD camera on \k goniostat'
_diffrn_detector_area_resol_mean 10.3801
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.938
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans with \k offsets'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_source         'SuperNova (Mo) X-ray Source'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0466
_diffrn_reflns_av_sigmaI/netI    0.0307
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       48
_diffrn_reflns_limit_k_min       -48
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            56708
_diffrn_reflns_theta_full        25.0
_diffrn_reflns_theta_max         27.67
_diffrn_reflns_theta_min         3.26
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.358
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.89382
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.106
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             5724
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;  THF has 40 e, so 6 THF per cavity (around 3-fold axis)
gives 240 e per cavity.  If some THF has left the crystal,
this would be consistent with slight underoccupation of the site.
One THF could be discerned from the peaks, but refined to give
large ADPs.  The other THF could not be discerned readily from
the weak peaks remaining.  Therefore SQUEEZE was employed.
No significant residual e-denity peaks remain.
;
_refine_diff_density_max         0.351
_refine_diff_density_min         -0.282
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.018(6)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     695
_refine_ls_number_reflns         15371
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0359
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0805P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1045
_refine_ls_wR_factor_ref         0.1059
_reflns_number_gt                14304
_reflns_number_total             15371
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om300484z_si_001.cif
_cod_data_source_block           2a
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4079096