Synthesis, Structural Studies, and Oxidation Catalysis of the Late-First-Row-Transition-Metal Complexes of a 2-Pyridylmethyl Pendant-Armed Ethylene Cross-Bridged Cyclam.
Jones, Donald G.; Wilson, Kevin R.; Cannon-Smith, Desiray J; Shircliff, Anthony D.; Zhang, Zhan; Chen, Zhuqi; Prior, Timothy J.; Yin, Guochuan; Hubin, Timothy J.; Inorganic chemistry 54 (2015) 2221–; doi:10.1021/ic502699m

data_4342391
_publ_section_title
;
 Synthesis, Structural Studies, and Oxidation Catalysis of the
 Late-First-Row-Transition-Metal Complexes of a 2-Pyridylmethyl
 Pendant-Armed Ethylene Cross-Bridged Cyclam.
;
_journal_issue                   5
_journal_name_full               'Inorganic chemistry'
_journal_page_first              2221
_journal_paper_doi               10.1021/ic502699m
_journal_volume                  54
_journal_year                    2015
_chemical_formula_moiety
;
C19 H33 Cu N5, 2(F6 P)
;
_chemical_formula_sum            'C19 H33 Cu F12 N5 P2'
_chemical_formula_weight         684.98
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 98.149(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.5546(6)
_cell_length_b                   13.2043(11)
_cell_length_c                   18.6149(10)
_cell_measurement_reflns_used    11102
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.4
_cell_measurement_theta_min      1.9
_cell_volume                     2568.1(3)
_computing_cell_refinement       'Stoe X-AREA'
_computing_data_collection       'Stoe X-AREA'
_computing_data_reduction        'Stoe X-AREA'
_computing_structure_refinement  'SHELXL-2013 (Sheldrick, 2013)'
_computing_structure_solution    SHELXS-86
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.997
_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  0.0622
_diffrn_reflns_av_unetI/netI     0.0823
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            13139
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.300
_diffrn_reflns_theta_max         27.000
_diffrn_reflns_theta_min         1.897
_exptl_absorpt_coefficient_mu    1.083
_exptl_absorpt_correction_T_max  0.930
_exptl_absorpt_correction_T_min  0.7798
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
A face indexed absorption correction was applied within
the Stoe X-AREA suite.
;
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.772
_exptl_crystal_description       blovk
_exptl_crystal_F_000             1396
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.220
_exptl_crystal_size_min          0.110
_refine_diff_density_max         0.653
_refine_diff_density_min         -1.160
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.896
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     373
_refine_ls_number_reflns         5602
_refine_ls_number_restraints     36
_refine_ls_restrained_S_all      0.893
_refine_ls_R_factor_all          0.0921
_refine_ls_R_factor_gt           0.0476
_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^)+(0.0713P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1110
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3255
_reflns_number_total             5602
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502699m_si_002.cif
_cod_data_source_block           shelx
_cod_depositor_comments
'Adding full bibliography for 4342387--4342393.cif.'
_cod_database_code               4342391
_shelx_estimated_absorpt_t_min   0.773
_shelx_estimated_absorpt_t_max   0.890
_shelxl_version_number           2013-4
_shelx_res_checksum              10120
_shelx_hkl_checksum              60684