Copper(II) complexes of pentadentate 17-membered macrocyclic diamidodiamines with N, O or S as additional donors
Herman, Gerrit G.; Lippens, Werner; Goeminne, Andre M.; Steenland, Mathieu; Blaton, Norbert M.; Acta Crystallographica Section C 59 (2003) m294–m298; doi:10.1107/S0108270102023247

data_2013483
_publ_section_title
;
 Copper(II) complexes of pentadentate 17-membered macrocyclic
 diamidodiamines with N, O or S as additional donors
;
_journal_issue                   7
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m294
_journal_page_last               m298
_journal_paper_doi               10.1107/S0108270102023247
_journal_volume                  59
_journal_year                    2003
_chemical_formula_iupac          '[Cu (C12 H22 N4 O2 S)] , 3H2 O'
_chemical_formula_moiety         'C12 H22 Cu N4 O2 S , 3H2 O'
_chemical_formula_sum            'C12 H28 Cu N4 O5 S'
_chemical_formula_weight         403.98
_chemical_name_systematic
;
(3,16-dioxo-1-thia-4,8,11,15-tetraazacycloheptadecanato)copper(II) trihydrate
;
_space_group_IT_number           11
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yb'
_symmetry_space_group_name_H-M   'P 1 21/m 1'
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 107.553(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.4905(6)
_cell_length_b                   16.1160(9)
_cell_length_c                   7.6404(4)
_cell_measurement_reflns_used    38
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      56.033
_cell_measurement_theta_min      22.021
_cell_volume                     879.38(10)
_computing_cell_refinement       XSCANS
_computing_data_collection       'XSCANS (Siemens, 1996)'
_computing_data_reduction        'REDUCE in XSCANS'
_computing_molecular_graphics    'DIAMOND (Bergerhoff, 1996)'
_computing_publication_material  'WinGX (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_measurement_device_type  'Siemens P4 four-circle'
_diffrn_measurement_method       \w/2\q
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0498
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2013
_diffrn_reflns_theta_max         68.87
_diffrn_standards_decay_%        3
_diffrn_standards_interval_count 100
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.127
_exptl_absorpt_correction_T_max  0.645
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_type   '\y scan'
_exptl_absorpt_process_details   '(XEMP; Siemens, 1989)'
_exptl_crystal_colour            'dark blue'
_exptl_crystal_density_diffrn    1.526
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             426
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.41
_refine_diff_density_min         -0.609
_refine_ls_extinction_coef       0.0022(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL97
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     119
_refine_ls_number_reflns         1536
_refine_ls_R_factor_all          0.0502
_refine_ls_R_factor_gt           0.047
_refine_ls_shift/su_max          0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w = 1/[\s^2^(Fo^2^)+(0.0756P)^2^+0.7615P] where P = (Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1297
_refine_ls_wR_factor_ref         0.1328
_reflns_number_gt                1415
_reflns_number_total             1536
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            na1585.cif
_cod_data_source_block           III
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               2013483
_cod_database_fobs_code          2013483