Fe4 Cluster and a Buckled Macrocycle Complex from the Reduction of [(dmgBF2)2Fe(L)2] (L = MeCN,tBuiNC)
Michael J. Rose; Jay R. Winkler; Harry B. Gray; Inorganic Chemistry 51 (2012) 1980–1982; doi:10.1021/ic202253v

data_4328341
_publ_contact_author_address
;
Division of Chemistry and Chemical Engineering,
California Institute of Technology,
1200 E California Blvd,
Pasdena, CA 91125
USA
;
_publ_contact_author_email       mrose@caltech.edu
_publ_contact_author_fax         '+1 626 459 2935'
_publ_contact_author_name        'Michael Rose'
_publ_contact_author_phone       '+1 626 395 2846'
_publ_section_title
;
 Fe4 Cluster and a Buckled Macrocycle Complex from the Reduction of
 [(dmgBF2)2Fe(L)2] (L = MeCN,tBuiNC)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1980
_journal_page_last               1982
_journal_paper_doi               10.1021/ic202253v
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         'C36 H54 B3 F6 Fe4 N18 O12'
_chemical_formula_sum            'C36 H54 B3 F6 Fe4 N18 O12'
_chemical_formula_weight         1300.80
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           148
_symmetry_cell_setting           rhombohedral
_symmetry_space_group_name_Hall  '-R 3'
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_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
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_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                120.00
_cell_formula_units_Z            18
_cell_length_a                   35.6736(7)
_cell_length_b                   35.6736(7)
_cell_length_c                   32.5160(9)
_cell_measurement_reflns_used    9894
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.52
_cell_measurement_theta_min      2.20
_cell_volume                     35836.2(14)
_computing_cell_refinement       'Bruker SAINT-Plus v7.66A'
_computing_data_collection       'Bruker APEX2 v2009.7-0'
_computing_data_reduction        'Bruker SAINT-Plus v7.66A'
_computing_molecular_graphics    'Bruker XP v5.1'
_computing_publication_material  'Bruker XCIF 2008'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.890
_diffrn_measured_fraction_theta_max 0.890
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       '\w scans; 4 settings'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0767
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       46
_diffrn_reflns_limit_k_min       -40
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            88192
_diffrn_reflns_theta_full        28.01
_diffrn_reflns_theta_max         28.01
_diffrn_reflns_theta_min         1.42
_exptl_absorpt_coefficient_mu    0.778
_exptl_absorpt_correction_T_max  0.8989
_exptl_absorpt_correction_T_min  0.8923
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Dark red-orange'
_exptl_crystal_density_diffrn    1.085
_exptl_crystal_description       'Triangular prism'
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_platon_squeeze_details
;
;
_refine_diff_density_max         1.538
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_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    Riding
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     743
_refine_ls_number_reflns         17159
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      3.091
_refine_ls_R_factor_all          0.1438
_refine_ls_R_factor_gt           0.0886
_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^)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.1183
_refine_ls_wR_factor_ref         0.1197
_reflns_number_gt                8005
_reflns_number_total             17159
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202253v_si_002_2.cif
_cod_data_source_block           mjr03
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'direct methods' was changed to
'direct'.

'_atom_sites_solution_secondary' value 'Difference Fourier map' was
changed to 'difmap'.

'_atom_sites_solution_hydrogens' value 'Geometric positions' was
changed to 'geom'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        35836.1(14)
_cod_original_sg_symbol_H-M      'R -3'
_cod_database_code               4328341