Nickelalactones with an allyl subunit - the effect of penta-coordination on structures and stability.
Freund, Robert R. A.; Görls, Helmar; Langer, Jens; Dalton transactions (Cambridge, England : 2003) 43 (2014) 13988–14000; doi:10.1039/c4dt01863j

data_7032422
_publ_section_title
;
 Nickelalactones with an allyl subunit - the effect of penta-coordination
 on structures and stability.
;
_journal_issue                   37
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              13988
_journal_page_last               14000
_journal_paper_doi               10.1039/c4dt01863j
_journal_volume                  43
_journal_year                    2014
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C16 H26 N2 Ni O2'
_chemical_formula_sum            'C16 H26 N2 Ni O2'
_chemical_formula_weight         337.10
_space_group_IT_number           46
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'I 2 -2a'
_symmetry_space_group_name_H-M   'I m a 2'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   28.090(2)
_cell_length_b                   13.7216(9)
_cell_length_c                   10.9264(7)
_cell_measurement_reflns_used    15012
_cell_measurement_temperature    133(2)
_cell_measurement_theta_max      27.74
_cell_measurement_theta_min      2.63
_cell_volume                     4211.5(5)
_computing_cell_refinement       DENZO
_computing_data_collection       COLLECT
_computing_data_reduction        DENZO
_computing_molecular_graphics    SHELXTL/PC
_computing_publication_material  SHELXL-97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      133(2)
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_device_type  KappaCCD
_diffrn_measurement_method       'phi- + omega-scan'
_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  0.0491
_diffrn_reflns_av_sigmaI/netI    0.0645
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            4286
_diffrn_reflns_theta_full        27.74
_diffrn_reflns_theta_max         27.74
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    0.933
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            brown
_exptl_crystal_density_diffrn    1.063
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1440.0
_exptl_crystal_size_max          0.068
_exptl_crystal_size_mid          0.064
_exptl_crystal_size_min          0.052
_refine_diff_density_max         1.104
_refine_diff_density_min         -1.199
_refine_diff_density_rms         0.126
_refine_ls_abs_structure_details
;
 Flack x determined using 1522 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.097(15)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     192
_refine_ls_number_reflns         4844
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0970
_refine_ls_R_factor_gt           0.0802
_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^)+(0.1050P)^2^+34.6077P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2090
_refine_ls_wR_factor_ref         0.2185
_reflns_number_gt                3643
_reflns_number_total             4286
_reflns_threshold_expression     >2sigma(I)
_cod_duplicate_entry             7031730
_cod_data_source_file            c4dt01863j2.cif
_cod_data_source_block           FO5231
_cod_original_cell_volume        4211.4(5)
_cod_database_code               7032422
_publcif_datablock.id            {cdaa60af-ed14-4996-a03e-657269297004}