#------------------------------------------------------------------------------
#$Date: 2018-10-05 15:19:55 +0300 (Fri, 05 Oct 2018) $
#$Revision: 211332 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/32/83/4328340.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4328340
loop_
_publ_author_name
'Michael J. Rose'
'Jay R. Winkler'
'Harry B. Gray'
_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         'C12 H18 B2 F4 Fe N6 O4'
_chemical_formula_sum            'C12 H18 B2 F4 Fe N6 O4'
_chemical_formula_weight         463.79
_chemical_name_systematic
;
 ?
;
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 112.894(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.6038(4)
_cell_length_b                   11.6895(6)
_cell_length_c                   9.4407(4)
_cell_measurement_reflns_used    9931
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      45.24
_cell_measurement_theta_min      2.72
_cell_volume                     874.70(7)
_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 0.984
_diffrn_measured_fraction_theta_max 0.984
_diffrn_measurement_device_type  'Bruker KAPPA APEX II'
_diffrn_measurement_method       'ω scans; 16 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  0.0355
_diffrn_reflns_av_sigmaI/netI    0.0292
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            35628
_diffrn_reflns_theta_full        45.43
_diffrn_reflns_theta_max         45.43
_diffrn_reflns_theta_min         2.57
_exptl_absorpt_coefficient_mu    0.939
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_correction_T_min  0.8957
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'Red orange'
_exptl_crystal_density_diffrn    1.761
_exptl_crystal_description       Blade
_exptl_crystal_F_000             472
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.07
_refine_diff_density_max         0.811
_refine_diff_density_min         -1.546
_refine_diff_density_rms         0.072
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.787
_refine_ls_hydrogen_treatment    Unrestrained
_refine_ls_matrix_type           'Full matrix'
_refine_ls_number_parameters     169
_refine_ls_number_reflns         7257
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.787
_refine_ls_R_factor_all          0.0354
_refine_ls_R_factor_gt           0.0264
_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/s²(Fo²)
_refine_ls_weighting_scheme      sigma
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0481
_reflns_number_gt                5970
_reflns_number_total             7257
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202253v_si_002_1.cif
_cod_data_source_block           mjr01
_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 'Difference Fourier map' was
changed to 'difmap'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
;
_cod_original_cell_volume        874.69(7)
_cod_database_code               4328340
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.0000 0.5000 0.5000 0.00675(2) Uani 1 2 d S
F1 F 0.38026(5) 0.63513(3) 0.72408(5) 0.01495(7) Uani 1 1 d .
F2 F 0.32093(5) 0.67402(3) 0.93685(4) 0.01499(7) Uani 1 1 d .
O1 O 0.10993(5) 0.69575(4) 0.70165(5) 0.01066(7) Uani 1 1 d .
O2 O 0.23604(5) 0.50283(4) 0.81699(5) 0.01098(7) Uani 1 1 d .
N1 N 0.15871(6) 0.43967(4) 0.68597(6) 0.00855(7) Uani 1 1 d .
N2 N 0.01645(6) 0.65609(4) 0.55691(6) 0.00849(7) Uani 1 1 d .
N3 N 0.17090(6) 0.52552(4) 0.41712(6) 0.00971(8) Uani 1 1 d .
B1 B 0.26278(8) 0.62609(6) 0.79225(8) 0.01055(10) Uani 1 1 d .
C1 C 0.18107(7) 0.32959(5) 0.69248(7) 0.00905(8) Uani 1 1 d .
C2 C 0.07486(7) 0.27210(5) 0.54695(7) 0.00921(8) Uani 1 1 d .
C3 C 0.30183(7) 0.26545(5) 0.82597(7) 0.01215(9) Uani 1 1 d .
C4 C 0.07379(8) 0.14557(5) 0.52787(8) 0.01284(10) Uani 1 1 d .
C5 C 0.26725(7) 0.55165(5) 0.36649(7) 0.01085(9) Uani 1 1 d .
C6 C 0.39120(8) 0.58406(6) 0.30339(8) 0.01524(11) Uani 1 1 d .
H3A H 0.3588(11) 0.3187(9) 0.9077(12) 0.025(2) Uiso 1 1 d .
H3B H 0.3830(11) 0.2277(8) 0.7949(11) 0.023(2) Uiso 1 1 d .
H3C H 0.2446(11) 0.2050(8) 0.8588(11) 0.019(2) Uiso 1 1 d .
H4A H 0.0210(12) 0.1077(9) 0.5891(12) 0.030(3) Uiso 1 1 d .
