#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:39:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178661 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077204.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_4077204
loop_
_publ_author_name
'Yamaguchi, Takeshi'
'Ueno, Keiji'
'Ogino, Hiroshi'
_publ_section_title
;
 Synthesis and Structures of Mesitylgallylene-Bridged Diiron Complexes
 [Cp‘Fe(CO)]2(μ-CO)(μ-GaMes) (Cp‘ = η-C5Me5, η-C5H5; Mes
 = 2,4,6-Trimethylphenyl) and Kinetic Study of the Cis−Trans
 Isomerization of [(η-C5H5)Fe(CO)]2(μ-CO)(μ-GaMes)
;
_journal_issue                   3
_journal_name_full               Organometallics
_journal_page_first              501
_journal_paper_doi               10.1021/om000675a
_journal_volume                  20
_journal_year                    2001
_chemical_formula_moiety         '[(C5 (C H3)5) Fe (C O)2]2 (Ga C9 H11)'
_chemical_formula_sum            'C33 H41 Fe2 Ga O4'
_chemical_formula_weight         683.08
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           88
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_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            8
_cell_length_a                   14.484(8)
_cell_length_b                   14.484(8)
_cell_length_c                   31.703(15)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      12.70
_cell_measurement_theta_min      10.02
_cell_volume                     6651(6)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        TeXsan
_computing_molecular_graphics    ORTEP
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.492
_diffrn_measured_fraction_theta_max 0.492
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       ω-2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0626
_diffrn_reflns_av_sigmaI/netI    0.2084
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            4130
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         1.55
_diffrn_standards_decay_%        0.444
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.698
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.8797
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.364
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             2832
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.30
_refine_diff_density_max         0.335
_refine_diff_density_min         -0.327
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.933
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     190
_refine_ls_number_reflns         3832
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.933
_refine_ls_R_factor_all          0.2371
_refine_ls_R_factor_gt           0.0629
_refine_ls_shift/su_max          0.503
_refine_ls_shift/su_mean         0.012
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0474P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1087
_refine_ls_wR_factor_ref         0.1543
_reflns_number_gt                1367
_reflns_number_total             3832
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000675a.cif
_cod_data_source_block           '[(C5Me5)Fe(CO)2]2(GaMes)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0474P)^2^+0.0000P] 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^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_sg_symbol_H-M      'I 41/a'
_cod_database_code               4077204
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-y-1/4, x+1/4, z+1/4'
'-x, -y+1/2, z'
'y+1/4, -x+1/4, z+1/4'
'x+1/2, y+1/2, z+1/2'
'-y+1/4, x+3/4, z+3/4'
'-x+1/2, -y+1, z+1/2'
'y+3/4, -x+3/4, z+3/4'
'-x, -y, -z'
'y+1/4, -x-1/4, -z-1/4'
'x, y-1/2, -z'
'-y-1/4, x-1/4, -z-1/4'
'-x+1/2, -y+1/2, -z+1/2'
'y+3/4, -x+1/4, -z+1/4'
'x+1/2, y, -z+1/2'
'-y+1/4, x+1/4, -z+1/4'
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_calc_flag
_atom_site_refinement_flags
Ga Ga 0.0000 0.2500 0.37535(3) 0.0459(3) Uani 1 d S
Fe1 Fe -0.04571(8) 0.39131(7) 0.41110(3) 0.0496(3) Uani 1 d .
O1 O -0.1036(4) 0.2797(4) 0.48179(17) 0.093(2) Uani 1 d .
O2 O 0.1525(4) 0.3979(4) 0.42338(19) 0.0847(19) Uani 1 d .
C1 C -0.0767(6) 0.3200(5) 0.4528(2) 0.063(2) Uani 1 d .
C2 C 0.0723(6) 0.3919(5) 0.4193(2) 0.059(2) Uani 1 d .
C3 C -0.1803(6) 0.4409(5) 0.4020(3) 0.063(2) Uani 1 d .
C4 C -0.1309(7) 0.4992(6) 0.4309(2) 0.066(2) Uani 1 d .
