#------------------------------------------------------------------------------
#$Date: 2016-03-22 11:35:40 +0200 (Tue, 22 Mar 2016) $
#$Revision: 178906 $
#$URL: svn://www.crystallography.net/cod/cif/4/11/35/4113514.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_4113514
loop_
_publ_author_name
'Ned J. Hardman'
'Robert J. Wright'
'Andrew D. Phillips'
'Philip P. Power'
_publ_section_title
;
 Structures, Bonding, and Reaction Chemistry of the Neutral
 Organogallium(I) Compounds (GaAr)n (n= 1 or 2) (Ar = Terphenyl or Related
 Ligand): An Experimental Investigation of Ga-Ga Multiple Bonding
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2667
_journal_page_last               2679
_journal_paper_doi               10.1021/ja028579j
_journal_volume                  125
_journal_year                    2003
_chemical_formula_sum            'C40 H49 Fe Ga N2 O4'
_chemical_formula_weight         747.38
_chemical_melting_point          553
_chemical_name_common            Dipp2N^NGaFe(CO)4
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           62
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2n'
_symmetry_space_group_name_H-M   'P n m a'
_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                   22.0914(8)
_cell_length_b                   16.5373(6)
_cell_length_c                   10.5410(4)
_cell_measurement_reflns_used    6572
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      31.4
_cell_measurement_theta_min      2.2
_cell_volume                     3851.0(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'SHELXTL 5, XP (Sheldrick, 1994)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      90(2)
_diffrn_detector_area_resol_mean 8.3
_diffrn_measured_fraction_theta_full 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  'Bruker SMART 1000'
_diffrn_measurement_method       ω
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0288
_diffrn_reflns_av_sigmaI/netI    0.0160
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            53468
_diffrn_reflns_theta_full        31.48
_diffrn_reflns_theta_max         31.48
_diffrn_reflns_theta_min         1.84
_diffrn_standards_decay_%        <0.1
_diffrn_standards_interval_time
;
frames measured at beginning and end of data collection
;
_diffrn_standards_number         '50 frames remeasured'
_exptl_absorpt_coefficient_mu    1.117
_exptl_absorpt_correction_T_max  0.7027
_exptl_absorpt_correction_T_min  0.6393
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SADABS 2.0 (Sheldrick, 2000)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_description       block
_exptl_crystal_F_000             1568
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.34
_refine_diff_density_max         1.005
_refine_diff_density_min         -0.694
_refine_diff_density_rms         0.076
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         6505
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0412
_refine_ls_R_factor_gt           0.0330
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0522P)²+2.3054P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0886
_refine_ls_wR_factor_ref         0.0948
_reflns_number_gt                5607
_reflns_number_total             6505
_reflns_threshold_expression     I>2/s(I)
_cod_data_source_file            ja028579jsi20021203_051446.cif
_cod_data_source_block           nh15
_cod_database_code               4113514
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Ga1 Ga 0.347816(8) 0.2500 0.351324(19) 0.01321(6) Uani 1 2 d S . .
N1 N 0.40292(5) 0.16332(6) 0.39134(10) 0.01427(19) Uani 1 1 d . . .
O1 O 0.22424(6) 0.09433(7) 0.37522(13) 0.0317(3) Uani 1 1 d . . .
C1 C 0.46255(6) 0.17405(8) 0.40864(13) 0.0172(2) Uani 1 1 d . . .
Fe1 Fe 0.254801(12) 0.2500 0.25649(3) 0.01543(7) Uani 1 2 d S . .
C2 C 0.49019(8) 0.2500 0.4086(2) 0.0186(3) Uani 1 2 d S . .
O2 O 0.32487(8) 0.2500 0.01963(16) 0.0318(4) Uani 1 2 d S . .
O3 O 0.14026(8) 0.2500 0.1193(2) 0.0376(4) Uani 1 2 d S . .
C3 C 0.50305(6) 0.10241(9) 0.43283(17) 0.0255(3) Uani 1 1 d . . .
H3A H 0.4891 0.0563 0.3823 0.038 Uiso 1 1 calc R . .
H3B H 0.5017 0.0883 0.5231 0.038 Uiso 1 1 calc R . .
H3C H 0.5447 0.1160 0.4089 0.038 Uiso 1 1 calc R . .
C4 C 0.37763(6) 0.08324(8) 0.40941(12) 0.0150(2) Uani 1 1 d . . .
C5 C 0.36940(6) 0.03229(8) 0.30391(13) 0.0174(2) Uani 1 1 d . . .
C6 C 0.34560(7) -0.04488(9) 0.32569(15) 0.0228(3) Uani 1 1 d . . .
H6A H 0.3404 -0.0809 0.2563 0.027 Uiso 1 1 calc R . .
