Structurally characterised new twisted conformer for cyclen, controlled by metal ion complexation as seen in NiII and CuII complexes with halides and pseudohalides
Verma, Abhineet; Bhuvanesh, Nattamai; Reibenspies, Joseph; Tayade, Sakharam B.; Kumbhar, Avinash S.; Bretosh, Kateryna; Sutter, Jean-Pascal; Sunkari, Sailaja S.; CrystEngComm 24 (2022) 119–131; doi:10.1039/D1CE01096D

data_7243815
_publ_section_title
;
 Structurally characterised new twisted conformer for cyclen, controlled
 by metal ion complexation as seen in NiII and CuII complexes with halides
 and pseudohalides
;
_journal_issue                   1
_journal_name_full               CrystEngComm
_journal_page_first              119
_journal_page_last               131
_journal_paper_doi               10.1039/D1CE01096D
_journal_volume                  24
_journal_year                    2022
_chemical_formula_moiety         'C8 H20 Br2 Cu N4'
_chemical_formula_sum            'C8 H20 Br2 Cu N4'
_chemical_formula_weight         395.64
_chemical_melting_point          474.15
_space_group_crystal_system      tetragonal
_space_group_IT_number           129
_space_group_name_Hall           '-P 4a 2a'
_space_group_name_H-M_alt        'P 4/n m m :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     'ShelXS-97 (Sheldrick 2008)'
_audit_creation_method           SHELXL-2018/1
_audit_update_record
;
2021-09-27 deposited with the CCDC.	2021-10-04 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.5813(6)
_cell_length_b                   9.5813(6)
_cell_length_c                   7.5171(5)
_cell_measurement_reflns_used    2408
_cell_measurement_temperature    300(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.65
_cell_volume                     690.08(8)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/1 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      300(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.951
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0554
_diffrn_reflns_av_unetI/netI     0.0314
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.951
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            14543
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.951
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         34.945
_diffrn_reflns_theta_min         3.445
_exptl_absorpt_coefficient_mu    7.351
_exptl_absorpt_correction_T_max  0.7469
_exptl_absorpt_correction_T_min  0.5215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Sadabs (Sheldrick, 2018)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_description       block
_exptl_crystal_F_000             390
_exptl_crystal_recrystallization_method
'Ether diffusion into methnolic mother liquor'
_exptl_crystal_size_max          0.212
_exptl_crystal_size_mid          0.201
_exptl_crystal_size_min          0.198
_refine_diff_density_max         1.050
_refine_diff_density_min         -0.511
_refine_diff_density_rms         0.114
_refine_ls_extinction_coef       0.0059(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/1 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     34
_refine_ls_number_reflns         846
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0468
_refine_ls_R_factor_gt           0.0288
_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^)+(0.0045P)^2^+0.5894P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0327
_refine_ls_wR_factor_ref         0.0350
_reflns_Friedel_coverage         0.000
_reflns_number_gt                708
_reflns_number_total             846
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1ce01096d2.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 7243811--7243817.cif.'
_cod_original_cell_volume        690.08(10)
_cod_original_sg_symbol_H-M      'P 4/n m m'
_cod_database_code               7243815
_shelx_shelxl_version_number     2018/1
_shelx_res_checksum              77860
_shelx_hkl_checksum              37022