Spin-State Variation in Solid State and Solution of Mononuclear Iron(II) 1,4,7-Trimethyl-1,4,7-triazacyclonane Complexes
David W. Blakesley; Sonha C. Payne; Karl S. Hagen; Inorganic Chemistry 39 (2000) 1979–1989; doi:10.1021/ic990584+

data_4327639
_publ_contact_author_address
;
Emory University
Department of Chemistry
X-ray Crystallography Center
Atlanta GA  30322
USA
;
_publ_contact_author_email       chemksh@emory.edu
_publ_contact_author_fax         404-727-6586
_publ_contact_author_name        'Karl S. Hagen'
_publ_contact_author_phone       404-727-6556
_publ_section_title
;
 Spin-State Variation in Solid State and Solution of Mononuclear Iron(II)
 1,4,7-Trimethyl-1,4,7-triazacyclonane Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1979
_journal_page_last               1989
_journal_paper_doi               10.1021/ic990584+
_journal_volume                  39
_journal_year                    2000
_chemical_formula_sum            'C11 H23 F6 Fe N3 O7 S2'
_chemical_formula_weight         543.29
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 94.02(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.253(3)
_cell_length_b                   12.624(5)
_cell_length_c                   14.683(5)
_cell_measurement_reflns_used    29
_cell_measurement_temperature    211(2)
_cell_measurement_theta_max      27.89
_cell_measurement_theta_min      11.57
_cell_volume                     2080.7(12)
_computing_cell_refinement       'Siemens XSCANS'
_computing_data_collection       'Siemens XSCANS'
_computing_data_reduction        'Siemens SHELXTL'
_computing_molecular_graphics    'Siemens SHELXTL'
_computing_publication_material  'Siemens SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      211(2)
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Siemens P4-RA'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_sigmaI/netI    0.0467
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            3560
_diffrn_reflns_theta_full        56.79
_diffrn_reflns_theta_max         56.79
_diffrn_reflns_theta_min         4.62
_diffrn_standards_decay_%        16
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    8.570
_exptl_absorpt_correction_T_max  0.0621
_exptl_absorpt_correction_T_min  0.0024
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'XPREP psi scans'
_exptl_crystal_colour            'colorless         '
_exptl_crystal_density_diffrn    1.734
_exptl_crystal_description       plate
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.5
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.652
_refine_diff_density_min         -0.444
_refine_diff_density_rms         0.126
_refine_ls_extinction_coef       0.0000(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     280
_refine_ls_number_reflns         2741
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0703
_refine_ls_shift/su_max          0.739
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1224P)^2^+2.0809P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1776
_refine_ls_wR_factor_ref         0.1864
_reflns_number_gt                2408
_reflns_number_total             2741
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           db2125b
_cod_database_code               4327639