#------------------------------------------------------------------------------
#$Date: 2016-03-23 21:18:00 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179446 $
#$URL: svn://www.crystallography.net/cod/cif/4/33/43/4334324.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_4334324
loop_
_publ_author_name
'Jamie Hicks'
'Cameron Jones'
_publ_section_title
;
 Extremely Bulky Amido First Row Transition Metal(II) Halide Complexes:
 Potential Precursors to Low Coordinate Metal-Metal Bonded Systems
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3900
_journal_page_last               3907
_journal_paper_doi               10.1021/ic302672a
_journal_volume                  52
_journal_year                    2013
_chemical_formula_sum            'C80 H88 Br2 Fe2 N2 O2 Si2'
_chemical_formula_weight         1437.22
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 114.497(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   16.4622(14)
_cell_length_b                   12.6193(7)
_cell_length_c                   18.6176(14)
_cell_measurement_temperature    123(2)
_cell_volume                     3519.5(5)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'Oxford Gemini Ultra'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            13984
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.96
_exptl_absorpt_coefficient_mu    1.630
_exptl_absorpt_correction_T_max  0.841
_exptl_absorpt_correction_T_min  0.750
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SCALE3 ABSPACK'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       block
_exptl_crystal_F_000             1496
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.710
_refine_diff_density_min         -0.431
_refine_diff_density_rms         0.102
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.057
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     429
_refine_ls_number_reflns         6877
_refine_ls_number_restraints     3
_refine_ls_restrained_S_all      1.056
_refine_ls_R_factor_all          0.0592
_refine_ls_R_factor_gt           0.0451
_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)+(0.0486P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1073
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                5545
_reflns_number_total             6877
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic302672a_si_002_05.cif
_cod_data_source_block           compound5
_cod_original_cell_volume        3519.5(4)
_cod_database_code               4334324
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -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
Br1 Br 0.60521(2) 0.06267(2) 0.560320(17) 0.02043(11) Uani 1 1 d . . .
Fe1 Fe 0.52843(3) 0.00604(3) 0.41602(2) 0.01694(13) Uani 1 1 d . . .
Si1 Si 0.61563(5) -0.21074(6) 0.39629(4) 0.01427(19) Uani 1 1 d . . .
O1 O 0.47458(14) 0.14742(16) 0.36530(12) 0.0229(5) Uani 1 1 d . B .
N1 N 0.57443(15) -0.08656(18) 0.35960(13) 0.0127(5) Uani 1 1 d . . .
C1 C 0.57725(19) -0.0421(2) 0.28983(16) 0.0110(6) Uani 1 1 d . . .
C2 C 0.65673(19) 0.0035(2) 0.29117(16) 0.0134(6) Uani 1 1 d . . .
C3 C 0.6557(2) 0.0509(2) 0.22315(17) 0.0160(6) Uani 1 1 d . . .
H3 H 0.7087 0.0834 0.2254 0.019 Uiso 1 1 calc R . .
C4 C 0.5804(2) 0.0524(2) 0.15232(17) 0.0141(6) Uani 1 1 d . . .
C5 C 0.5031(2) 0.0070(2) 0.15185(16) 0.0150(6) Uani 1 1 d . . .
H5 H 0.4504 0.0081 0.1042 0.018 Uiso 1 1 calc R . .
C6 C 0.50001(19) -0.0398(2) 0.21837(16) 0.0137(6) Uani 1 1 d . . .
C7 C 0.5841(2) 0.0975(2) 0.07875(16) 0.0204(7) Uani 1 1 d . . .
H7A H 0.6228 0.1601 0.0925 0.031 Uiso 1 1 calc R . .
H7B H 0.5238 0.1178 0.0414 0.031 Uiso 1 1 calc R . .
H7C H 0.6079 0.0441 0.0545 0.031 Uiso 1 1 calc R . .
C8 C 0.74303(19) 0.0009(2) 0.36587(16) 0.0141(6) Uani 1 1 d . . .
H8 H 0.7290 -0.0399 0.4054 0.017 Uiso 1 1 calc R . .
C9 C 0.77247(18) 0.1103(2) 0.40196(16) 0.0150(6) Uani 1 1 d . . .
C10 C 0.7617(2) 0.1377(3) 0.46956(18) 0.0269(8) Uani 1 1 d . . .
H10 H 0.7366 0.0877 0.4928 0.032 Uiso 1 1 calc R . .
C11 C 0.7868(2) 0.2365(3) 0.5037(2) 0.0367(9) Uani 1 1 d . . .
H11 H 0.7779 0.2543 0.5496 0.044 Uiso 1 1 calc R . .