C5 C -0.0544(6) 0.5349(5) 0.4091(3) 0.069(2) Uani 1 d .
C6 C -0.0566(6) 0.5002(6) 0.3674(3) 0.068(2) Uani 1 d .
C7 C -0.1338(7) 0.4464(6) 0.3632(2) 0.066(2) Uani 1 d .
C8 C -0.2691(6) 0.3918(7) 0.4102(4) 0.123(4) Uani 1 d .
H8A H -0.3196 0.4296 0.4010 0.184 Uiso 1 calc R
H8B H -0.2749 0.3797 0.4398 0.184 Uiso 1 calc R
H8C H -0.2697 0.3345 0.3950 0.184 Uiso 1 calc R
C9 C -0.1583(8) 0.5204(7) 0.4755(3) 0.121(4) Uani 1 d .
H9A H -0.1046 0.5378 0.4914 0.181 Uiso 1 calc R
H9B H -0.1858 0.4667 0.4880 0.181 Uiso 1 calc R
H9C H -0.2020 0.5702 0.4757 0.181 Uiso 1 calc R
C10 C 0.0142(7) 0.6034(6) 0.4274(4) 0.134(5) Uani 1 d .
H10A H -0.0023 0.6648 0.4189 0.202 Uiso 1 calc R
H10B H 0.0751 0.5892 0.4174 0.202 Uiso 1 calc R
H10C H 0.0132 0.5995 0.4577 0.202 Uiso 1 calc R
C11 C 0.0084(8) 0.5289(7) 0.3324(3) 0.142(5) Uani 1 d .
H11A H 0.0078 0.4831 0.3105 0.213 Uiso 1 calc R
H11B H 0.0698 0.5348 0.3434 0.213 Uiso 1 calc R
H11C H -0.0112 0.5872 0.3210 0.213 Uiso 1 calc R
C12 C -0.1722(8) 0.4122(7) 0.3214(3) 0.125(5) Uani 1 d .
H12A H -0.2014 0.4624 0.3068 0.188 Uiso 1 calc R
H12B H -0.2167 0.3643 0.3265 0.188 Uiso 1 calc R
H12C H -0.1228 0.3882 0.3044 0.188 Uiso 1 calc R
C13 C 0.0000 0.2500 0.3118(3) 0.062(3) Uani 1 d S
C14 C 0.0736(8) 0.2886(6) 0.2894(3) 0.084(3) Uani 1 d .
C15 C 0.0694(10) 0.2877(8) 0.2452(3) 0.142(6) Uani 1 d .
H15 H 0.1176 0.3150 0.2305 0.170 Uiso 1 calc R
C16 C 0.0000 0.2500 0.2228(4) 0.185(15) Uani 1 d S
C17 C 0.1551(7) 0.3286(6) 0.3125(4) 0.114(4) Uani 1 d .
H17A H 0.1623 0.2978 0.3391 0.170 Uiso 1 calc R
H17B H 0.1450 0.3933 0.3172 0.170 Uiso 1 calc R
H17C H 0.2099 0.3204 0.2959 0.170 Uiso 1 calc R
C18 C 0.0000 0.2500 0.1751(4) 0.307(19) Uani 1 d S
H18A H 0.0534 0.2824 0.1650 0.460 Uiso 0.50 calc PR
H18B H -0.0548 0.2800 0.1650 0.460 Uiso 0.50 calc PR
H18C H 0.0014 0.1875 0.1650 0.460 Uiso 0.50 calc PR
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'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ga Ga 0.2307 1.6083 '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'
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
C13 Ga Fe1 117.79(4) . .
C13 Ga Fe1 117.79(4) . 3
Fe1 Ga Fe1 124.42(7) . 3
C2 Fe1 C1 98.3(4) . .
C2 Fe1 C5 93.4(4) . .
C1 Fe1 C5 126.9(4) . .
C2 Fe1 C4 122.4(4) . .
C1 Fe1 C4 93.7(3) . .
C5 Fe1 C4 39.3(3) . .
C2 Fe1 C3 159.7(3) . .
C1 Fe1 C3 93.9(3) . .
C5 Fe1 C3 66.3(3) . .
