An ethylene cross-bridged pentaazamacrocycle and its Cu<sup>2+</sup> complex: constrained ligand topology and excellent kinetic stability.
Shircliff, Anthony D.; Burke, Benjamin P.; Davilla, Dustin J.; Burgess, Gwendolyn E.; Okorocha, Faith A.; Shrestha, Alina; Allbritton, Elisabeth M. A.; Nguyen, Phillip T.; Lamar, Rachael L.; Jones, Donald G.; Gorbet, Michael-Joseph; Allen, Michael B.; Eze, John I.; Fernandez, Andrea T.; Ramirez, Daniel; Archibald, Stephen J.; Prior, Timothy J.; Krause, Jeanette A.; Oliver, Allen G.; Hubin, Timothy J.; Chemical communications (Cambridge, England) 56 (2020) 7519–7522; doi:10.1039/d0cc00919a

data_7126636
_publ_section_title
;
 An ethylene cross-bridged pentaazamacrocycle and its Cu<sup>2+</sup>
 complex: constrained ligand topology and excellent kinetic stability.
;
_journal_issue                   54
_journal_name_full
'Chemical communications (Cambridge, England)'
_journal_page_first              7519
_journal_page_last               7522
_journal_paper_doi               10.1039/d0cc00919a
_journal_volume                  56
_journal_year                    2020
_chemical_formula_moiety
;
8(C15 H31 N5), 5(C H4 O), 16(I), 8(H2 O)
;
_chemical_formula_sum            'C15.62 H35.5 I2 N5 O1.62'
_chemical_formula_weight         573.29
_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
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2020-02-03 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.514(2)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.5537(9)
_cell_length_b                   18.0400(9)
_cell_length_c                   15.0137(7)
_cell_measurement_reflns_used    9732
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.066
_cell_measurement_theta_min      2.3155
_cell_volume                     4445.0(4)
_computing_cell_refinement       'Bruker SAINT v8.38A'
_computing_data_collection       'Bruker APEX3 v2016.9.0'
_computing_data_reduction        'Bruker SAINT v8.38A'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker PHOTON-II'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7288
_diffrn_reflns_av_R_equivalents  0.0532
_diffrn_reflns_av_unetI/netI     0.0292
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            50133
_diffrn_reflns_point_group_measured_fraction_full 0.999
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_diffrn_reflns_theta_full        25.930
_diffrn_reflns_theta_max         29.100
_diffrn_reflns_theta_min         2.112
_diffrn_source
'Beamline 12.2.1 at the Advanced Light Source (ALS)'
_exptl_absorpt_coefficient_mu    3.006
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6624
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2016.2 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.713
_exptl_crystal_description       plate
_exptl_crystal_F_000             2266
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.056
_exptl_crystal_size_min          0.036
_refine_diff_density_max         0.615
_refine_diff_density_min         -0.869
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     242
_refine_ls_number_reflns         5526
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.0307
_refine_ls_R_factor_gt           0.0258
_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^)+(0.0142P)^2^+10.0003P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0532
_refine_ls_wR_factor_ref         0.0560
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4913
_reflns_number_total             5526
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00919a2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7126634--7126636.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_original_formula_sum        'C15.62 H35.50 I2 N5 O1.62'
_cod_database_code               7126636
_shelx_shelxl_version_number     2018/3
_shelx_res_checksum              11591
_shelx_hkl_checksum              29979