C12 C 0.8247(2) 0.3095(3) 0.4714(2) 0.0327(8) Uani 1 1 d . . .
H12 H 0.8419 0.3774 0.4949 0.039 Uiso 1 1 calc R . .
C13 C 0.8373(2) 0.2830(2) 0.40469(19) 0.0252(7) Uani 1 1 d . . .
H13 H 0.8635 0.3328 0.3822 0.030 Uiso 1 1 calc R . .
C14 C 0.8120(2) 0.1840(2) 0.37057(17) 0.0192(6) Uani 1 1 d . . .
H14 H 0.8216 0.1660 0.3252 0.023 Uiso 1 1 calc R . .
C15 C 0.8200(2) -0.0588(2) 0.35783(17) 0.0158(6) Uani 1 1 d . . .
C16 C 0.8998(2) -0.0706(2) 0.42553(18) 0.0196(7) Uani 1 1 d . . .
H16 H 0.9051 -0.0395 0.4737 0.023 Uiso 1 1 calc R . .
C17 C 0.9710(2) -0.1267(2) 0.42365(18) 0.0228(7) Uani 1 1 d . . .
H17 H 1.0243 -0.1339 0.4704 0.027 Uiso 1 1 calc R . .
C18 C 0.9651(2) -0.1723(2) 0.35416(18) 0.0243(7) Uani 1 1 d . . .
H18 H 1.0143 -0.2100 0.3527 0.029 Uiso 1 1 calc R . .
C19 C 0.8870(2) -0.1625(3) 0.28718(19) 0.0272(8) Uani 1 1 d . . .
H19 H 0.8819 -0.1944 0.2393 0.033 Uiso 1 1 calc R . .
C20 C 0.8152(2) -0.1059(3) 0.28939(18) 0.0220(7) Uani 1 1 d . . .
H20 H 0.7618 -0.0996 0.2426 0.026 Uiso 1 1 calc R . .
C21 C 0.41455(19) -0.0946(2) 0.21196(16) 0.0143(6) Uani 1 1 d . . .
H21 H 0.4157 -0.0928 0.2661 0.017 Uiso 1 1 calc R . .
C22 C 0.32976(19) -0.0378(2) 0.15836(17) 0.0147(6) Uani 1 1 d . . .
C23 C 0.2890(2) 0.0339(3) 0.19036(19) 0.0247(7) Uani 1 1 d . . .
H23 H 0.3154 0.0473 0.2455 0.030 Uiso 1 1 calc R . .
C24 C 0.2112(2) 0.0856(3) 0.1431(2) 0.0298(8) Uani 1 1 d . . .
H24 H 0.1846 0.1342 0.1659 0.036 Uiso 1 1 calc R . .
C25 C 0.1719(2) 0.0669(3) 0.0628(2) 0.0289(8) Uani 1 1 d . . .
H25 H 0.1181 0.1021 0.0304 0.035 Uiso 1 1 calc R . .
C26 C 0.2110(2) -0.0029(2) 0.03017(18) 0.0225(7) Uani 1 1 d . . .
H26 H 0.1844 -0.0155 -0.0251 0.027 Uiso 1 1 calc R . .
C27 C 0.2893(2) -0.0554(2) 0.07755(17) 0.0181(6) Uani 1 1 d . . .
H27 H 0.3155 -0.1038 0.0543 0.022 Uiso 1 1 calc R . .
C28 C 0.41167(19) -0.2124(2) 0.18961(16) 0.0153(6) Uani 1 1 d . . .
C29 C 0.3538(2) -0.2797(2) 0.20502(17) 0.0195(7) Uani 1 1 d . . .
H29 H 0.3167 -0.2518 0.2282 0.023 Uiso 1 1 calc R . .
C30 C 0.3494(2) -0.3862(3) 0.18714(18) 0.0244(7) Uani 1 1 d . . .
H30 H 0.3095 -0.4308 0.1982 0.029 Uiso 1 1 calc R . .
C31 C 0.4026(2) -0.4284(2) 0.15336(19) 0.0258(8) Uani 1 1 d . . .
H31 H 0.4003 -0.5020 0.1420 0.031 Uiso 1 1 calc R . .
C32 C 0.4594(2) -0.3625(3) 0.13618(19) 0.0270(7) Uani 1 1 d . . .
H32 H 0.4956 -0.3906 0.1122 0.032 Uiso 1 1 calc R . .
C33 C 0.4634(2) -0.2552(2) 0.15405(18) 0.0226(7) Uani 1 1 d . . .