C7 C 0.32948(7) -0.06984(9) 0.44654(15) 0.0247(3) Uani 1 1 d . . .
H7A H 0.3136 -0.1226 0.4594 0.030 Uiso 1 1 calc R . .
C8 C 0.33648(7) -0.01790(9) 0.54879(14) 0.0219(3) Uani 1 1 d . . .
H8A H 0.3248 -0.0353 0.6311 0.026 Uiso 1 1 calc R . .
C9 C 0.36049(6) 0.05967(8) 0.53256(13) 0.0175(2) Uani 1 1 d . . .
C10 C 0.38436(6) 0.05794(9) 0.16928(13) 0.0205(3) Uani 1 1 d . . .
H10A H 0.3934 0.1172 0.1701 0.025 Uiso 1 1 calc R . .
C11 C 0.33062(8) 0.04397(11) 0.08069(15) 0.0293(3) Uani 1 1 d . . .
H11A H 0.2948 0.0712 0.1149 0.044 Uiso 1 1 calc R . .
H11B H 0.3227 -0.0142 0.0738 0.044 Uiso 1 1 calc R . .
H11C H 0.3400 0.0659 -0.0034 0.044 Uiso 1 1 calc R . .
C12 C 0.44009(9) 0.01388(16) 0.11825(19) 0.0465(5) Uani 1 1 d . . .
H12A H 0.4755 0.0285 0.1692 0.070 Uiso 1 1 calc R . .
H12B H 0.4469 0.0296 0.0298 0.070 Uiso 1 1 calc R . .
H12C H 0.4335 -0.0446 0.1230 0.070 Uiso 1 1 calc R . .
C13 C 0.36585(7) 0.11531(9) 0.64678(13) 0.0215(3) Uani 1 1 d . . .
H13A H 0.3832 0.1679 0.6172 0.026 Uiso 1 1 calc R . .
C14 C 0.30324(8) 0.13233(13) 0.70429(17) 0.0341(4) Uani 1 1 d . . .
H14A H 0.2768 0.1556 0.6392 0.051 Uiso 1 1 calc R . .
H14B H 0.3074 0.1705 0.7748 0.051 Uiso 1 1 calc R . .
H14C H 0.2856 0.0817 0.7355 0.051 Uiso 1 1 calc R . .
C15 C 0.40818(8) 0.08044(13) 0.74802(16) 0.0338(4) Uani 1 1 d . . .
H15A H 0.4487 0.0734 0.7121 0.051 Uiso 1 1 calc R . .
H15B H 0.3927 0.0280 0.7765 0.051 Uiso 1 1 calc R . .
H15C H 0.4102 0.1176 0.8203 0.051 Uiso 1 1 calc R . .
C16 C 0.23862(6) 0.15524(9) 0.33223(14) 0.0216(3) Uani 1 1 d . . .
C17 C 0.29869(9) 0.2500 0.1152(2) 0.0215(4) Uani 1 2 d S . .
C18 C 0.18491(10) 0.2500 0.1740(2) 0.0245(4) Uani 1 2 d S . .
C19 C 0.0957(2) 0.2500 0.5155(4) 0.0616(9) Uani 1 2 d S A 1
H19A H 0.1010 0.2500 0.4261 0.074 Uiso 1 2 calc SR A 1
C20 C 0.14484(18) 0.2500 0.5898(4) 0.0543(8) Uani 1 2 d S A 1
H20A H 0.1839 0.2500 0.5520 0.065 Uiso 1 2 calc SR A 1
C21 C 0.13989(14) 0.2500 0.7166(3) 0.0392(6) Uani 1 2 d S A 1
H21A H 0.1757 0.2500 0.7666 0.047 Uiso 1 2 calc SR A 1
C22 C 0.08455(15) 0.2500 0.7762(3) 0.0429(6) Uani 1 2 d S A 1
H22A H 0.0820 0.2500 0.8661 0.051 Uiso 1 2 calc SR A 1
C23 C 0.03189(16) 0.2500 0.7016(5) 0.0631(11) Uani 1 2 d S A 1
H23A H -0.0070 0.2500 0.7402 0.076 Uiso 1 2 calc SR A 1
C24 C 0.0379(2) 0.2500 0.5635(4) 0.0649(11) Uani 1 2 d S A 1
C25 C -0.0172(2) 0.2500 0.4775(7) 0.0992(19) Uani 1 2 d S A 1
H2A H 0.5326(12) 0.2500 0.415(3) 0.020(6) Uiso 1 2 d S B 1
C19B C 0.0060 0.2500 0.6278 0.050 Uiso 0.12 2 d SP C 2
C20B C 0.0204 0.2500 0.7552 0.050 Uiso 0.12 2 d SP C 2
C21B C 0.0784 0.2500 0.7920 0.050 Uiso 0.12 2 d SP C 2
C22B C 0.1243 0.2500 0.7044 0.050 Uiso 0.12 2 d SP C 2
C23B C 0.1130 0.2500 0.5753 0.050 Uiso 0.12 2 d SP C 2
C24B C 0.0499 0.2500 0.5356 0.050 Uiso 0.12 2 d SP C 2
C25B C 0.0393 0.2500 0.3919 0.050 Uiso 0.12 2 d SP C 2
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'
Ga Ga 0.2307 1.6083 '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 Ga1 N1 96.10(6) 7_565 .
