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_4342387
_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 Cl Mn N5, F6P
;
_chemical_formula_sum            'C19 H33 Cl F6 Mn N5 P'
_chemical_formula_weight         566.86
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      orthorhombic
_space_group_IT_number           29
_space_group_name_Hall           'P 2c -2ac'
_space_group_name_H-M_alt        'P c a 21'
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.5536(10)
_cell_length_b                   8.6768(4)
_cell_length_c                   14.9938(6)
_cell_measurement_reflns_used    23243
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      29.05
_cell_measurement_theta_min      1.75
_cell_volume                     2413.8(2)
_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 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  0.0459
_diffrn_reflns_av_unetI/netI     0.0345
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            20656
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.147
_diffrn_reflns_theta_min         2.195
_diffrn_source                   'Fine focus sealed tube'
_exptl_absorpt_coefficient_mu    0.788
_exptl_absorpt_correction_T_max  0.8298
_exptl_absorpt_correction_T_min  0.7509
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
A face-index absorption correction was applied
within the Stoe X-AREA suite.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.560
_exptl_crystal_description       block
_exptl_crystal_F_000             1172
_exptl_crystal_size_max          0.360
_exptl_crystal_size_mid          0.350
_exptl_crystal_size_min          0.320
_refine_diff_density_max         0.289
_refine_diff_density_min         -0.300
_refine_diff_density_rms         0.049
_refine_ls_abs_structure_details
;
 Flack x determined using 2491 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons and Flack (2004), Acta Cryst. A60, s61).
;
_refine_ls_abs_structure_Flack   -0.007(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     299
_refine_ls_number_reflns         6495
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0387
_refine_ls_R_factor_gt           0.0337
_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^)+(0.0548P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0832
_refine_ls_wR_factor_ref         0.0848
_reflns_Friedel_coverage         0.925
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                5709
_reflns_number_total             6495
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic502699m_si_002.cif
_cod_data_source_block           DGJ010B
_cod_depositor_comments
'Adding full bibliography for 4342387--4342393.cif.'
_cod_database_code               4342387
_shelx_estimated_absorpt_t_min   0.765
_shelx_estimated_absorpt_t_max   0.787
_shelxl_version_number           2013-4
_shelx_res_checksum              11290
_shelx_hkl_checksum              97613