H33 H 0.5023 -0.2104 0.1417 0.027 Uiso 1 1 calc R . .
C34 C 0.7063(2) -0.1943(2) 0.49752(17) 0.0214(7) Uani 1 1 d . . .
H34A H 0.7637 -0.1860 0.4940 0.032 Uiso 1 1 calc R . .
H34B H 0.7083 -0.2569 0.5294 0.032 Uiso 1 1 calc R . .
H34C H 0.6943 -0.1312 0.5223 0.032 Uiso 1 1 calc R . .
C35 C 0.5263(2) -0.2968(2) 0.40293(18) 0.0219(7) Uani 1 1 d . . .
H35A H 0.4884 -0.2543 0.4208 0.033 Uiso 1 1 calc R . .
H35B H 0.5538 -0.3543 0.4406 0.033 Uiso 1 1 calc R . .
H35C H 0.4899 -0.3268 0.3509 0.033 Uiso 1 1 calc R . .
C36 C 0.6625(2) -0.2821(2) 0.33426(18) 0.0232(7) Uani 1 1 d . . .
H36A H 0.6153 -0.2930 0.2812 0.035 Uiso 1 1 calc R . .
H36B H 0.6861 -0.3509 0.3582 0.035 Uiso 1 1 calc R . .
H36C H 0.7106 -0.2399 0.3307 0.035 Uiso 1 1 calc R . .
C37 C 0.5150(3) 0.2154(3) 0.3252(2) 0.0350(9) Uani 1 1 d D . .
H37A H 0.4949 0.1942 0.2693 0.042 Uiso 1 1 calc R A 1
H37B H 0.5809 0.2109 0.3514 0.042 Uiso 1 1 calc R A 1
C38 C 0.4841(7) 0.3259(7) 0.3312(8) 0.041(3) Uani 0.585(18) 1 d P B 1
H38A H 0.4825 0.3713 0.2872 0.049 Uiso 0.585(18) 1 calc PR B 1
H38B H 0.5222 0.3596 0.3821 0.049 Uiso 0.585(18) 1 calc PR B 1
C38A C 0.4460(13) 0.3040(12) 0.2936(8) 0.048(5) Uani 0.415(18) 1 d PD B 2
H38C H 0.4729 0.3687 0.2826 0.057 Uiso 0.415(18) 1 calc PR B 2
H38D H 0.3950 0.2816 0.2448 0.057 Uiso 0.415(18) 1 calc PR B 2
C39 C 0.3910(7) 0.3032(8) 0.3253(7) 0.038(3) Uani 0.585(18) 1 d P B 1
H39A H 0.3496 0.2843 0.2707 0.045 Uiso 0.585(18) 1 calc PR B 1
H39B H 0.3667 0.3645 0.3432 0.045 Uiso 0.585(18) 1 calc PR B 1
C39A C 0.4168(12) 0.3231(6) 0.3600(8) 0.030(3) Uani 0.415(18) 1 d PD B 2
H39C H 0.4625 0.3621 0.4046 0.036 Uiso 0.415(18) 1 calc PR B 2
H39D H 0.3591 0.3612 0.3414 0.036 Uiso 0.415(18) 1 calc PR B 2
C40 C 0.4084(2) 0.2090(3) 0.3812(2) 0.0288(8) Uani 1 1 d D . .
H40A H 0.4324 0.2325 0.4369 0.035 Uiso 1 1 calc R B 1
H40B H 0.3532 0.1675 0.3690 0.035 Uiso 1 1 calc R B 1
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'
Si Si 0.0817 0.0704 '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_3
Fe1 Br1 Fe1 90.024(18) 3_656
N1 Fe1 O1 118.17(9) .
N1 Fe1 Br1 127.57(7) .
O1 Fe1 Br1 99.95(6) .
N1 Fe1 Br1 116.60(7) 3_656
O1 Fe1 Br1 97.81(6) 3_656
Br1 Fe1 Br1 89.976(18) 3_656
N1 Si1 C36 112.80(13) .
N1 Si1 C34 108.40(13) .
C36 Si1 C34 108.43(14) .
N1 Si1 C35 111.14(13) .
C36 Si1 C35 107.39(15) .
C34 Si1 C35 108.57(14) .
C40 O1 C37 109.0(2) .
C40 O1 Fe1 125.95(17) .
C37 O1 Fe1 123.06(18) .
C1 N1 Si1 123.86(18) .
C1 N1 Fe1 115.16(17) .
Si1 N1 Fe1 120.84(12) .
C6 C1 C2 118.2(2) .
C6 C1 N1 120.5(2) .
