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_4330700
_publ_section_title
;
 Synthesis of Binucleating Macrocycles and Their Nickel(II) Hydroxo- and
 Cyano-Bridged Complexes with Divalent Ions: Anatomical Variation of
 Ligand Features
;
_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         'C33 H42 N7 Ni O3, C2 H5 O0.5, C4 H12 N'
_chemical_formula_sum            'C39 H59 N8 Ni O3.5'
_chemical_formula_weight         754.65
_chemical_name_common            '{Ni[pyN2N4(Me)2](OH)}, 0.5Et2O, Me4N'
_space_group_IT_number           5
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'C 2y'
_symmetry_space_group_name_H-M   'C 1 2 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
SHELXL-97

This is a racemic twin structure with flack parameter of about 0.50. The
TWIN/BASF commands have been applied in the final refinement.

The main problem of this structure is about the disorder of the fourteen
members ring [14]aneN4-Me2. The whole ring was disorder into two parts with
occupancies of 50/50. Their bond lengths and bond angles were constrained by
using DFIX. The temperature factors of all the atoms were constrained and
avaraged by using DELU/SIMU commands, including the atoms of cation Me4N and
solvate molecule Et2O.

All the hydrogens were added geometrically except for the hydrogen of -OH
group, of which the hydrogen was added by Fourier Map and its bond length
and bond angle was constrained to point to one of phenyl rings of the arm
of structure.
;
_cell_angle_alpha                90.00
_cell_angle_beta                 94.8400(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1014(8)
_cell_length_b                   12.8847(8)
_cell_length_c                   23.4563(15)
_cell_measurement_reflns_used    6705
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.61
_cell_measurement_theta_min      2.34
_cell_volume                     3945.5(4)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0296
_diffrn_reflns_av_sigmaI/netI    0.0344
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            23667
_diffrn_reflns_theta_full        26.39
_diffrn_reflns_theta_max         26.39
_diffrn_reflns_theta_min         1.74
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.540
_exptl_absorpt_correction_T_max  0.9234
_exptl_absorpt_correction_T_min  0.7778
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.270
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1620
_exptl_crystal_size_max          0.49
_exptl_crystal_size_mid          0.49
_exptl_crystal_size_min          0.15
_refine_diff_density_max         0.915
_refine_diff_density_min         -1.091
_refine_diff_density_rms         0.088
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.51(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.060
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     653
_refine_ls_number_reflns         8102
_refine_ls_number_restraints     1278
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0882
_refine_ls_R_factor_gt           0.0701
_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^)+(0.1010P)^2^+16.0959P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1837
_refine_ls_wR_factor_ref         0.2033
_reflns_number_gt                6596
_reflns_number_total             8102
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic301506x_si_002_18.cif
_cod_data_source_block           compound26
_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_formula_sum        'C39 H59 N8 Ni O3.50'
_cod_database_code               4330700