H4B H 0.1889(12) 0.1152(8) 0.5636(12) 0.026(2) Uiso 1 1 d .
H4C H 0.0148(12) 0.1257(9) 0.4248(13) 0.029(3) Uiso 1 1 d .
H6A H 0.4611(13) 0.6386(10) 0.3681(13) 0.035(3) Uiso 1 1 d .
H6B H 0.3335(12) 0.6154(9) 0.2047(12) 0.026(2) Uiso 1 1 d .
H6C H 0.4602(12) 0.5177(9) 0.3040(12) 0.027(2) Uiso 1 1 d .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
N1 Fe1 N2 98.55(2) . .
N1 Fe1 N1 180.0 . 3_566
N2 Fe1 N1 81.45(2) . 3_566
N1 Fe1 N2 81.45(2) . 3_566
N2 Fe1 N2 180.0 . 3_566
N1 Fe1 N2 98.55(2) 3_566 3_566
N1 Fe1 N3 92.58(2) . .
N2 Fe1 N3 88.942(19) . .
N1 Fe1 N3 87.42(2) 3_566 .
N2 Fe1 N3 91.057(18) 3_566 .
N1 Fe1 N3 87.42(2) . 3_566
N2 Fe1 N3 91.059(18) . 3_566
N1 Fe1 N3 92.58(2) 3_566 3_566
N2 Fe1 N3 88.942(18) 3_566 3_566
N3 Fe1 N3 180.0 . 3_566
N2 O1 B1 115.46(4) . .
N1 O2 B1 115.43(4) . .
C1 N1 O2 118.69(5) . .
C1 N1 Fe1 116.96(4) . .
O2 N1 Fe1 123.96(4) . .
C2 N2 O1 118.89(5) 3_566 .
C2 N2 Fe1 116.93(4) 3_566 .
O1 N2 Fe1 124.06(4) . .
C5 N3 Fe1 173.28(5) . .
F2 B1 F1 112.14(5) . .
F2 B1 O2 104.86(5) . .
F1 B1 O2 109.17(5) . .
F2 B1 O1 104.14(5) . .
F1 B1 O1 109.10(5) . .
O2 B1 O1 117.34(5) . .
N1 C1 C2 112.25(5) . .
N1 C1 C3 125.55(5) . .
C2 C1 C3 122.17(5) . .
N2 C2 C1 112.38(5) 3_566 .
N2 C2 C4 125.27(5) 3_566 .
C1 C2 C4 122.34(5) . .
C1 C3 H3A 108.8(6) . .
C1 C3 H3B 108.9(6) . .
H3A C3 H3B 109.6(7) . .
C1 C3 H3C 111.2(6) . .
H3A C3 H3C 112.1(7) . .
H3B C3 H3C 106.2(7) . .
C2 C4 H4A 111.3(6) . .
C2 C4 H4B 111.1(6) . .
H4A C4 H4B 105.9(8) . .
C2 C4 H4C 110.3(7) . .
H4A C4 H4C 108.4(8) . .
H4B C4 H4C 109.5(8) . .
N3 C5 C6 179.35(7) . .
C5 C6 H6A 107.4(6) . .
C5 C6 H6B 108.5(5) . .
H6A C6 H6B 110.0(9) . .
C5 C6 H6C 109.3(5) . .
H6A C6 H6C 107.9(8) . .
H6B C6 H6C 113.6(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 N1 1.8918(5) .
Fe1 N2 1.8918(5) .
Fe1 N1 1.8918(5) 3_566
Fe1 N2 1.8918(5) 3_566
Fe1 N3 1.9387(4) .
Fe1 N3 1.9387(4) 3_566
F1 B1 1.3974(6) .
F2 B1 1.3771(8) .
O1 N2 1.3688(6) .
O1 B1 1.4997(8) .
O2 N1 1.3702(6) .
O2 B1 1.4918(8) .
N1 C1 1.2990(7) .
N2 C2 1.2976(7) 3_566
N3 C5 1.1477(7) .
C1 C2 1.4824(8) .
C1 C3 1.4870(8) .
C2 N2 1.2977(7) 3_566
C2 C4 1.4895(8) .
C3 H3A 0.963(10) .
C3 H3B 0.963(8) .
C3 H3C 0.979(9) .
C4 H4A 0.969(9) .
C4 H4B 0.980(10) .
C4 H4C 0.934(11) .
C5 C6 1.4595(7) .
C6 H6A 0.925(12) .
C6 H6B 0.943(11) .
C6 H6C 0.975(10) .
