[FeIII(tmdta)]–twist-boat/half-chair conformer ratio reliably deduced from DFT-calculated Raman spectra.
Meier, Roland; Maigut, Joachim; Kallies, Bernd; Lehnert, Nicolai; Paulat, Florian; Heinemann, Frank W; Zahn, Gernot; Feth, Martin P; Krautscheid, Harald; van Eldik, Rudi; Chemical communications (Cambridge, England)  (2007) 3960–3962; doi:10.1039/b708437d

data_7102165
_publ_section_title
;
 [FeIII(tmdta)]--twist-boat/half-chair conformer ratio reliably deduced
 from DFT-calculated Raman spectra.
;
_journal_issue                   38
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              3960
_journal_page_last               3962
_journal_paper_doi               10.1039/b708437d
_journal_year                    2007
_chemical_compound_source        'synthesis as described'
_chemical_formula_moiety         'C11 H14 Fe N2 O8, H4 N, 0.5 (H2 O)'
_chemical_formula_sum            'C11 H19 Fe N3 O8.5'
_chemical_formula_weight         385.14
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_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_date             2007-08-06T13:23:18-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'
_cell_angle_alpha                90
_cell_angle_beta                 103.859(9)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   8.6446(13)
_cell_length_b                   11.0545(10)
_cell_length_c                   16.837(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.726
_cell_measurement_theta_min      9.821
_cell_measurement_wavelength     0.71073
_cell_volume                     1562.1(4)
_computing_cell_refinement       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_collection       'CAD4 Express (Enraf Nonius, 1994)'
_computing_data_reduction        'XCAD4 (Harms & Wocadlo, 1995)'
_computing_molecular_graphics    'Ortep-3 for Windows (Farrugia, 1997)'
_computing_publication_material  'WinGX publication routines (Farrugia, 1999)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'scintillation LiI'
_diffrn_detector_dtime           1.195
_diffrn_measured_fraction_theta_full 1
_diffrn_measured_fraction_theta_max 1
_diffrn_measurement_device       '\k-geometry diffractometer'
_diffrn_measurement_device_type  'Enraf Nonius CAD4'
_diffrn_measurement_method       'non-profiled omega/2theta scans'
_diffrn_orient_matrix_type
;
x-axis points to radiation source
the matrix is specified in reciprocal space
;
_diffrn_orient_matrix_UB_11      0.078776
_diffrn_orient_matrix_UB_12      0.058701
_diffrn_orient_matrix_UB_13      -0.012829
_diffrn_orient_matrix_UB_21      0.047604
_diffrn_orient_matrix_UB_22      0.011409
_diffrn_orient_matrix_UB_23      0.059951
_diffrn_orient_matrix_UB_31      0.075913
_diffrn_orient_matrix_UB_32      -0.06795
_diffrn_orient_matrix_UB_33      -0.001055
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.1023
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7134
_diffrn_reflns_theta_full        27.45
_diffrn_reflns_theta_max         27.45
_diffrn_reflns_theta_min         2.22
_diffrn_source                   'Enraf Nonius FR590'
_diffrn_standards_decay_%        3
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.015
_exptl_absorpt_correction_T_max  0.8764
_exptl_absorpt_correction_T_min  0.5045
_exptl_absorpt_correction_type   refdelf
_exptl_absorpt_process_details
;
Walker, N. & Stuart, D (1983) Acta. Cryst. A39, 158-166
;
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.638
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cube
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.7
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.13
_refine_diff_density_max         0.348
_refine_diff_density_min         -0.359
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       0.0020(7)
_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   1.013
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     236
_refine_ls_number_reflns         3573
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.009
_refine_ls_R_factor_all          0.1084
_refine_ls_R_factor_gt           0.0468
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0424P)^2^+0.1653P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0996
_refine_ls_wR_factor_ref         0.1163
_reflns_number_gt                2094
_reflns_number_total             3573
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b708437d.txt
_cod_data_source_block           NH4Fe(tmdta)x0.5H2O_CCDC649050
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C11 H19 Fe N3 O8.50'
_cod_database_code               7102165