Crystal Structures and Solution Behavior of Paramagnetic Divalent Transition Metal Complexes (Fe, Co) of the Sterically Encumbered Tridentate Macrocycles 1,4,7-R3-1,4,7-Triazacyclononane: Coordination Numbers 5 (R = i-Pr) and 6 (R = i-Bu)
Alain Diebold; Abdelaziz Elbouadili; Karl S. Hagen; Inorganic Chemistry 39 (2000) 3915–3923; doi:10.1021/ic000456h

data_4321272
_publ_section_title
;
 Crystal Structures and Solution Behavior of Paramagnetic Divalent
 Transition Metal Complexes (Fe, Co) of the Sterically Encumbered
 Tridentate Macrocycles 1,4,7-R3-1,4,7-Triazacyclononane: Coordination
 Numbers 5 (R = i-Pr) and 6 (R = i-Bu)
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3915
_journal_page_last               3923
_journal_paper_doi               10.1021/ic000456h
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '[Fe(i-Bu3TACN)(CH3CN)2(SO3CF3)](SO3CF3)'
_chemical_formula_sum            'C24 H45 F6 Fe N5 O6 S2'
_chemical_formula_weight         733.62
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 96.32(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.953(6)
_cell_length_b                   16.780(6)
_cell_length_c                   15.790(5)
_cell_measurement_reflns_used    69
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      28.00
_cell_measurement_theta_min      0.00
_cell_volume                     3411(2)
_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-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_measurement_device       'Siemens P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0439
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -1
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            5647
_diffrn_reflns_theta_max         56.74
_diffrn_reflns_theta_min         3.43
_diffrn_standards_decay_%        6.12
_diffrn_standards_interval_count 97
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.371
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_description       cut_from_large_crystal
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.42
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.856
_refine_diff_density_min         -0.576
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.034
_refine_ls_goodness_of_fit_obs   1.021
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     398
_refine_ls_number_reflns         4518
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.034
_refine_ls_restrained_S_obs      1.021
_refine_ls_R_factor_all          0.0667
_refine_ls_R_factor_obs          0.0581
_refine_ls_shift/esd_max         -0.002
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+10.5727P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1561
_refine_ls_wR_factor_obs         0.1451
_reflns_number_observed          4040
_reflns_number_total             4518
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic000456h_3.cif
_cod_data_source_block           Complex6
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+10.5727P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0820P)^2^+10.5727P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3411.1(23)
_cod_database_code               4321272