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_7126634
_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_absolute_configuration ad
_chemical_formula_moiety
;
C15 H36 N5, 2(F6 P), C2 H3 N, Br
;
_chemical_formula_sum            'C17 H39 Br F12 N6 P2'
_chemical_formula_weight         697.39
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_audit_update_record
;
2019-05-20 deposited with the CCDC.	2020-06-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9823(8)
_cell_length_b                   13.9805(14)
_cell_length_c                   24.662(3)
_cell_measurement_reflns_used    9825
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.691
_cell_measurement_theta_min      2.401
_cell_volume                     2752.2(5)
_computing_cell_refinement       'Bruker SAINT v8.37A'
_computing_data_collection       'Bruker APEX3 v2016.1.0'
_computing_data_reduction        'Bruker SAINT v8.37A'
_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 0.998
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.7749
_diffrn_reflns_av_R_equivalents  0.0635
_diffrn_reflns_av_unetI/netI     0.0455
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            48044
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        27.706
_diffrn_reflns_theta_max         29.832
_diffrn_reflns_theta_min         2.401
_diffrn_source                   'ALS beamline 11.3.1.'
_exptl_absorpt_coefficient_mu    2.114
_exptl_absorpt_correction_T_max  0.9281
_exptl_absorpt_correction_T_min  0.7831
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2014/5'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.683
_exptl_crystal_description       blade
_exptl_crystal_F_000             1424
_exptl_crystal_size_max          0.110
_exptl_crystal_size_mid          0.050
_exptl_crystal_size_min          0.010
_refine_diff_density_max         1.414
_refine_diff_density_min         -0.568
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2096 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.039(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     350
_refine_ls_number_reflns         6085
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.068
_refine_ls_R_factor_all          0.0486
_refine_ls_R_factor_gt           0.0411
_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^)+(0.0557P)^2^+1.9739P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1072
_refine_ls_wR_factor_ref         0.1105
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.997
_reflns_number_gt                5430
_reflns_number_total             6085
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cc00919a2.cif
_cod_data_source_block           L
_cod_depositor_comments
'Adding full bibliography for 7126634--7126636.cif.'
_cod_database_code               7126634
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.801
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              2577
_shelx_hkl_checksum              10151