#------------------------------------------------------------------------------
#$Date: 2016-03-21 14:40:50 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178719 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/30/4083030.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_4083030
loop_
_publ_author_name
'Zhao, Pei'
'Brown, Zachary'
'Fettinger, James C.'
'Grandjean, Fernande'
'Long, Gary J.'
'Power, Philip P.'
_publ_section_title
;
 Synthesis and Structural Characterization of a Dimeric Cobalt(I)
 Homoleptic Alkyl and an Iron(II) Alkyl Halide Complex
;
_journal_issue                   8
_journal_name_full               Organometallics
_journal_page_first              1917
_journal_paper_doi               10.1021/om500180u
_journal_volume                  33
_journal_year                    2014
_chemical_formula_moiety         'C50 H66 Cl3 Fe2 Si6'
_chemical_formula_sum            'C50 H66 Cl3 Fe2 Si6'
_chemical_formula_weight         1053.61
_chemical_name_systematic
; 
 ? 
;
_space_group_crystal_system      hexagonal
_space_group_IT_number           176
_space_group_name_Hall           '-P 6c'
_space_group_name_H-M_alt        'P 63/m'
_symmetry_space_group_name_Hall  '-P 6c'
_symmetry_space_group_name_H-M   'P 63/m'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            2
_cell_length_a                   13.1170(3)
_cell_length_b                   13.1170(3)
_cell_length_c                   27.3137(8)
_cell_measurement_reflns_used    9875
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      68.22
_cell_measurement_theta_min      3.89
_cell_volume                     4069.87(18)
_computing_cell_refinement       'SAINT (8.27b) (Bruker, 2012)'
_computing_data_collection       'Apex2 (2012.2-0) (Bruker, 2012)'
_computing_data_reduction        'SAINT (8.27b) (Bruker, 2012)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      90(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0509
_diffrn_reflns_av_unetI/netI     0.0316
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            16507
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.232
_diffrn_reflns_theta_min         3.891
_exptl_absorpt_coefficient_mu    4.771
_exptl_absorpt_correction_T_max  0.2548
_exptl_absorpt_correction_T_min  0.1215
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2012/1 (Sheldrick, 2012)'
_exptl_crystal_colour            White
_exptl_crystal_density_diffrn    0.860
_exptl_crystal_description       Block
_exptl_crystal_F_000             1106
_exptl_crystal_size_max          0.693
_exptl_crystal_size_mid          0.544
_exptl_crystal_size_min          0.390
_refine_diff_density_max         0.461
_refine_diff_density_min         -0.186
_refine_diff_density_rms         0.043
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.155
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     96
_refine_ls_number_reflns         2554
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.155
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0427
_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)+(0.0265P)²+3.1745P] 
 where P=(Fo²+2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1070
_refine_ls_wR_factor_ref         0.1078
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2423
_reflns_number_total             2554
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om500180u_si_002.cif
_cod_data_source_block           PZ26FMI_SQ_S
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/rss-feeds/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 2281 2013-09-26 08:29:07Z andrius 

 Adding full bibliography for 4083030--4083031.cif.
;
_cod_original_cell_volume        4069.9(2)
_cod_database_code               4083030
#BEGIN Tags that were not found in dictionaries:
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.137
_shelx_estimated_absorpt_t_max   0.258
_shelxl_version_number           2012-9
#END Tags that were not found in dictionaries
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-y, x-y, z'
'-x+y, -x, z'
'-x, -y, z+1/2'
'y, -x+y, z+1/2'
'x-y, x, z+1/2'
'-x, -y, -z'
'y, -x+y, -z'
'x-y, x, -z'
'x, y, -z-1/2'
'-y, x-y, -z-1/2'
'-x+y, -x, -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_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
Fe1 Fe 0.6667 0.3333 0.69837(3) 0.0482(2) Uani 1 3 d S T P
Si1 Si 0.51723(5) 0.31110(5) 0.60817(3) 0.03954(18) Uani 1 1 d . . .
Cl1 Cl 0.58846(8) 0.42713(8) 0.7500 0.0517(2) Uani 1 2 d S T P
C1 C 0.6667 0.3333 0.62318(15) 0.0361(8) Uani 1 3 d S T P
C2 C 0.3993(2) 0.2034(2) 0.65054(11) 0.0502(6) Uani 1 1 d . . .
H2A H 0.3990 0.1286 0.6501 0.075 Uiso 1 1 calc R U .
H2B H 0.3224 0.1904 0.6397 0.075 Uiso 1 1 calc R U .
H2C H 0.4150 0.2352 0.6839 0.075 Uiso 1 1 calc R U .
C3 C 0.5090(2) 0.4496(2) 0.61477(10) 0.0460(6) Uani 1 1 d . . .
H3A H 0.5314 0.4801 0.6482 0.069 Uiso 1 1 calc R U .
H3B H 0.4284 0.4322 0.6082 0.069 Uiso 1 1 calc R U .
H3C H 0.5630 0.5086 0.5914 0.069 Uiso 1 1 calc R U .
C4 C 0.4636(2) 0.2566(2) 0.54421(10) 0.0413(5) Uani 1 1 d . . .
C5 C 0.3744(2) 0.1397(2) 0.53445(11) 0.0463(6) Uani 1 1 d . . .
H5 H 0.3398 0.0867 0.5611 0.056 Uiso 1 1 calc R U .
C6 C 0.3360(2) 0.1001(2) 0.48778(11) 0.0514(7) Uani 1 1 d . . .
H6 H 0.2761 0.0208 0.4825 0.062 Uiso 1 1 calc R U .
C7 C 0.3851(3) 0.1763(3) 0.44832(11) 0.0547(7) Uani 1 1 d . . .
