Synthesis of Binucleating Macrocycles and Their Nickel(II) Hydroxo- and Cyano-Bridged Complexes with Divalent Ions: Anatomical Variation of Ligand Features
Xiaofeng Zhang; Deguang Huang; Yu-Sheng Chen; R. H. Holm; Inorganic Chemistry 51 (2012) 11017–11029; doi:10.1021/ic301506x

data_4330694
_publ_section_title
;
 Synthesis of Binucleating Macrocycles and Their Nickel(II) Hydroxo- and
 Cyano-Bridged Complexes with Divalent Ions: Anatomical Variation of
 Ligand Features
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              11017
_journal_page_last               11029
_journal_paper_doi               10.1021/ic301506x
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         C28H32N6NiO2,C8H20N,CF3O3S,C3H7NO
_chemical_formula_sum            'C40 H59 F3 N8 Ni O6 S'
_chemical_formula_weight         895.72
_chemical_name_common            '[Ni(H2pyN2dien(Me3))] (Et4N)(OTf) DMF'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

In the main structure, three carbon atoms on the dien(Me3) chain were treated
as diordered model into two positions with occupancies of 70/30. The refinement
of this model gave good result without any constraint on the atoms.
No disorder work was required on the Et4N cation.

The solvate DMF molecule was NOT treated as disordered model, because short
intermolecular contact would  be generated when atoms were disordered.
Fortunately, constraint of temperature factor of all the DMF atoms with
DELU/SIMU gave acceptable result.

The CF3SO3 anion was disordered into two positions with occupancies
of 55/45 and the temperature factors of all its atoms were restrained by using
command DELU/SIMU. The following refinement gave good ellipsoid plot.

The final model of this structure was well accepted by CIFcheck program.
;
_cell_angle_alpha                76.443(2)
_cell_angle_beta                 80.907(2)
_cell_angle_gamma                61.410(2)
_cell_formula_units_Z            2
_cell_length_a                   12.4478(19)
_cell_length_b                   13.120(2)
_cell_length_c                   15.302(2)
_cell_measurement_reflns_used    10252
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      26.11
_cell_measurement_theta_min      2.26
_cell_volume                     2130.1(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  0.0344
_diffrn_reflns_av_sigmaI/netI    0.0322
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            33926
_diffrn_reflns_theta_full        26.53
_diffrn_reflns_theta_max         26.53
_diffrn_reflns_theta_min         1.87
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.573
_exptl_absorpt_correction_T_max  0.9449
_exptl_absorpt_correction_T_min  0.7625
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             948
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.34
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.285
_refine_diff_density_min         -0.781
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     597
_refine_ls_number_reflns         8821
_refine_ls_number_restraints     289
_refine_ls_restrained_S_all      1.078
_refine_ls_R_factor_all          0.0774
_refine_ls_R_factor_gt           0.0646
_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^)+(0.1011P)^2^+4.2821P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1780
_refine_ls_wR_factor_ref         0.1899
_reflns_number_gt                7270
_reflns_number_total             8821
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301506x_si_002_12.cif
_cod_data_source_block           compound20
_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        2130.0(6)
_cod_database_code               4330694