C2 C1 N1 121.2(2) .
C3 C2 C1 119.6(3) .
C3 C2 C8 119.7(3) .
C1 C2 C8 120.8(2) .
C4 C3 C2 122.7(3) .
C3 C4 C5 117.1(3) .
C3 C4 C7 120.9(3) .
C5 C4 C7 122.0(3) .
C4 C5 C6 122.7(3) .
C5 C6 C1 119.8(3) .
C5 C6 C21 119.7(3) .
C1 C6 C21 120.4(2) .
C2 C8 C9 112.9(2) .
C2 C8 C15 114.7(2) .
C9 C8 C15 111.3(2) .
C10 C9 C14 118.2(3) .
C10 C9 C8 119.3(3) .
C14 C9 C8 122.5(2) .
C11 C10 C9 121.1(3) .
C10 C11 C12 120.2(3) .
C13 C12 C11 119.5(3) .
C12 C13 C14 120.0(3) .
C13 C14 C9 120.9(3) .
C20 C15 C16 117.3(3) .
C20 C15 C8 124.7(3) .
C16 C15 C8 118.0(3) .
C17 C16 C15 121.4(3) .
C16 C17 C18 120.4(3) .
C19 C18 C17 119.2(3) .
C18 C19 C20 120.2(3) .
C15 C20 C19 121.6(3) .
C22 C21 C6 113.9(2) .
C22 C21 C28 111.2(2) .
C6 C21 C28 112.5(2) .
C27 C22 C23 117.8(3) .
C27 C22 C21 122.3(3) .
C23 C22 C21 119.9(3) .
C24 C23 C22 121.1(3) .
C23 C24 C25 120.2(3) .
C26 C25 C24 119.6(3) .
C25 C26 C27 120.4(3) .
C22 C27 C26 120.9(3) .
C33 C28 C29 118.0(3) .
C33 C28 C21 123.3(3) .
C29 C28 C21 118.7(2) .
C30 C29 C28 121.1(3) .
C29 C30 C31 120.5(3) .
C30 C31 C32 119.4(3) .
C31 C32 C33 120.0(3) .
C28 C33 C32 121.0(3) .
O1 C37 C38 105.5(5) .
O1 C37 C38A 101.7(7) .
C38 C37 C38A 29.5(6) .
C37 C38 C39 100.5(7) .
C39A C38A C37 103.8(9) .
C38 C39 C40 101.5(8) .
C40 C39A C38A 98.9(9) .
O1 C40 C39A 107.2(6) .
O1 C40 C39 102.7(5) .
C39A C40 C39 25.0(4) .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Br1 Fe1 2.5514(6) .
Br1 Fe1 2.5671(5) 3_656
Fe1 N1 1.924(2) .
Fe1 O1 2.041(2) .
Fe1 Br1 2.5671(5) 3_656
Si1 N1 1.732(2) .
Si1 C36 1.865(3) .
Si1 C34 1.868(3) .
Si1 C35 1.873(3) .
O1 C40 1.465(4) .
O1 C37 1.465(4) .
N1 C1 1.433(3) .
C1 C6 1.409(4) .
C1 C2 1.420(4) .
C2 C3 1.394(4) .
C2 C8 1.522(4) .
C3 C4 1.385(4) .
C4 C5 1.392(4) .
C4 C7 1.508(4) .
C5 C6 1.392(4) .
C6 C21 1.527(4) .
C8 C9 1.524(4) .
C8 C15 1.534(4) .
C9 C10 1.386(4) .
C9 C14 1.394(4) .
C10 C11 1.383(5) .
C11 C12 1.383(5) .
C12 C13 1.383(5) .
C13 C14 1.386(4) .
C15 C20 1.378(4) .
C15 C16 1.401(4) .
C16 C17 1.381(4) .
C17 C18 1.382(4) .
C18 C19 1.376(4) .
C19 C20 1.396(4) .
C21 C22 1.517(4) .
C21 C28 1.540(4) .
C22 C27 1.388(4) .
C22 C23 1.398(4) .
C23 C24 1.381(5) .
C24 C25 1.381(5) .
C25 C26 1.372(5) .
C26 C27 1.392(4) .
C28 C33 1.387(4) .
C28 C29 1.392(4) .
C29 C30 1.379(4) .
C30 C31 1.380(5) .
C31 C32 1.384(5) .
C32 C33 1.389(4) .
C37 C38 1.504(9) .
C37 C38A 1.527(7) .
C38 C39 1.517(12) .
C38A C39A 1.520(8) .
C39 C40 1.527(9) .
C39A C40 1.514(7) .
