Fast Carbon Dioxide Fixation by 2,6-Pyridinedicarboxamidato-nickel(II)-hydroxide Complexes: Influence of Changes in Reactive Site Environment on Reaction Rates
Deguang Huang; Olga V. Makhlynets; Lay Ling Tan; Sonny C. Lee; Elena V. Rybak-Akimova; R. H. Holm; Inorganic Chemistry 50 (2011) 10070–10081; doi:10.1021/ic200942u

data_4326483
_publ_section_title
;
 Fast Carbon Dioxide Fixation by
 2,6-Pyridinedicarboxamidato-nickel(II)-hydroxide Complexes: Influence of
 Changes in Reactive Site Environment on Reaction Rates
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              10070
_journal_page_last               10081
_journal_paper_doi               10.1021/ic200942u
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C32 H38 N3 Ni O5, C8 H20 N'
_chemical_formula_sum            'C40 H58 N4 Ni O5'
_chemical_formula_weight         733.61
_chemical_name_common            (Et4N)[Ni(pyN2iPr2)(HCO3)]
_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

Some atoms on main part of this structure were treated as disordered two
positions such as the two methyl atoms on iPr groups and the four atoms on
HCO3- group. All the atoms on Et4N+ were disordered into two position
except for the N atom which happened to locate on the symmetrical mirror
with an occupancy of 0.5. The bond lengths and bond angles of these disordered
atoms were not constrained, but they were all restrained by commands DELU
and SIMU for a aim to have their anisotropic displacement parameters along
chemical bonds evened in magnitude.

Hydrogen addition was not applied to the disordered Et4N+ since their positions
were highly disordered as same as the hydrogen on HCO3- group, but they have
been counted in the reported formula.

All the non-hydrogen atoms were refined anisotropically and the final model
gave satisfied result from CIFcheck program.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   22.6785(16)
_cell_length_b                   11.6237(8)
_cell_length_c                   14.9172(10)
_cell_measurement_reflns_used    7702
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.67
_cell_measurement_theta_min      2.22
_cell_volume                     3932.3(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_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      100(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w 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  0.0403
_diffrn_reflns_av_sigmaI/netI    0.0220
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            33850
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.9380
_exptl_absorpt_correction_T_min  0.8462
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1576
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.029
_refine_diff_density_min         -1.600
_refine_diff_density_rms         0.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4217
_refine_ls_number_restraints     438
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0951
_refine_ls_R_factor_gt           0.0798
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1459P)^2^+8.7914P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2290
_refine_ls_wR_factor_ref         0.2498
_reflns_number_gt                3351
_reflns_number_total             4217
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic200942u_si_001_6.cif
_cod_data_source_block           Compound9
_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 
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_cod_database_code               4326483