H7 H 0.3592 0.1492 0.4160 0.066 Uiso 1 1 calc R U .
C8 C 0.4722(2) 0.2922(2) 0.45642(10) 0.0495(6) Uani 1 1 d . . .
H8 H 0.5059 0.3447 0.4296 0.059 Uiso 1 1 calc R U .
C9 C 0.5095(2) 0.3309(2) 0.50354(10) 0.0447(6) Uani 1 1 d . . .
H9 H 0.5684 0.4108 0.5086 0.054 Uiso 1 1 calc R U .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 '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'
Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.3639 0.7018 '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 Fe1 Cl1 125.782(19) . .
C1 Fe1 Cl1 125.781(19) . 3_665
Cl1 Fe1 Cl1 89.27(3) . 3_665
C1 Fe1 Cl1 125.781(19) . 2_655
Cl1 Fe1 Cl1 89.27(3) . 2_655
Cl1 Fe1 Cl1 89.27(3) 3_665 2_655
C1 Fe1 Fe1 180.0 . 10_557
Cl1 Fe1 Fe1 54.217(19) . 10_557
Cl1 Fe1 Fe1 54.219(19) 3_665 10_557
Cl1 Fe1 Fe1 54.219(19) 2_655 10_557
C1 Si1 C3 112.86(9) . .
C1 Si1 C2 112.63(13) . .
C3 Si1 C2 104.08(12) . .
C1 Si1 C4 115.10(14) . .
C3 Si1 C4 105.33(11) . .
C2 Si1 C4 105.91(12) . .
Fe1 Cl1 Fe1 71.56(4) 10_557 .
Si1 C1 Si1 115.36(9) 2_655 3_665
Si1 C1 Si1 115.36(9) 2_655 .
Si1 C1 Si1 115.36(9) 3_665 .
Si1 C1 Fe1 102.63(12) 2_655 .
Si1 C1 Fe1 102.63(12) 3_665 .
Si1 C1 Fe1 102.62(12) . .
Si1 C2 H2A 109.5 . .
Si1 C2 H2B 109.5 . .
H2A C2 H2B 109.5 . .
Si1 C2 H2C 109.5 . .
H2A C2 H2C 109.5 . .
H2B C2 H2C 109.5 . .
Si1 C3 H3A 109.5 . .
Si1 C3 H3B 109.5 . .
H3A C3 H3B 109.5 . .
Si1 C3 H3C 109.5 . .
H3A C3 H3C 109.5 . .
H3B C3 H3C 109.5 . .
C9 C4 C5 116.1(2) . .
C9 C4 Si1 121.44(18) . .
C5 C4 Si1 122.4(2) . .
C6 C5 C4 122.3(3) . .
C6 C5 H5 118.9 . .
C4 C5 H5 118.9 . .
C5 C6 C7 119.8(3) . .
C5 C6 H6 120.1 . .
C7 C6 H6 120.1 . .
C8 C7 C6 119.7(3) . .
C8 C7 H7 120.1 . .
C6 C7 H7 120.1 . .
C9 C8 C7 119.8(3) . .
C9 C8 H8 120.1 . .
C7 C8 H8 120.1 . .
C8 C9 C4 122.2(2) . .
C8 C9 H9 118.9 . .
C4 C9 H9 118.9 . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C1 2.054(4) .
Fe1 Cl1 2.4119(8) .
Fe1 Cl1 2.4119(8) 3_665
Fe1 Cl1 2.4119(8) 2_655
Fe1 Fe1 2.8204(15) 10_557
Si1 C1 1.8772(11) .
Si1 C3 1.881(2) .
Si1 C2 1.882(3) .
Si1 C4 1.886(3) .
Cl1 Fe1 2.4118(8) 10_557
C1 Si1 1.8772(11) 2_655
C1 Si1 1.8772(11) 3_665
C2 H2A 0.9800 .
C2 H2B 0.9800 .
C2 H2C 0.9800 .
C3 H3A 0.9800 .
C3 H3B 0.9800 .
C3 H3C 0.9800 .
C4 C9 1.400(4) .
C4 C5 1.413(3) .
C5 C6 1.374(4) .
C5 H5 0.9500 .
C6 C7 1.390(4) .
C6 H6 0.9500 .
C7 C8 1.389(4) .
C7 H7 0.9500 .
C8 C9 1.381(4) .
C8 H8 0.9500 .
C9 H9 0.9500 .
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_4
C3 Si1 C1 Si1 -170.86(16) 2_655
C2 Si1 C1 Si1 71.6(2) 2_655
C4 Si1 C1 Si1 -49.9(2) 2_655
C3 Si1 C1 Si1 -32.3(3) 3_665
C2 Si1 C1 Si1 -149.83(18) 3_665
C4 Si1 C1 Si1 88.62(18) 3_665
C3 Si1 C1 Fe1 78.40(11) .
C2 Si1 C1 Fe1 -39.10(10) .
C4 Si1 C1 Fe1 -160.65(9) .
C1 Si1 C4 C9 -74.4(2) .
C3 Si1 C4 C9 50.6(2) .
C2 Si1 C4 C9 160.52(19) .
C1 Si1 C4 C5 106.42(19) .
C3 Si1 C4 C5 -128.6(2) .
C2 Si1 C4 C5 -18.7(2) .
C9 C4 C5 C6 1.2(3) .
Si1 C4 C5 C6 -179.6(2) .
C4 C5 C6 C7 -0.3(4) .
C5 C6 C7 C8 -0.4(4) .
C6 C7 C8 C9 0.1(4) .
C7 C8 C9 C4 0.8(4) .
C5 C4 C9 C8 -1.4(3) .
Si1 C4 C9 C8 179.30(19) .
