“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_4079099
_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         'C77 H52 N2 Ni O4 P2, C4 H10 O, C6 H6'
_chemical_formula_sum            'C87 H68 N2 Ni O5 P2'
_chemical_formula_weight         1342.15
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_date             12-Jan-2012
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5470(3)
_cell_length_b                   22.4042(5)
_cell_length_c                   25.2593(6)
_cell_measurement_reflns_used    15269
_cell_measurement_temperature    160(1)
_cell_measurement_theta_max      27.3229
_cell_measurement_theta_min      1.9847
_cell_volume                     7100.5(3)
_computing_cell_refinement
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_data_collection
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_data_reduction
'CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)'
_computing_molecular_graphics    'ORTEPII (Johnson, 1976)'
_computing_publication_material  'SHELXL97 and PLATON (Spek, 2009)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_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 0.999
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type
'Oxford Diffraction SuperNova, dual radiation diffractometer'
_diffrn_measurement_method       '\w scans'
_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  0.0570
_diffrn_reflns_av_sigmaI/netI    0.0678
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            39344
_diffrn_reflns_theta_full        25.01
_diffrn_reflns_theta_max         27.38
_diffrn_reflns_theta_min         1.99
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.374
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.66932
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
CrysAlisPro, Version 1.171.35.19 (Agilent Technologies, 2011)
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.255
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2808
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;
The C6D6 molecule could not be modelled adequately, so the SQUEEZE routine 
of the program PLATON was employed.  When the C6D6 molecule is omitted 
from the model, each unit cell contains two cavities of 565 \%A^3^.  The 
electron count in each cavity was calculated to be approximately 70 e, which 
is a little less than two molecules of C6D6 (42 e) per cavity.  It is 
assumed there is one molecule of C6D6 per asymmetric unit and this 
assumption was used in the subsequent calculation of the empirical formula, 
formula weight, density, linear absorption coefficient and F(000).   Based 
on the assumption, the ratio of Ni-complex molecules to Et2O and C6D6 
molecules in the structure is 1:1:1.
;
_refine_diff_density_max         1.162
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   -0.020(12)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.046
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     906
_refine_ls_number_reflns         14458
_refine_ls_number_restraints     266
_refine_ls_restrained_S_all      1.042
_refine_ls_R_factor_all          0.0720
_refine_ls_R_factor_gt           0.0548
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0818P)^2^+0.8996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1407
_refine_ls_wR_factor_ref         0.1505
_reflns_number_gt                11500
_reflns_number_total             14458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            om300484z_si_001.cif
_cod_data_source_block           10
_cod_database_code               4079099