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(5-methyltetrazolato-κ<i>N</i>)nickel(II) from synchrotron data
Kim, Dae-Woong; Shin, Jong Won; Kim, Jin Hong; Moon, Dohyun; Acta Crystallographica Section E 71 (2015) 173–175; doi:10.1107/S2056989015000651

data_2240402
_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(5-methyltetrazolato-\k<i>N</i>)nickel(II)
 from synchrotron data
;
_journal_coeditor_code           IS5389
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              173
_journal_page_last               175
_journal_paper_doi               10.1107/S2056989015000651
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (C2 H3 N4)2 (C16 H38 N6)]'
_chemical_formula_moiety         'C20 H44 N14 Ni'
_chemical_formula_sum            'C20 H44 N14 Ni'
_chemical_formula_weight         539.40
_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(5-methyltetrazolato-\k<i>N</i>^2^)nickel(II)
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 98.94(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   24.040(5)
_cell_length_b                   12.923(3)
_cell_length_c                   8.7170(17)
_cell_measurement_reflns_used    25946
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.55
_cell_measurement_theta_min      0.36
_cell_volume                     2675.2(10)
_computing_cell_refinement
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_data_collection
;
<i>PAL ADSC Quantum-210 ADX</i> (Arvai & Nielsen, 1983)
;
_computing_data_reduction
;
<i>HKL3000sm</i> (Otwinowski & Minor, 1997)
;
_computing_molecular_graphics
;
<i>DIAMOND4</i> (Putz & Brandenburg, 2014)
;
_computing_publication_material
;
publCIF (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014/7</i> (Sheldrick, 2008, 2015<i>b</i>)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015<i>a</i>)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.62998
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_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            12808
_diffrn_reflns_theta_full        22.209
_diffrn_reflns_theta_max         25.999
_diffrn_reflns_theta_min         1.590
_exptl_absorpt_coefficient_mu    0.551
_exptl_absorpt_correction_T_max  0.978
_exptl_absorpt_correction_T_min  0.973
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>;  Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            pink
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.040
_exptl_crystal_size_min          0.040
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.788
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.079
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     162
_refine_ls_number_reflns         3761
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.0406
_refine_ls_R_factor_gt           0.0321
_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^)+(0.0565P)^2^+0.1060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0868
_refine_ls_wR_factor_ref         0.0899
_reflns_number_gt                3150
_reflns_number_total             3761
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            is5389sup1.cf
_cod_data_source_block           I
_cod_original_cell_volume        2675.1(9)
_cod_database_code               2240402
_cod_database_fobs_code          2240402
_shelx_estimated_absorpt_t_min   0.973
_shelx_estimated_absorpt_t_max   0.978
_shelx_hkl_checksum              66766
_shelx_res_checksum              41399