C4 Fe1 C3 40.1(3) . .
C2 Fe1 C6 99.7(4) . .
C1 Fe1 C6 158.0(3) . .
C5 Fe1 C6 39.5(3) . .
C4 Fe1 C6 65.9(3) . .
C3 Fe1 C6 65.4(3) . .
C2 Fe1 C7 134.0(4) . .
C1 Fe1 C7 127.5(4) . .
C5 Fe1 C7 64.5(3) . .
C4 Fe1 C7 65.2(3) . .
C3 Fe1 C7 38.7(3) . .
C6 Fe1 C7 37.6(3) . .
C2 Fe1 Ga 78.7(2) . .
C1 Fe1 Ga 85.7(2) . .
C5 Fe1 Ga 147.4(3) . .
C4 Fe1 Ga 158.6(3) . .
C3 Fe1 Ga 118.5(2) . .
C6 Fe1 Ga 110.1(2) . .
C7 Fe1 Ga 98.4(2) . .
O1 C1 Fe1 172.9(7) . .
O2 C2 Fe1 175.5(8) . .
C7 C3 C4 106.6(7) . .
C7 C3 C8 126.3(9) . .
C4 C3 C8 126.8(9) . .
C7 C3 Fe1 72.2(5) . .
C4 C3 Fe1 69.6(5) . .
C8 C3 Fe1 127.9(6) . .
C5 C4 C3 107.3(7) . .
C5 C4 C9 126.6(9) . .
C3 C4 C9 126.0(10) . .
C5 C4 Fe1 70.2(5) . .
C3 C4 Fe1 70.3(4) . .
C9 C4 Fe1 126.3(6) . .
C4 C5 C6 108.1(7) . .
C4 C5 C10 124.7(10) . .
C6 C5 C10 127.2(10) . .
C4 C5 Fe1 70.5(5) . .
C6 C5 Fe1 71.0(4) . .
C10 C5 Fe1 126.9(6) . .
C7 C6 C5 108.1(7) . .
C7 C6 C11 126.4(9) . .
C5 C6 C11 125.0(10) . .
C7 C6 Fe1 72.4(5) . .
C5 C6 Fe1 69.5(4) . .
C11 C6 Fe1 129.9(6) . .
C6 C7 C3 109.9(7) . .
C6 C7 C12 124.6(9) . .
C3 C7 C12 124.7(10) . .
C6 C7 Fe1 69.9(5) . .
C3 C7 Fe1 69.1(4) . .
C12 C7 Fe1 135.7(6) . .
C14 C13 C14 118.9(11) 3 .
C14 C13 Ga 120.5(6) 3 .
C14 C13 Ga 120.5(6) . .
C13 C14 C15 118.1(12) . .
C13 C14 C17 120.3(8) . .
C15 C14 C17 121.6(11) . .
C16 C15 C14 124.4(14) . .
C15 C16 C15 116.2(14) . 3
C15 C16 C18 121.9(7) . .
C15 C16 C18 121.9(7) 3 .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga C13 2.014(10) .
Ga Fe1 2.4315(15) .
Ga Fe1 2.4315(15) 3
Fe1 C2 1.729(9) .
Fe1 C1 1.736(9) .
Fe1 C5 2.085(8) .
Fe1 C4 2.088(8) .
Fe1 C3 2.097(8) .
Fe1 C6 2.105(7) .
Fe1 C7 2.137(8) .
O1 C1 1.157(8) .
O2 C2 1.172(8) .
C3 C7 1.404(11) .
C3 C4 1.436(11) .
C3 C8 1.492(11) .
C4 C5 1.403(11) .
C4 C9 1.502(10) .
C5 C6 1.415(11) .
C5 C10 1.519(11) .
C6 C7 1.369(11) .
C6 C11 1.514(10) .
C7 C12 1.523(11) .
C13 C14 1.398(10) 3
C13 C14 1.398(10) .
C14 C15 1.402(12) .
C14 C17 1.505(13) .
C15 C16 1.347(13) .
C16 C15 1.347(13) 3
C16 C18 1.511(17) .
