Copper(ii) and zinc(ii) complexation with N-ethylene hydroxycyclams and consequences on the macrocyclic backbone configuration
AlHaddad, Nancy; Lelong, Evan; Suh, Jong-Min; Cordier, Marie; Lim, Mi Hee; Royal, Guy; Platas-Iglesias, Carlos; Bernard, Hélène; Tripier, Raphaël; Dalton Transactions  (2022) –; doi:10.1039/D2DT00941B

data_7710355
_publ_section_title
;
 Copper(ii) and zinc(ii) complexation with N-ethylene hydroxycyclams and
 consequences on the macrocyclic backbone configuration
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT00941B
_journal_year                    2022
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C12 H31 Cl2 Cu N4 O2.50'
_chemical_formula_sum            'C12 H31 Cl2 Cu N4 O2.5'
_chemical_formula_weight         405.85
_chemical_name_common            Cu(TE1EtOH)
_chemical_name_systematic
'Copper(II) 2-(1,4,8,11-tetraazacyclotetradecan-1-yl)ethan-1-ol dichloride'
_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'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
_audit_update_record
;
2021-11-17 deposited with the CCDC.	2022-05-18 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 105.052(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   17.5231(10)
_cell_length_b                   9.0433(5)
_cell_length_c                   23.9772(13)
_cell_measurement_reflns_used    9907
_cell_measurement_temperature    150
_cell_measurement_theta_max      27.4805
_cell_measurement_theta_min      2.4072
_cell_measurement_wavelength     0.710730
_cell_volume                     3669.2(4)
_computing_cell_refinement       'APEX3 (Bruker, 2015)'
_computing_data_collection       'SAINT (Bruker, 2014)'
_computing_data_reduction        'SAINT (Bruker, 2014)'
_computing_molecular_graphics
'PLATON, A.L.Spek, Acta Cryst. 2009, D65, 148-155'
_computing_publication_material
'CRYSCALC (T. Roisnel, local program, ver. 2020)'
_computing_structure_refinement  'SHELXL-2018_3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT (G. Sheldrick, 2015)'
_diffrn_ambient_temperature      150
_diffrn_detector                 '(CMOS) PHOTON 100'
_diffrn_detector_area_resol_mean 10.4167
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'D8 VENTURE Bruker AXS'
_diffrn_measurement_method       'rotation images'
_diffrn_orient_matrix_UB_11      -0.0505877
_diffrn_orient_matrix_UB_12      -0.0385469
_diffrn_orient_matrix_UB_13      -0.0255201
_diffrn_orient_matrix_UB_21      -0.0266506
_diffrn_orient_matrix_UB_22      0.0157887
_diffrn_orient_matrix_UB_23      0.0316868
_diffrn_orient_matrix_UB_31      -0.0149289
_diffrn_orient_matrix_UB_32      0.1024337
_diffrn_orient_matrix_UB_33      -0.0144876
_diffrn_radiation_monochromator  'multilayer monochromator'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_source         'Incoatec microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0705
_diffrn_reflns_av_unetI/netI     0.0470
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            24504
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.505
_diffrn_reflns_theta_min         2.407
_diffrn_source_current           1.0
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    1.494
_exptl_absorpt_correction_T_max  0.861
_exptl_absorpt_correction_T_min  0.595
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
  [Sheldrick, G.M. (2014). SADABS Bruker AXS Inc., Madison, Wisconsin, USA]
;
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.469
_exptl_crystal_description       prism
_exptl_crystal_F_000             1712
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.280
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.520
_refine_diff_density_min         -1.197
_refine_diff_density_rms         0.123
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     215
_refine_ls_number_reflns         4151
_refine_ls_number_restraints     5
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0475
_refine_ls_R_factor_gt           0.0442
_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^)+(0.0486P)^2^+15.4357P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1107
_refine_ls_wR_factor_ref         0.1132
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3827
_reflns_number_total             4151
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            d2dt00941b2.cif
_cod_data_source_block           CuCycNE
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C12 H31 Cl2 Cu N4 O2.50'
_cod_database_code               7710355
_shelx_res_checksum              3896