Synthesis, structural studies, kinetic stability, and oxidation catalysis of the late first row transition metal complexes of 4,10-dimethyl-1,4,7,10-tetraazabicyclo[6.5.2]pentadecane.
Matz, Dallas L.; Jones, Donald G.; Roewe, Kimberly D.; Gorbet, Michael-Joseph; Zhang, Zhan; Chen, Zhuqi; Prior, Timothy J.; Archibald, Stephen J.; Yin, Guochuan; Hubin, Timothy J.; Dalton transactions (Cambridge, England : 2003) 44 (2015) 12210–12224; doi:10.1039/c5dt00742a

data_7034916
_publ_section_title
;
 Synthesis, structural studies, kinetic stability, and oxidation catalysis
 of the late first row transition metal complexes of
 4,10-dimethyl-1,4,7,10-tetraazabicyclo[6.5.2]pentadecane.
;
_journal_issue                   27
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12210
_journal_page_last               12224
_journal_paper_doi               10.1039/c5dt00742a
_journal_volume                  44
_journal_year                    2015
_chemical_formula_moiety
;
2(C13 H30 Cl N4 O Zn), Cl4 Zn, C2 H3 N
;
_chemical_formula_sum            'C28 H63 Cl6 N9 O2 Zn3'
_chemical_formula_weight         966.68
_space_group_crystal_system      triclinic
_space_group_IT_number           1
_space_group_name_Hall           'P 1'
_space_group_name_H-M_alt        'P 1'
_symmetry_space_group_name_Hall  'P 1'
_symmetry_space_group_name_H-M   'P 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/6
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                72.755(10)
_cell_angle_beta                 89.362(10)
_cell_angle_gamma                63.372(8)
_cell_formula_units_Z            1
_cell_length_a                   8.7520(10)
_cell_length_b                   9.3289(10)
_cell_length_c                   14.889(2)
_cell_measurement_reflns_used    3555
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      22.15
_cell_measurement_theta_min      2.5
_cell_volume                     1027.2(2)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_refinement  'SHELXL-2014/6 (Sheldrick, 2014)'
_computing_structure_solution    SHELXT
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.961
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.2027
_diffrn_reflns_laue_measured_fraction_full 0.994
_diffrn_reflns_laue_measured_fraction_max 0.961
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            11246
_diffrn_reflns_point_group_measured_fraction_full 0.911
_diffrn_reflns_point_group_measured_fraction_max 0.880
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.620
_diffrn_reflns_theta_min         1.447
_diffrn_source                   'Fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    2.166
_exptl_absorpt_correction_T_max  0.9255
_exptl_absorpt_correction_T_min  0.7182
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
A face-index absorption correction was carried out
within the Stoe X-AREA suite (twinAbs).
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_description       block
_exptl_crystal_F_000             502
_exptl_crystal_size_max          0.140
_exptl_crystal_size_mid          0.090
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.257
_refine_diff_density_min         -0.946
_refine_diff_density_rms         0.151
_refine_ls_abs_structure_details
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   0.31(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.898
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     447
_refine_ls_number_reflns         11246
_refine_ls_number_restraints     10
_refine_ls_restrained_S_all      0.898
_refine_ls_R_factor_all          0.1637
_refine_ls_R_factor_gt           0.1012
_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^)+(0.1567P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2497
_refine_ls_wR_factor_ref         0.2773
_reflns_Friedel_coverage         0.832
_reflns_friedel_fraction_full    0.828
_reflns_friedel_fraction_max     0.799
_reflns_number_gt                5681
_reflns_number_total             11246
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00742a2.cif
_cod_data_source_block           DGJ034
_cod_depositor_comments
'Adding full bibliography for 7034911--7034917.cif.'
_cod_database_code               7034916
_shelx_estimated_absorpt_t_min   0.751
_shelx_estimated_absorpt_t_max   0.918
_diffrn_reflns_v_r_equivalents   0.1511
_shelxl_version_number           2014/6
_shelx_res_checksum              43322