#------------------------------------------------------------------------------
#$Date: 2020-08-07 04:15:51 +0300 (Fri, 07 Aug 2020) $
#$Revision: 255148 $
#$URL: file:///home/coder/svn-repositories/cod/cif/1/55/88/1558803.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_1558803
loop_
_publ_author_name
'Nagelski, Alexandra L.'
'Fataftah, Majed S.'
'Bollmeyer, Melissa M.'
'McWilliams, Sean F.'
'MacMillan, Samantha N.'
'Mercado, Brandon Q.'
'Lancaster, Kyle M.'
'Holland, Patrick L.'
_publ_section_title
;
 The influences of carbon donor ligands on biomimetic multi-iron complexes
 for N2 reduction
;
_journal_name_full               'Chemical Science'
_journal_paper_doi               10.1039/D0SC03447A
_journal_year                    2020
_chemical_formula_moiety         'C26 H38 Fe N2 Si'
_chemical_formula_sum            'C26 H38 Fe N2 Si'
_chemical_formula_weight         462.52
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     SHELXT
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2020-06-15 deposited with the CCDC.	2020-07-28 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 99.0427(14)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.46458(13)
_cell_length_b                   17.4351(3)
_cell_length_c                   10.11223(13)
_cell_measurement_reflns_used    26188
_cell_measurement_temperature    93(2)
_cell_measurement_theta_max      66.6370
_cell_measurement_theta_min      4.3860
_cell_volume                     1299.71(4)
_computing_cell_refinement       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.67a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'CIFTAB-2014/2 (Sheldrick, 2014)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXT-2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      93(2)
_diffrn_detector_area_resol_mean 22.2
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku Saturn 944+ CCD'
_diffrn_measurement_method       ω
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0463
_diffrn_reflns_av_unetI/netI     0.0144
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       8
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            43855
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        66.741
_diffrn_reflns_theta_max         66.741
_diffrn_reflns_theta_min         4.427
_diffrn_source                   'microfocus rotating anode'
_exptl_absorpt_coefficient_mu    5.182
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.69337
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.40.67a (Rigaku Oxford Diffraction, 2019) 
Empirical absorption correction using spherical harmonics, 
 implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    1.182
_exptl_crystal_description       Plate
_exptl_crystal_F_000             496
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.020
_refine_diff_density_max         0.240
_refine_diff_density_min         -0.278
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     183
_refine_ls_number_reflns         2375
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.063
_refine_ls_R_factor_all          0.0320
_refine_ls_R_factor_gt           0.0303
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0546P)²+0.3268P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0850
_refine_ls_wR_factor_ref         0.0864
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2270
_reflns_number_total             2375
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d0sc03447a2.cif
_cod_data_source_block           007b-17080
_cod_original_cell_volume        1299.70(3)
_cod_original_sg_symbol_H-M      'P 21/m'
_cod_database_code               1558803
_shelx_shelxl_version_number     2014/7
_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   0.424
_shelx_estimated_absorpt_t_max   0.903
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z'
'-x, -y, -z'
'x, -y-1/2, z'
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.39755(5) 0.74008(14) 0.29865(4) 0.0188(4) Uani 0.5 1 d . . P A -1
N11 N 0.40802(17) 0.66910(8) 0.16291(12) 0.0286(3) Uani 1 1 d . . . . .
C11 C 0.4802(2) 0.60822(10) -0.04083(16) 0.0343(4) Uani 1 1 d . . . . .
H11A H 0.6053 0.5892 -0.0284 0.051 Uiso 1 1 calc R U . . .
H11B H 0.4419 0.6219 -0.1350 0.051 Uiso 1 1 calc R U . . .
H11C H 0.4002 0.5682 -0.0152 0.051 Uiso 1 1 calc R U . . .
C21 C 0.4699(2) 0.67834(10) 0.04606(14) 0.0289(4) Uani 1 1 d . . . . .
C31 C 0.5203(3) 0.7500 -0.0020(2) 0.0289(5) Uani 1 2 d S T P . .
C41 C 0.6204(4) 0.7577(15) -0.1226(3) 0.029(3) Uani 0.5 1 d . . P B -1
H41A H 0.7055 0.7149 -0.1230 0.044 Uiso 0.5 1 calc R U P B -1
H41B H 0.6874 0.8063 -0.1165 0.044 Uiso 0.5 1 calc R U P B -1
H41C H 0.5324 0.7569 -0.2054 0.044 Uiso 0.5 1 calc R U P B -1
C12 C 0.3421(2) 0.59590(10) 0.19911(14) 0.0293(4) Uani 1 1 d . . . . .
C22 C 0.1597(2) 0.57649(10) 0.15769(16) 0.0313(4) Uani 1 1 d . . . . .
C32 C 0.0967(2) 0.50692(11) 0.19986(17) 0.0384(4) Uani 1 1 d . . . . .
H32 H -0.0260 0.4925 0.1714 0.046 Uiso 1 1 calc R U . . .
C42 C 0.2111(3) 0.45846(11) 0.28295(19) 0.0442(5) Uani 1 1 d . . . . .
H42 H 0.1665 0.4111 0.3110 0.053 Uiso 1 1 calc R U . . .
C52 C 0.3898(3) 0.47897(12) 0.32496(18) 0.0421(5) Uani 1 1 d . . . . .
H52 H 0.4668 0.4457 0.3827 0.051 Uiso 1 1 calc R U . . .
