#------------------------------------------------------------------------------
#$Date: 2016-03-21 10:39:08 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178661 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/72/4077205.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_4077205
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 (C O) (Ga C9 H11)'
_chemical_formula_sum            'C32 H41 Fe2 Ga O3'
_chemical_formula_weight         655.07
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_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                 99.59(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.090(6)
_cell_length_b                   17.178(9)
_cell_length_c                   12.532(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.98
_cell_measurement_theta_min      29.41
_cell_volume                     2991(2)
_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 0.485
_diffrn_measured_fraction_theta_max 0.485
_diffrn_measurement_device_type  'Rigaku AFC6S'
_diffrn_measurement_method       ω-2θ
_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  0.0183
_diffrn_reflns_av_sigmaI/netI    0.0259
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       0
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3615
_diffrn_reflns_theta_full        27.51
_diffrn_reflns_theta_max         27.51
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        -0.237
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    1.882
_exptl_absorpt_correction_T_max  0.9998
_exptl_absorpt_correction_T_min  0.9718
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.455
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             1360
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_refine_diff_density_max         0.276
_refine_diff_density_min         -0.294
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         3456
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.021
_refine_ls_R_factor_all          0.0451
_refine_ls_R_factor_gt           0.0276
_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/[σ²(Fo²)+(0.0379P)²+1.4813P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0737
_reflns_number_gt                2746
_reflns_number_total             3456
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om000675a.cif
_cod_data_source_block           '[(C5Me5)Fe(CO)]2(CO)(GaMes)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0379P)^2^+1.4813P] 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^)+(0.0379P)^2^+1.4813P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4077205
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -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_calc_flag
_atom_site_refinement_flags
Fe Fe 0.95819(2) 0.335666(17) 0.33950(2) 0.02732(9) Uani 1 d .
Ga Ga 1.0000 0.226254(19) 0.2500 0.02920(10) Uani 1 d S
O1 O 1.13667(13) 0.32659(12) 0.49156(15) 0.0533(5) Uani 1 d .
O2 O 1.0000 0.48523(13) 0.2500 0.0457(6) Uani 1 d S
C1 C 1.06701(17) 0.33058(13) 0.42774(18) 0.0356(5) Uani 1 d .
C2 C 1.0000 0.41610(18) 0.2500 0.0315(6) Uani 1 d S
C3 C 1.0000 0.11125(17) 0.2500 0.0319(6) Uani 1 d S
C4 C 1.04710(16) 0.06997(13) 0.34054(18) 0.0356(5) Uani 1 d .
C5 C 1.0462(2) -0.01093(15) 0.3380(2) 0.0451(6) Uani 1 d .
C6 C 1.0000 -0.0521(2) 0.2500 0.0488(9) Uani 1 d S
C7 C 1.0996(2) 0.11040(18) 0.4397(2) 0.0471(6) Uani 1 d .
C8 C 1.0000 -0.1404(2) 0.2500 0.0778(15) Uani 1 d S
H8A H 0.9445 -0.1590 0.2018 0.117 Uiso 0.50 calc PR
H8B H 0.9983 -0.1590 0.3219 0.117 Uiso 0.50 calc PR
H8C H 1.0573 -0.1590 0.2263 0.117 Uiso 0.50 calc PR
C9 C 0.81114(16) 0.29564(14) 0.30222(19) 0.0372(5) Uani 1 d .
C10 C 0.85384(16) 0.27062(14) 0.40770(19) 0.0368(5) Uani 1 d .
C11 C 0.88312(17) 0.33888(14) 0.47015(18) 0.0375(5) Uani 1 d .
C12 C 0.85759(16) 0.40526(14) 0.40411(19) 0.0375(5) Uani 1 d .
C13 C 0.81334(16) 0.37870(15) 0.29986(19) 0.0376(5) Uani 1 d .
C14 C 0.7586(2) 0.2445(2) 0.2142(3) 0.0541(7) Uani 1 d .
C15 C 0.8561(2) 0.18940(18) 0.4516(3) 0.0528(7) Uani 1 d .
C16 C 0.9239(3) 0.3401(2) 0.5890(2) 0.0558(8) Uani 1 d .
C17 C 0.8656(3) 0.48861(18) 0.4390(3) 0.0555(7) Uani 1 d .
C18 C 0.7691(2) 0.4302(2) 0.2085(3) 0.0564(8) Uani 1 d .
H14A H 0.694(2) 0.2427(18) 0.221(2) 0.069(9) Uiso 1 d .
H5 H 1.079(2) -0.0375(17) 0.398(2) 0.058(8) Uiso 1 d .
H14B H 0.777(2) 0.190(2) 0.224(3) 0.076(11) Uiso 1 d .
H18A H 0.804(3) 0.475(2) 0.198(3) 0.097(13) Uiso 1 d .
H14C H 0.769(3) 0.259(2) 0.146(3) 0.088(12) Uiso 1 d .
H18B H 0.712(3) 0.447(2) 0.218(3) 0.080(11) Uiso 1 d .
H18C H 0.765(3) 0.405(2) 0.141(3) 0.105(15) Uiso 1 d .
H16A H 0.959(3) 0.388(2) 0.606(3) 0.082(11) Uiso 1 d .
H7B H 1.084(3) 0.164(2) 0.447(3) 0.077(11) Uiso 1 d .
H16C H 0.971(3) 0.301(2) 0.604(3) 0.089(12) Uiso 1 d .
H15B H 0.912(3) 0.180(2) 0.497(3) 0.085(12) Uiso 1 d .
H15A H 0.852(3) 0.151(2) 0.395(3) 0.083(12) Uiso 1 d .
H7A H 1.165(2) 0.1121(19) 0.440(3) 0.070(10) Uiso 1 d .
