The Two Faces of Tetramethylcyclam in Iron Chemistry: Distinct Fe-O-M Complexes Derived from [Fe<sup>IV</sup>(O<sub>anti/syn</sub>)(TMC)]<sup>2+</sup> Isomers.
Zhou, Ang; Prakash, Jai; Rohde, Gregory T.; Klein, Johannes E. M. N.; Kleespies, Scott T.; Draksharapu, Apparao; Fan, Ruixi; Guo, Yisong; Cramer, Christopher J.; Que, Jr, Lawrence; Inorganic chemistry 56 (2017) 518–527; doi:10.1021/acs.inorgchem.6b02417

data_4349330
_publ_section_title
;
 The Two Faces of Tetramethylcyclam in Iron Chemistry: Distinct Fe-O-M
 Complexes Derived from
 [Fe<sup>IV</sup>(O<sub>anti/syn</sub>)(TMC)]<sup>2+</sup> Isomers.
;
_journal_issue                   1
_journal_name_full               'Inorganic chemistry'
_journal_page_first              518
_journal_page_last               527
_journal_paper_doi               10.1021/acs.inorgchem.6b02417
_journal_volume                  56
_journal_year                    2017
_chemical_formula_moiety         'C14 H32 Cl3 Fe2 N4 O, C F3 O3 S, 2(C2 H3 N)'
_chemical_formula_sum            'C19 H38 Cl3 F3 Fe2 N6 O4 S'
_chemical_formula_weight         721.66
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.9480(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.1776(8)
_cell_length_b                   9.2395(7)
_cell_length_c                   33.194(3)
_cell_measurement_reflns_used    239
_cell_measurement_temperature    173(2)
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_cell_measurement_theta_min      2.28
_cell_volume                     3119.6(4)
_computing_cell_refinement       'SAINT+ V2012/1'
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_computing_data_reduction        'SAINT+ V2012/1'
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_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0376
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       11
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_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            32519
_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         26.410
_diffrn_reflns_theta_min         1.228
_exptl_absorpt_coefficient_mu    1.307
_exptl_absorpt_correction_T_max  0.7456
_exptl_absorpt_correction_T_min  0.6317
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS, R. Blessing, 1995'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.537
_exptl_crystal_description       block
_exptl_crystal_F_000             1488
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.289
_refine_diff_density_min         -0.811
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     501
_refine_ls_number_reflns         6404
_refine_ls_number_restraints     313
_refine_ls_restrained_S_all      1.288
_refine_ls_R_factor_all          0.0658
_refine_ls_R_factor_gt           0.0479
_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^)+(0.0393P)^2^+6.2762P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1056
_refine_ls_wR_factor_ref         0.1167
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4984
_reflns_number_total             6404
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ic6b02417_si_001.cif
_cod_data_source_block           14202a1
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4349330
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              77680
_shelx_hkl_checksum              65985