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(thiocyanato-κ<i>N</i>)nickel(II) from synchrotron data
Kim, Dae-Woong; Kim, Jong Jin; Shin, Jong Won; Kim, Jin Hong; Moon, Dohyun; Acta Crystallographica Section E 71 (2015) 779–782; doi:10.1107/S205698901501110X

data_2240834
_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(thiocyanato-\k<i>N</i>)nickel(II)
 from synchrotron data
;
_journal_coeditor_code           GK2635
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              779
_journal_page_last               782
_journal_paper_doi               10.1107/S205698901501110X
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Ni (N C S)2 (C16 H38 N6)]'
_chemical_formula_moiety         'C18 H38 N8 Ni S2'
_chemical_formula_sum            'C18 H38 N8 Ni S2'
_chemical_formula_weight         489.39
_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(thiocyanato-\k<i>N</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                94.66(3)
_cell_angle_beta                 97.99(3)
_cell_angle_gamma                110.04(3)
_cell_formula_units_Z            2
_cell_length_a                   8.6610(17)
_cell_length_b                   12.027(2)
_cell_length_c                   12.560(3)
_cell_measurement_reflns_used    49914
_cell_measurement_temperature    180(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     1205.4(5)
_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>DIAMOND</i> (Putz & Brandenburg, 2007)
;
_computing_publication_material
;
<i>publCIF</i> (Westrip, 2010)
;
_computing_structure_refinement
;
<i>SHELXL2014</i> (Sheldrick, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      180(2)
_diffrn_measured_fraction_theta_full 0.951
_diffrn_measured_fraction_theta_max 0.968
_diffrn_measurement_device_type  'ADSC Q210 CCD area-detector'
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.630
_diffrn_reflns_av_R_equivalents  0.0135
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            12812
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         26.000
_diffrn_reflns_theta_min         1.613
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.916
_exptl_absorpt_correction_T_min  0.841
_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    1.348
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.150
_exptl_crystal_size_min          0.125
_refine_diff_density_max         1.584
_refine_diff_density_min         -1.111
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         6583
_refine_ls_number_restraints     11
_refine_ls_restrained_S_all      1.111
_refine_ls_R_factor_all          0.0436
_refine_ls_R_factor_gt           0.0416
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0541P)^2^+0.7946P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1099
_refine_ls_wR_factor_ref         0.1113
_reflns_number_gt                6243
_reflns_number_total             6583
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            gk2635sup1.cf
_cod_data_source_block           I
_cod_database_code               2240834
_cod_database_fobs_code          2240834
_shelx_estimated_absorpt_t_min   0.841
_shelx_estimated_absorpt_t_max   0.916
_shelx_hkl_checksum              67053
_shelx_res_checksum              33637