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_4327637
_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            'C63 H70 B2 Fe N6'
_chemical_formula_weight         988.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 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                 90.320(11)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.4560(9)
_cell_length_b                   11.8230(12)
_cell_length_c                   26.258(4)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    368(2)
_cell_measurement_theta_max      27.88
_cell_measurement_theta_min      10.16
_cell_volume                     5729.5(11)
_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      368(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_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  0.0578
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       1
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            7104
_diffrn_reflns_theta_full        50.02
_diffrn_reflns_theta_max         50.02
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        30
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    2.432
_exptl_absorpt_correction_T_max  0.6178
_exptl_absorpt_correction_T_min  0.3917
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'XPREP psi scans'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.146
_exptl_crystal_description       very_large_rod_in_
_exptl_crystal_F_000             2104
_exptl_crystal_size_max          0.8
_exptl_crystal_size_mid          0.5
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.313
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.044
_refine_ls_extinction_coef       0.00215(18)
_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   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     662
_refine_ls_number_reflns         5787
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0849
_refine_ls_R_factor_gt           0.0587
_refine_ls_shift/su_max          0.162
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1057P)^2^+2.2903P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1548
_refine_ls_wR_factor_ref         0.1759
_reflns_number_gt                4211
_reflns_number_total             5787
_reflns_threshold_expression     >2sigma(I)
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_cod_data_source_block           db3285e
_cod_database_code               4327637