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_7034917
_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
;
C15 H33 N4 O3 Zn, F6 P
;
_chemical_formula_sum            'C15 H33 F6 N4 O3 P Zn'
_chemical_formula_weight         527.79
_space_group_crystal_system      trigonal
_space_group_IT_number           161
_space_group_name_Hall           'R 3 -2"c'
_space_group_name_H-M_alt        'R 3 c :H'
_symmetry_space_group_name_Hall  'R 3 -2"c'
_symmetry_space_group_name_H-M   'R 3 c :H'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2015-02-17 deposited with the CCDC.
2015-04-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            18
_cell_length_a                   25.8872(12)
_cell_length_b                   25.8872(12)
_cell_length_c                   17.1214(8)
_cell_measurement_reflns_used    35977
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.9
_cell_measurement_theta_min      2.55
_cell_volume                     9936.7(8)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Stoe IPDS2'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0804
_diffrn_reflns_av_unetI/netI     0.0397
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -36
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            54418
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.999
_diffrn_reflns_theta_min         2.547
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    1.259
_exptl_absorpt_correction_T_max  0.893
_exptl_absorpt_correction_T_min  0.630
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
Empirical absorption correction applied within Sortav 
(Blessing, 1995)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.588
_exptl_crystal_description       'hexagonal plate'
_exptl_crystal_F_000             4932
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.150
_refine_diff_density_max         0.648
_refine_diff_density_min         -0.393
_refine_diff_density_rms         0.083
_refine_ls_abs_structure_details
;
 Flack x determined using 2346 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.006(5)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     278
_refine_ls_number_reflns         6458
_refine_ls_number_restraints     7
_refine_ls_restrained_S_all      0.995
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0748P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1042
_refine_ls_wR_factor_ref         0.1106
_reflns_Friedel_coverage         0.994
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                5468
_reflns_number_total             6458
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c5dt00742a2.cif
_cod_data_source_block           sja23_09
_cod_depositor_comments
'Adding full bibliography for 7034911--7034917.cif.'
_cod_original_cell_volume        9936.6(10)
_cod_database_code               7034917
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.704
_shelx_estimated_absorpt_t_max   0.834
_shelx_res_checksum              11822