#------------------------------------------------------------------------------
#$Date: 2016-03-21 11:15:17 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178685 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/96/4079642.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_4079642
loop_
_publ_author_name
'Hosokawa, Satomi'
'Ito, Jun-ichi'
'Nishiyama, Hisao'
_publ_section_title
;
 Change in Coordination of NCN Pincer Iron Complexes Containing
 Bis(oxazolinyl)phenyl Ligands
;
_journal_issue                   23
_journal_name_full               Organometallics
_journal_page_first              8283
_journal_paper_doi               10.1021/om300901k
_journal_volume                  31
_journal_year                    2012
_chemical_formula_sum            'C35 H54 Br Fe N5 O3'
_chemical_formula_weight         728.59
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           63
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-C 2c 2'
_symmetry_space_group_name_H-M   'C m c m'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.304(4)
_cell_length_b                   17.373(4)
_cell_length_c                   14.898(4)
_cell_measurement_reflns_used    1753
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.11
_cell_measurement_theta_min      2.34
_cell_volume                     4478.7(19)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0707
_diffrn_reflns_av_sigmaI/netI    0.0591
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            16776
_diffrn_reflns_theta_full        28.43
_diffrn_reflns_theta_max         28.43
_diffrn_reflns_theta_min         2.15
_exptl_absorpt_coefficient_mu    1.261
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.734197
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.081
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1536
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.676
_refine_diff_density_min         -0.628
_refine_diff_density_rms         0.164
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.106
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     139
_refine_ls_number_reflns         3018
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.105
_refine_ls_R_factor_all          0.1088
_refine_ls_R_factor_gt           0.0781
_refine_ls_shift/su_max          0.018
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.1291P)²+20.8860P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2311
_refine_ls_wR_factor_ref         0.2513
_reflns_number_gt                1998
_reflns_number_total             3018
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om300901k_si_001.cif
_cod_data_source_block           7a
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from
2011-04-26.

'_exptl_absorpt_correction_type' value 'Empirical'
changed to 'empirical' according to
/home/saulius/struct/CIF-dictionaries/cif_core.dic dictionary named
'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 
;
_cod_original_cell_volume        4478.7(17)
_cod_original_sg_symbol_H-M      Cmcm
_cod_database_code               4079642
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'-x, y, -z+1/2'
'x, -y, -z'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x, y, -z-1/2'
'x, -y, z-1/2'
'-x, y, z'
'-x+1/2, -y+1/2, -z'
'x+1/2, y+1/2, -z-1/2'
'x+1/2, -y+1/2, z-1/2'
'-x+1/2, y+1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.5000 0.77140(6) 0.2500 0.0224(3) Uani 1 4 d S . .
N1 N 0.5000 0.7943(3) 0.1177(4) 0.0303(12) Uani 1 2 d S . .
N2 N 0.6757(4) 0.7695(4) 0.2500 0.0455(16) Uani 1 2 d S A .
N3 N 0.5000 0.5956(5) 0.2500 0.039(2) Uani 1 4 d S . .
O1 O 0.5000 0.8849(3) 0.0102(4) 0.081(3) Uani 1 2 d S . .
Br1 Br 0.5000 0.72413(5) 0.7500 0.0313(3) Uani 1 4 d S . .
C1 C 0.5000 0.8813(5) 0.2500 0.036(2) Uani 1 4 d S . .
C2 C 0.5000 0.9214(4) 0.1704(5) 0.057(2) Uani 1 2 d S . .
C3 C 0.5000 1.0029(5) 0.1697(6) 0.089(5) Uani 1 2 d S . .
H3 H 0.5000 1.0307 0.1147 0.107 Uiso 1 2 calc SR . .
C4 C 0.5000 1.0402(7) 0.2500 0.112(9) Uani 1 4 d S . .
H4 H 0.5000 1.0949 0.2500 0.135 Uiso 1 4 calc SR . .
C5 C 0.5000 0.8659(4) 0.0978(5) 0.051(2) Uani 1 2 d S . .
C6 C 0.5000 0.8141(5) -0.0387(6) 0.078(4) Uani 1 2 d S . .
H6A H 0.5465 0.8103 -0.0772 0.093 Uiso 0.50 1 calc PR . .
H6B H 0.4535 0.8103 -0.0772 0.093 Uiso 0.50 1 calc PR . .
C7 C 0.5000 0.7491(4) 0.0335(5) 0.0416(17) Uani 1 2 d S . .
C8 C 0.5714(5) 0.7006(4) 0.0266(5) 0.0645(18) Uani 1 1 d . . .
H8A H 0.6172 0.7333 0.0328 0.097 Uiso 1 1 calc R . .
H8B H 0.5725 0.6748 -0.0319 0.097 Uiso 1 1 calc R . .
H8C H 0.5712 0.6619 0.0744 0.097 Uiso 1 1 calc R . .
C9 C 0.6087(4) 0.7704(4) 0.2500 0.0348(15) Uani 1 2 d S . .
