Reactions of the Terminal NiII-OH Group in Substitution and Electrophilic Reactions with Carbon Dioxide and Other Substrates: Structural Definition of Binding Modes in an Intramolecular NiII...FeII Bridged Site
Deguang Huang; R. H. Holm; Journal of the American Chemical Society 132 (2010) 4693–4701; doi:10.1021/ja1003125

data_4102201
_publ_section_title
;
 Reactions of the Terminal NiII-OH Group in Substitution and Electrophilic
 Reactions with Carbon Dioxide and Other Substrates: Structural Definition
 of Binding Modes in an Intramolecular NiII...FeII Bridged Site
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4693
_journal_page_last               4701
_journal_paper_doi               10.1021/ja1003125
_journal_volume                  132
_journal_year                    2010
_chemical_formula_moiety         'C28 H33 N6 Ni O3, C8 H20 N'
_chemical_formula_sum            'C36 H53 N7 Ni O3'
_chemical_formula_weight         690.56
_chemical_name_common            (Et4N)[Ni(PyN2dien(Me3))OH]
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

This data was obtained from a crappy crystal at 153K.

A definition of whole molecule as a two-set disordered model (50/50) was
tried, but the following refinement of that model gave worse result
than the model presented here, in which only the atoms on triamine chain
and atoms of Et4N+ were treated as a two-set disordered model (50/50).
All the temperature factors of atoms in this model were evened out by using
commands DELU & SIMU. All the non-hydrogen atoms were anisotroped.

The cation Et4N+ was not added hydrogen atoms due to its high symmetry
and the disordered ethylene carbon atoms on it, but these hydrogen atoms
were included in the reported formula.

The constraint of disordered model and temperature factors of their atoms
influenced the ratio of Maximum/Minimum Residual Density, but it is still
acceptable.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   25.599(7)
_cell_length_b                   14.354(4)
_cell_length_c                   9.927(3)
_cell_measurement_reflns_used    7411
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.85
_cell_measurement_theta_min      2.20
_cell_volume                     3647.7(18)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega 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  0.0609
_diffrn_reflns_av_sigmaI/netI    0.0349
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            29639
_diffrn_reflns_theta_full        25.97
_diffrn_reflns_theta_max         25.97
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.576
_exptl_absorpt_correction_T_max  0.9447
_exptl_absorpt_correction_T_min  0.8554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.257
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1480
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.788
_refine_diff_density_min         -0.704
_refine_diff_density_rms         0.106
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.067
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     283
_refine_ls_number_reflns         3696
_refine_ls_number_restraints     224
_refine_ls_restrained_S_all      1.178
_refine_ls_R_factor_all          0.0896
_refine_ls_R_factor_gt           0.0787
_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^)+(0.1483P)^2^+5.0425P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2189
_refine_ls_wR_factor_ref         0.2362
_reflns_number_gt                3039
_reflns_number_total             3696
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja1003125_si_009.cif
_cod_data_source_block           Compound14
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_cell_volume        3647.8(17)
_cod_original_sg_symbol_Hall     -P2ac2n
_cod_database_code               4102201