N1 Ga1 Fe1 131.59(3) 7_565 .
N1 Ga1 Fe1 131.59(3) . .
C1 N1 C4 118.77(11) . .
C1 N1 Ga1 123.47(9) . .
C4 N1 Ga1 117.69(8) . .
N1 C1 C2 123.25(13) . .
N1 C1 C3 120.14(12) . .
C2 C1 C3 116.59(12) . .
C18 Fe1 C17 93.66(10) . .
C18 Fe1 C16 92.57(6) . .
C17 Fe1 C16 118.78(5) . .
C18 Fe1 C16 92.57(6) . 7_565
C17 Fe1 C16 118.78(5) . 7_565
C16 Fe1 C16 121.66(10) . 7_565
C18 Fe1 Ga1 176.54(8) . .
C17 Fe1 Ga1 82.88(7) . .
C16 Fe1 Ga1 89.11(5) . .
C16 Fe1 Ga1 89.11(5) 7_565 .
C1 C2 C1 128.14(17) . 7_565
C5 C4 C9 121.90(12) . .
C5 C4 N1 119.54(11) . .
C9 C4 N1 118.54(11) . .
C6 C5 C4 117.71(13) . .
C6 C5 C10 119.36(13) . .
C4 C5 C10 122.92(12) . .
C7 C6 C5 121.28(14) . .
C6 C7 C8 120.09(13) . .
C7 C8 C9 121.01(13) . .
C8 C9 C4 117.97(13) . .
C8 C9 C13 119.20(12) . .
C4 C9 C13 122.82(12) . .
C5 C10 C11 111.09(12) . .
C5 C10 C12 111.80(13) . .
C11 C10 C12 109.80(14) . .
C9 C13 C15 111.81(13) . .
C9 C13 C14 110.69(13) . .
C15 C13 C14 110.10(13) . .
O1 C16 Fe1 174.71(13) . .
O2 C17 Fe1 176.80(19) . .
O3 C18 Fe1 179.1(2) . .
C20 C19 C24 122.6(4) . .
C19 C20 C21 121.1(4) . .
C20 C21 C22 121.9(3) . .
C21 C22 C23 118.7(3) . .
C22 C23 C24 118.8(3) . .
C19 C24 C23 116.9(3) . .
C19 C24 C25 121.7(5) . .
C23 C24 C25 121.4(5) . .
C24B C19B C20B 121.8 . .
C21B C20B C19B 120.2 . .
C20B C21B C22B 120.9 . .
C21B C22B C23B 121.9 . .
C22B C23B C24B 117.2 . .
C19B C24B C23B 118.2 . .
C19B C24B C25B 126.4 . .
C23B C24B C25B 115.5 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Ga1 N1 1.9273(11) 7_565
Ga1 N1 1.9273(11) .
Ga1 Fe1 2.2851(3) .
N1 C1 1.3416(16) .
N1 C4 1.4499(16) .
O1 C16 1.1493(19) .
C1 C2 1.3965(15) .
C1 C3 1.5064(19) .
Fe1 C18 1.772(2) .
Fe1 C17 1.777(2) .
Fe1 C16 1.7946(15) .
Fe1 C16 1.7946(15) 7_565
C2 C1 1.3965(15) 7_565
O2 C17 1.162(3) .
O3 C18 1.142(3) .
C4 C5 1.4071(18) .
C4 C9 1.4073(18) .
C5 C6 1.399(2) .
C5 C10 1.5176(19) .
C6 C7 1.386(2) .
C7 C8 1.387(2) .
C8 C9 1.3986(19) .
C9 C13 1.5200(19) .
C10 C11 1.528(2) .
C10 C12 1.528(2) .
C13 C15 1.532(2) .
C13 C14 1.536(2) .
C19 C20 1.339(6) .
C19 C24 1.372(6) .
C20 C21 1.341(5) .
C21 C22 1.375(4) .
C22 C23 1.404(5) .
C23 C24 1.462(7) .
C24 C25 1.519(6) .
C19B C24B 1.3727 .
C19B C20B 1.3795 .
C20B C21B 1.3393 .
C21B C22B 1.3714 .
C22B C23B 1.3837 .
C23B C24B 1.4556 .
C24B C25B 1.5323 .