C10 C 0.7570(5) 0.7655(6) 0.2500 0.052(2) Uani 1 2 d S . .
C11 C 0.7867(12) 0.8210(12) 0.1751(13) 0.053(6) Uiso 0.330(17) 1 d P A 1
C12 C 0.783(3) 0.683(2) 0.2500 0.087(12) Uiso 0.330(17) 2 d SP A 1
C11A C 0.7883(13) 0.7748(13) 0.1569(17) 0.021(7) Uiso 0.170(17) 1 d P . 2
C12A C 0.785(6) 0.849(6) 0.2500 0.11(3) Uiso 0.170(17) 2 d SP . 2
C13 C 0.5000 0.6629(6) 0.2500 0.033(2) Uani 1 4 d S . .
C14 C 0.5000 0.5117(5) 0.2500 0.044(3) Uani 1 4 d S . .
C15 C 0.4615(14) 0.4863(12) 0.1647(17) 0.045(5) Uiso 0.25 1 d P . .
C16 C 0.4166(18) 0.4897(18) 0.2500 0.105(9) Uiso 0.50 2 d SP . .
O2 O 0.725(4) 0.5000 0.0000 0.31(3) Uiso 0.50 2 d SPD . .
C17 C 0.775(2) 0.437(3) -0.017(4) 0.24(2) Uiso 0.50 1 d PD . .
C18 C 0.8343(19) 0.4649(16) 0.038(2) 0.146(10) Uiso 0.50 1 d PD . .
C19 C 0.8114(18) 0.5097(19) 0.111(2) 0.152(10) Uiso 0.50 1 d PD . .
C20 C 0.738(2) 0.5344(18) 0.086(2) 0.160(13) Uiso 0.50 1 d PD . .
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'
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.2901 2.4595 '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
C9 Fe1 C9 179.0(4) 3_655 .
C9 Fe1 C13 89.5(2) 3_655 .
C9 Fe1 C13 89.5(2) . .
C9 Fe1 C1 90.5(2) 3_655 .
C9 Fe1 C1 90.5(2) . .
C13 Fe1 C1 180.000(2) . .
C9 Fe1 N1 90.10(4) 3_655 .
C9 Fe1 N1 90.10(4) . .
C13 Fe1 N1 101.43(15) . .
C1 Fe1 N1 78.57(15) . .
C9 Fe1 N1 90.10(4) 3_655 10_556
C9 Fe1 N1 90.10(4) . 10_556
C13 Fe1 N1 101.43(15) . 10_556
C1 Fe1 N1 78.57(15) . 10_556
N1 Fe1 N1 157.1(3) . 10_556
C5 N1 C7 108.6(6) . .
C5 N1 Fe1 114.8(5) . .
C7 N1 Fe1 136.5(4) . .
C9 N2 C10 177.9(8) . .
C13 N3 C14 180.000(3) . .
C5 O1 C6 106.5(6) . .
C2 C1 C2 119.1(9) 10_556 .
C2 C1 Fe1 120.4(4) 10_556 .
C2 C1 Fe1 120.4(4) . .
C1 C2 C3 120.9(7) . .
C1 C2 C5 107.9(6) . .
C3 C2 C5 131.3(7) . .
C4 C3 C2 118.0(8) . .
C3 C4 C3 123.0(11) . 10_556
N1 C5 O1 117.6(6) . .
N1 C5 C2 118.3(6) . .
O1 C5 C2 124.1(6) . .
O1 C6 C7 105.8(6) . .
N1 C7 C8 110.9(4) . .
N1 C7 C8 110.9(4) . 12_655
C8 C7 C8 111.0(8) . 12_655
N1 C7 C6 101.5(5) . .
C8 C7 C6 111.1(5) . .
C8 C7 C6 111.1(5) 12_655 .
N2 C9 Fe1 179.8(6) . .
N2 C10 C11A 110.8(10) . .
N2 C10 C11A 110.8(10) . 10_556
C11A C10 C11A 135.6(19) . 10_556
N2 C10 C12 110.5(19) . .
C11A C10 C12 89.6(12) . .
C11A C10 C12 89.6(12) 10_556 .
N2 C10 C12A 105(4) . .
C11A C10 C12A 77.6(16) . .
C11A C10 C12A 77.6(16) 10_556 .
C12 C10 C12A 144(5) . .
N2 C10 C11 107.3(9) . .
C11A C10 C11 32.1(9) . .
C11A C10 C11 118.4(14) 10_556 .
C12 C10 C11 119.3(13) . .
C12A C10 C11 46.4(10) . .
N2 C10 C11 107.3(9) . 10_556
C11A C10 C11 118.4(14) . 10_556
C11A C10 C11 32.1(9) 10_556 10_556
C12 C10 C11 119.3(13) . 10_556
C12A C10 C11 46.4(10) . 10_556
C11 C10 C11 91.2(16) . 10_556
C10 C11A C12A 52(3) . .
C10 C12A C11A 50(2) . .