H17B H 0.885(3) 0.522(2) 0.383(3) 0.087(12) Uiso 1 d .
H7C H 1.092(3) 0.086(2) 0.499(3) 0.090(12) Uiso 1 d .
H15C H 0.801(3) 0.1811(19) 0.488(3) 0.080(11) Uiso 1 d .
H17A H 0.798(3) 0.508(2) 0.455(3) 0.100(12) Uiso 1 d .
H17C H 0.904(3) 0.498(2) 0.498(3) 0.103(15) Uiso 1 d .
H16B H 0.877(3) 0.338(2) 0.627(3) 0.090(13) Uiso 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'
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
C1 Fe C2 94.78(8) . .
C1 Fe C11 90.62(10) . .
C2 Fe C11 132.68(9) . .
C1 Fe C12 111.19(10) . .
C2 Fe C12 96.12(9) . .
C11 Fe C12 39.42(9) . .
C1 Fe C10 108.21(10) . .
C2 Fe C10 154.60(7) . .
C11 Fe C10 39.57(9) . .
C12 Fe C10 65.95(10) . .
C1 Fe C13 150.22(10) . .
C2 Fe C13 89.40(8) . .
C11 Fe C13 65.64(9) . .
C12 Fe C13 39.04(9) . .
C10 Fe C13 65.28(9) . .
C1 Fe C9 146.65(10) . .
C2 Fe C9 118.46(7) . .
C11 Fe C9 65.53(9) . .
C12 Fe C9 65.34(9) . .
C10 Fe C9 38.74(9) . .
C13 Fe C9 38.70(10) . .
C1 Fe Ga 89.92(8) . .
C2 Fe Ga 99.93(7) . .
C11 Fe Ga 127.10(7) . .
C12 Fe Ga 152.26(7) . .
C10 Fe Ga 90.97(7) . .
C13 Fe Ga 118.41(7) . .
C9 Fe Ga 87.08(7) . .
C1 Fe Fe 93.88(8) . 2_755
C2 Fe Fe 45.64(7) . 2_755
C11 Fe Fe 175.32(7) . 2_755
C12 Fe Fe 136.92(7) . 2_755
C10 Fe Fe 139.19(7) . 2_755
C13 Fe Fe 109.68(7) . 2_755
C9 Fe Fe 110.85(7) . 2_755
Ga Fe Fe 54.289(19) . 2_755
C3 Ga Fe 144.289(19) . .
C3 Ga Fe 144.289(18) . 2_755
Fe Ga Fe 71.42(4) . 2_755
O1 C1 Fe 176.0(2) . .
O2 C2 Fe 135.64(7) . 2_755
O2 C2 Fe 135.64(7) . .
Fe C2 Fe 88.72(13) 2_755 .
C4 C3 C4 119.5(3) 2_755 .
C4 C3 Ga 120.26(14) 2_755 .
C4 C3 Ga 120.26(14) . .
C5 C4 C3 119.0(2) . .
C5 C4 C7 118.8(2) . .
C3 C4 C7 122.3(2) . .
C6 C5 C4 122.1(3) . .
C5 C6 C5 118.3(3) . 2_755
C5 C6 C8 120.84(17) . .
C5 C6 C8 120.85(17) 2_755 .
C13 C9 C10 108.3(2) . .
C13 C9 C14 125.3(3) . .
C10 C9 C14 125.7(3) . .
C13 C9 Fe 70.30(13) . .
C10 C9 Fe 69.73(13) . .
C14 C9 Fe 132.95(17) . .
C9 C10 C11 107.4(2) . .
C9 C10 C15 127.0(2) . .
C11 C10 C15 125.1(2) . .
C9 C10 Fe 71.53(13) . .
C11 C10 Fe 68.61(12) . .
C15 C10 Fe 131.31(18) . .
C12 C11 C10 108.5(2) . .
C12 C11 C16 125.7(2) . .
C10 C11 C16 125.5(2) . .
C12 C11 Fe 71.17(12) . .
C10 C11 Fe 71.82(12) . .
C16 C11 Fe 127.98(19) . .
C11 C12 C13 107.9(2) . .
C11 C12 C17 126.8(2) . .
C13 C12 C17 125.1(2) . .
C11 C12 Fe 69.41(13) . .
C13 C12 Fe 71.76(13) . .
C17 C12 Fe 129.03(19) . .
C9 C13 C12 108.0(2) . .
C9 C13 C18 126.7(3) . .
C12 C13 C18 125.1(3) . .
C9 C13 Fe 71.01(13) . .
C12 C13 Fe 69.20(13) . .
C18 C13 Fe 129.60(18) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe C1 1.737(2) .
Fe C2 1.932(2) .
Fe C11 2.093(2) .
Fe C12 2.116(2) .
Fe C10 2.135(2) .
Fe C13 2.150(2) .
Fe C9 2.159(2) .
Fe Ga 2.3147(9) .
Fe Fe 2.7022(11) 2_755
Ga C3 1.976(3) .
Ga Fe 2.3147(9) 2_755
O1 C1 1.160(3) .
O2 C2 1.188(4) .
C2 Fe 1.932(2) 2_755
C3 C4 1.407(3) 2_755
C3 C4 1.407(3) .
C4 C5 1.390(3) .
C4 C7 1.505(4) .
C5 C6 1.379(3) .
C6 C5 1.379(3) 2_755
C6 C8 1.516(5) .
C9 C13 1.428(4) .
C9 C10 1.424(3) .
C9 C14 1.505(4) .
C10 C11 1.432(3) .
C10 C15 1.498(4) .
C11 C12 1.420(3) .
C11 C16 1.505(4) .
C12 C13 1.426(3) .
C12 C17 1.496(4) .
C13 C18 1.498(4) .
