Remarkable Inertness of Copper(II) Chelates of Cyclen-Based Macrobicycles with Two trans-N-Acetate Arms
Catarina V. Esteves; Pedro Lamosa; Rita Delgado; Judite Costa; Pauline Désogère; Yoann Rousselin; Christine Goze; Franck Denat; Inorganic Chemistry 52 (2013) 5138–5153; doi:10.1021/ic400015v

data_4334643
_publ_contact_author_address
;
Institut de Chimie Molculaire de lUniversit de Bourgogne
UMR CNRS 6302
Universit de Bourgogne
9, Av. Alain Savary
21078 Dijon
France
;
_publ_contact_author_email       Yoann.Rousselin@u-bourgogne.fr
_publ_contact_author_fax         '+33 (0)3 80 39 38 35'
_publ_contact_author_name        'Yoann Rousselin'
_publ_contact_author_phone       '+33 (0)3 80 39 38 35'
_publ_section_title
;
 Remarkable Inertness of Copper(II) Chelates of Cyclen-Based Macrobicycles
 with Two trans-N-Acetate Arms
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5138
_journal_page_last               5153
_journal_paper_doi               10.1021/ic400015v
_journal_volume                  52
_journal_year                    2013
_chemical_formula_moiety         '2(C26 H32 Cu N4 O5), 7(H2 O)'
_chemical_formula_sum            'C52 H78 Cu2 N8 O17'
_chemical_formula_weight         1214.30
_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   mixed
_audit_creation_date             2013-02-13
_audit_creation_method
;
  Olex2 1.2
  (compiled 2012.12.05 svn.r2549, GUI svn.r4385)
;
_audit_update_record
;
2012-10-25 # Formatted by publCIF
;
_cell_angle_alpha                90
_cell_angle_beta                 94.425(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   9.6023(4)
_cell_length_b                   16.4735(6)
_cell_length_c                   33.8442(14)
_cell_measurement_reflns_used    4330
_cell_measurement_temperature    115(2)
_cell_measurement_theta_max      24.4353
_cell_measurement_theta_min      2.4143
_cell_volume                     5337.6(4)
_computing_cell_refinement       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_collection       'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_data_reduction        'SAINT V8.27B (Bruker AXS Inc., 2012)'
_computing_molecular_graphics
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_publication_material
;
O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann,
OLEX2: a complete structure solution, refinement and analysis program.
J. Appl. Cryst. (2009). 42, 339-341.
;
_computing_structure_refinement
;
SHELXL, G.M. Sheldrick, Acta Cryst.
(2008). A64, 112-122
;
_computing_structure_solution
'SHELXS-97, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122'
_diffrn_ambient_temperature      115
_diffrn_detector                 'CCD Plate'
_diffrn_detector_area_resol_mean 9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Nonius Kappa Apex II'
_diffrn_measurement_method       'CCD rotation images, thick slices'
_diffrn_radiation_collimation    '0.6 mm'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a~1~'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_xray_symbol    K-L~3~
_diffrn_reflns_av_R_equivalents  0.0751
_diffrn_reflns_av_unetI/netI     0.0680
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       44
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            31174
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.574
_diffrn_reflns_theta_min         2.545
_diffrn_source                   'x-ray tube'
_diffrn_source_target            Mo
_diffrn_source_type              'Siemens KFF Mo 2K-180'
_exptl_absorpt_coefficient_mu    0.878
_exptl_absorpt_correction_T_max  0.74
_exptl_absorpt_correction_T_min  0.66
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            'clear light blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.511
_exptl_crystal_description       prism
_exptl_crystal_F_000             2560
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.513
_refine_diff_density_min         -0.439
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6164
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0789
_refine_ls_R_factor_gt           0.0425
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 w=1/[\s^2^(Fo^2^)+(0.0342P)^2^+5.7136P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0779
_refine_ls_wR_factor_ref         0.0876
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4316
_reflns_number_total             6164
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic400015v_si_003.cif
_cod_data_source_block           13fd1102
_cod_database_code               4334643
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  {H9A,H9B} of C9, {H6A,H6B} of C6, H17 of C17, {H4A,H4B} of C4, {H8A,H8B} of
  C8, {H24A,H24B} of C24, {H11A,H11B} of C11, H14 of C14, H20 of C20, {H3A,H3B}
  of C3, {H22A,H22B} of C22, {H7A,H7B} of C7, {H1A,H1B} of C1, H1AA of C1A,
  H1BA of C1B, H19 of C19, {H2A,H2B} of C2, {H12A,H12B} of C12, H18 of C18, H13
  of C13
 At 1.5 times of:
  {H8C,H8D} of O8, {H9C,H9D} of O9, {H7C,H7D} of O7, {H6C,H6BB,H6AA} of O6
2. Restrained distances
 O6-H6C
 0.87 with sigma of 0.02
 H7E-O7
 0.87 with sigma of 0.02
3. others
 Fixed Sof: H6C(0.5) H6BB(0.5) H7C(0.5) O8(0.5) H8C(0.5) H8D(0.5) H7E(0.5)
4.a Free rotating group:
 O6(H6C,H6BB,H6AA), O7(H7C,H7D), O8(H8C,H8D), O9(H9C,H9D)
4.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C6(H6A,H6B), C7(H7A,H7B),
 C8(H8A,H8B), C9(H9A,H9B), C11(H11A,H11B), C12(H12A,H12B), C22(H22A,H22B),
 C24(H24A,H24B)
4.c Aromatic/amide H refined with riding coordinates:
 C1A(H1AA), C1B(H1BA), C13(H13), C14(H14), C17(H17), C18(H18), C19(H19),
 C20(H20)
;
_shelx_estimated_absorpt_t_max   0.957
_shelx_estimated_absorpt_t_min   0.917
_shelx_res_checksum              7020
_shelxl_version_number           2012-9