C10 C12A C11A 50(2) . 10_556
C11A C12A C11A 94(5) . 10_556
N3 C13 Fe1 180.000(1) . .
N3 C14 C16 104.8(12) . 3_655
N3 C14 C16 104.8(12) . .
C16 C14 C16 150(2) 3_655 .
N3 C14 C15 107.1(9) . 12_655
C16 C14 C15 59.7(9) 3_655 12_655
C16 C14 C15 110.7(11) . 12_655
N3 C14 C15 107.1(9) . .
C16 C14 C15 110.7(11) 3_655 .
C16 C14 C15 59.7(9) . .
C15 C14 C15 52.6(18) 12_655 .
N3 C14 C15 107.1(9) . 3_655
C16 C14 C15 59.7(9) 3_655 3_655
C16 C14 C15 110.7(11) . 3_655
C15 C14 C15 115.7(18) 12_655 3_655
C15 C14 C15 145.8(18) . 3_655
N3 C14 C15 107.1(9) . 10_556
C16 C14 C15 110.7(11) 3_655 10_556
C16 C14 C15 59.7(9) . 10_556
C15 C14 C15 145.8(18) 12_655 10_556
C15 C14 C15 115.7(18) . 10_556
C15 C14 C15 52.6(18) 3_655 10_556
C15 C15 C16 121.4(14) 12_655 .
C15 C15 C14 63.7(9) 12_655 .
C16 C15 C14 59.8(15) . .
C15 C16 C15 117(3) 10_556 .
C15 C16 C14 60.4(14) 10_556 .
C15 C16 C14 60.4(14) . .
C17 O2 C17 104(7) 4_565 .
C17 O2 C20 55(2) 4_565 .
C17 O2 C20 113(4) . .
C17 O2 C20 113(4) 4_565 4_565
C17 O2 C20 55(2) . 4_565
C20 O2 C20 162(7) . 4_565
C20 C17 C18 134(5) 4_565 .
C20 C17 O2 62.8(14) 4_565 .
C18 C17 O2 95(4) . .
C20 C17 C19 51(2) 4_565 4_565
C18 C17 C19 91(4) . 4_565
O2 C17 C19 88(3) . 4_565
C20 C17 C18 79(3) 4_565 4_565
C18 C17 C18 55(3) . 4_565
O2 C17 C18 72(4) . 4_565
C19 C17 C18 42.5(14) 4_565 4_565
C19 C18 C17 116(3) . .
C19 C18 C18 97(3) . 4_565
C17 C18 C18 82(3) . 4_565
C19 C18 C17 60(2) . 4_565
C17 C18 C17 80(3) . 4_565
C18 C18 C17 43.5(13) 4_565 4_565
C18 C19 C20 103(3) . .
C18 C19 C17 77(2) . 4_565
C20 C19 C17 47(2) . 4_565
C17 C20 C19 83(4) 4_565 .
C17 C20 O2 62.6(15) 4_565 .
C19 C20 O2 105(3) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C9 1.881(7) 3_655
Fe1 C9 1.881(7) .
Fe1 C13 1.886(10) .
Fe1 C1 1.909(9) .
Fe1 N1 2.010(5) .
Fe1 N1 2.010(5) 10_556
N1 C5 1.278(9) .
N1 C7 1.482(9) .
N2 C9 1.160(10) .
N2 C10 1.408(10) .
N3 C13 1.168(12) .
N3 C14 1.458(12) .
O1 C5 1.346(9) .
O1 C6 1.430(9) .
C1 C2 1.375(8) 10_556
C1 C2 1.375(8) .
C2 C3 1.416(11) .
C2 C5 1.448(10) .
C3 C4 1.362(11) .
C4 C3 1.362(11) 10_556
C6 C7 1.559(11) .
C7 C8 1.499(8) .
C7 C8 1.499(8) 12_655
C10 C11A 1.50(2) .
C10 C11A 1.50(2) 10_556
C10 C12 1.50(4) .
C10 C12A 1.54(10) .
C10 C11 1.56(2) .
C10 C11 1.56(2) 10_556
C11A C12A 1.90(7) .
C12A C11A 1.90(7) 10_556
C14 C16 1.49(3) 3_655
C14 C16 1.49(3) .
C14 C15 1.50(2) 12_655
C14 C15 1.50(2) .
C14 C15 1.50(2) 3_655
C14 C15 1.50(2) 10_556
C15 C15 1.33(5) 12_655
C15 C16 1.49(3) .
C16 C15 1.49(3) 10_556
O2 C17 1.42(4) 4_565
O2 C17 1.42(4) .
O2 C20 1.43(4) .
O2 C20 1.43(4) 4_565
C17 C20 1.31(5) 4_565
C17 C18 1.40(3) .
C17 C19 1.79(7) 4_565
C17 C18 2.01(6) 4_565
C18 C19 1.39(3) .
C18 C18 1.66(6) 4_565
C18 C17 2.01(6) 4_565
C19 C20 1.40(3) .
C19 C17 1.79(7) 4_565
C20 C17 1.31(6) 4_565
