Crystal structure of <i>trans</i>-(1,8-dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-κ^4^<i>N</i>^3^,<i>N</i>^6^,<i>N</i>^10^,<i>N</i>^13^)bis(isonicotinato-κ<i>O</i>)nickel(II) determined from synchrotron data
Shin, Jong Won; Kim, Dae-Woong; Moon, Dohyun; Acta Crystallographica Section E 72 (2016) 223–225; doi:10.1107/S2056989016001031

data_2241520
_publ_section_title
;
 Crystal structure of
 <i>trans</i>-(1,8-dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-\k^4^<i>N</i>^3^,<i>N</i>^6^,<i>N</i>^10^,<i>N</i>^13^)bis(isonicotinato-\k<i>O</i>)nickel(II)
 determined from synchrotron data
;
_journal_coeditor_code           WM5263
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              223
_journal_page_last               225
_journal_paper_doi               10.1107/S2056989016001031
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac          '[Ni (C6 H4 N O2)2 (C16 H38 N6)]'
_chemical_formula_moiety         'C28 H46 N8 Ni O4'
_chemical_formula_sum            'C28 H46 N8 Ni O4'
_chemical_formula_weight         617.44
_chemical_name_systematic
<i>trans</i>-(1,8-Dibutyl-1,3,6,8,10,13-hexaazacyclotetradecane-\k^4^<i>N</i>^3^,<i>N</i>^6^,<i>N</i>^10^,<i>N</i>^13^)bis(isonicotinato-\k<i>O</i>)nickel(II)
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                80.52(3)
_cell_angle_beta                 88.26(3)
_cell_angle_gamma                86.44(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0630(16)
_cell_length_b                   8.5110(17)
_cell_length_c                   10.927(2)
_cell_measurement_reflns_used    20128
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.547
_cell_measurement_theta_min      0.361
_cell_volume                     738.0(3)
_computing_cell_refinement
;
<i>HKL3000SM</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL BL2D-SMDC</i> (Shin <i>et al</i>., 2016<i>a</i>)
;
_computing_data_reduction
;
<i>HKL3000SM</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.931
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0231
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            7634
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.998
_diffrn_reflns_theta_min         2.504
_exptl_absorpt_coefficient_mu    0.510
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.995
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000SM SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            'pale pink'
_exptl_crystal_density_diffrn    1.389
_exptl_crystal_description       needle
_exptl_crystal_F_000             330
_exptl_crystal_size_max          0.009
_exptl_crystal_size_mid          0.004
_exptl_crystal_size_min          0.004
_refine_diff_density_max         1.117
_refine_diff_density_min         -0.946
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3879
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_R_factor_all          0.0499
_refine_ls_R_factor_gt           0.0404
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0649P)^2^+0.1918P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1050
_refine_ls_wR_factor_ref         0.1099
_reflns_number_gt                3326
_reflns_number_total             3879
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            wm5263sup1.cif
_cod_data_source_block           I
_cod_database_code               2241520
_cod_database_fobs_code          2241520
_shelx_estimated_absorpt_t_min   0.995
_shelx_estimated_absorpt_t_max   0.998
_shelx_hkl_checksum              7826
_shelx_res_checksum              48993