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>)copper(II) from synchrotron data
Shin, Jong Won; Kim, Dae-Woong; Kim, Jin Hong; Moon, Dohyun; Acta Crystallographica Section E 71 (2015) 203–205; doi:10.1107/S2056989015001115

data_2240419
_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>)copper(II)
 from synchrotron data
;
_journal_coeditor_code           WM5115
_journal_issue                   2
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              203
_journal_page_last               205
_journal_paper_doi               10.1107/S2056989015001115
_journal_volume                  71
_journal_year                    2015
_chemical_formula_iupac          '[Cu (C6 H4 N O2)2 (C16 H38 N6)]'
_chemical_formula_moiety         'C28 H46 Cu N8 O4'
_chemical_formula_sum            'C28 H46 Cu N8 O4'
_chemical_formula_weight         622.27
_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>)copper(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                81.16(3)
_cell_angle_beta                 87.14(3)
_cell_angle_gamma                86.68(3)
_cell_formula_units_Z            1
_cell_length_a                   8.0490(16)
_cell_length_b                   8.3000(17)
_cell_length_c                   11.175(2)
_cell_measurement_reflns_used    21514
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      33.548
_cell_measurement_theta_min      0.361
_cell_volume                     735.8(3)
_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, 2015b)
;
_computing_structure_solution
;
<i>SHELXT2014/5</i> (Sheldrick, 2015a)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.946
_diffrn_measured_fraction_theta_max 0.932
_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  0.0180
_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            7574
_diffrn_reflns_theta_full        22.210
_diffrn_reflns_theta_max         25.997
_diffrn_reflns_theta_min         2.726
_exptl_absorpt_coefficient_mu    0.572
_exptl_absorpt_correction_T_max  0.983
_exptl_absorpt_correction_T_min  0.958
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
(<i>HKL3000sm SCALEPACK</i>; Otwinowski & Minor, 1997)
;
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.404
_exptl_crystal_description       needle
_exptl_crystal_F_000             331
_exptl_crystal_size_max          0.075
_exptl_crystal_size_mid          0.030
_exptl_crystal_size_min          0.030
_refine_diff_density_max         0.433
_refine_diff_density_min         -0.623
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     188
_refine_ls_number_reflns         3882
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.0327
_refine_ls_R_factor_gt           0.0300
_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^)+(0.0510P)^2^+0.1939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0862
_reflns_number_gt                3608
_reflns_number_total             3882
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            wm5115sup1.cf
_cod_data_source_block           I
_cod_database_code               2240419
_cod_database_fobs_code          2240419
_shelx_estimated_absorpt_t_min   0.958
_shelx_estimated_absorpt_t_max   0.983
_shelx_hkl_checksum              57051
_shelx_res_checksum              50587