C62 C 0.4588(2) 0.54761(11) 0.28400(16) 0.0359(4) Uani 1 1 d . . . . .
C72 C 0.0346(2) 0.63031(11) 0.06913(18) 0.0375(4) Uani 1 1 d . . . . .
H72A H 0.0183 0.6775 0.1185 0.056 Uiso 1 1 calc R U . . .
H72B H -0.0833 0.6055 0.0424 0.056 Uiso 1 1 calc R U . . .
H72C H 0.0879 0.6428 -0.0108 0.056 Uiso 1 1 calc R U . . .
C82 C 0.6539(2) 0.57014(14) 0.32937(19) 0.0486(5) Uani 1 1 d . . . . .
H82A H 0.7117 0.5815 0.2510 0.073 Uiso 1 1 calc R U . . .
H82B H 0.7183 0.5278 0.3801 0.073 Uiso 1 1 calc R U . . .
H82C H 0.6585 0.6157 0.3865 0.073 Uiso 1 1 calc R U . . .
C14 C 0.3745(5) 0.7344(3) 0.4947(3) 0.0353(16) Uani 0.5 1 d . . P A -1
H14A H 0.4350 0.6867 0.5315 0.042 Uiso 0.5 1 calc R U P A -1
H14B H 0.4431 0.7779 0.5407 0.042 Uiso 0.5 1 calc R U P A -1
C24 C 0.1389(5) 0.6280(2) 0.5332(3) 0.0366(8) Uani 0.5 1 d . . P A -1
H24A H 0.1743 0.6090 0.4498 0.055 Uiso 0.5 1 calc R U P A -1
H24B H 0.0141 0.6122 0.5378 0.055 Uiso 0.5 1 calc R U P A -1
H24C H 0.2205 0.6066 0.6097 0.055 Uiso 0.5 1 calc R U P A -1
C34 C -0.0354(6) 0.7767(3) 0.4157(4) 0.0421(9) Uani 0.5 1 d . . P A -1
H34A H -0.014(7) 0.834(3) 0.409(5) 0.063 Uiso 0.5 1 d . U P C -1
H34B H -0.151(6) 0.769(3) 0.443(4) 0.063 Uiso 0.5 1 d . U P D -1
H34 H -0.049(5) 0.7500 0.335(4) 0.063 Uiso 1 2 d S U P . .
C44 C 0.1157(5) 0.7673(2) 0.7088(3) 0.0375(15) Uani 0.5 1 d . . P A -1
H44A H 0.2022 0.7412 0.7771 0.056 Uiso 0.5 1 calc R U P A -1
H44B H -0.0083 0.7543 0.7211 0.056 Uiso 0.5 1 calc R U P A -1
H44C H 0.1332 0.8229 0.7173 0.056 Uiso 0.5 1 calc R U P A -1
Si14 Si 0.15424(11) 0.73578(9) 0.53769(7) 0.0291(5) Uani 0.5 1 d . . P A -1
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 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'
Fe Fe -1.1336 3.1974 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 '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'
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
_geom_angle_publ_flag
N11 Fe1 C14 135.40(18) . . ?
C21 N11 C12 120.64(14) . . ?
C21 N11 Fe1 129.00(14) . . ?
C12 N11 Fe1 110.34(11) . . ?
C21 C11 H11A 109.5 . . ?
C21 C11 H11B 109.5 . . ?
H11A C11 H11B 109.5 . . ?
C21 C11 H11C 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
N11 C21 C31 123.75(16) . . ?
N11 C21 C11 117.96(15) . . ?
C31 C21 C11 118.26(14) . . ?
C21 C31 C21 124.29(19) . 4_575 ?
C21 C31 C41 122.8(10) . . ?
C21 C31 C41 112.7(10) 4_575 . ?
C31 C41 H41A 109.5 . . ?
C31 C41 H41B 109.5 . . ?
H41A C41 H41B 109.5 . . ?
C31 C41 H41C 109.5 . . ?
H41A C41 H41C 109.5 . . ?
H41B C41 H41C 109.5 . . ?
C22 C12 C62 121.23(16) . . ?
C22 C12 N11 119.63(14) . . ?
C62 C12 N11 118.97(15) . . ?
C32 C22 C12 118.55(16) . . ?
C32 C22 C72 121.00(16) . . ?
C12 C22 C72 120.45(16) . . ?
C42 C32 C22 120.76(17) . . ?
C42 C32 H32 119.6 . . ?
C22 C32 H32 119.6 . . ?
C52 C42 C32 120.07(18) . . ?
C52 C42 H42 120.0 . . ?
C32 C42 H42 120.0 . . ?
C42 C52 C62 121.04(17) . . ?
C42 C52 H52 119.5 . . ?
C62 C52 H52 119.5 . . ?
C52 C62 C12 118.34(17) . . ?
C52 C62 C82 121.22(16) . . ?
C12 C62 C82 120.45(17) . . ?
C22 C72 H72A 109.5 . . ?
C22 C72 H72B 109.5 . . ?
H72A C72 H72B 109.5 . . ?
C22 C72 H72C 109.5 . . ?
H72A C72 H72C 109.5 . . ?
H72B C72 H72C 109.5 . . ?
C62 C82 H82A 109.5 . . ?
C62 C82 H82B 109.5 . . ?
H82A C82 H82B 109.5 . . ?
C62 C82 H82C 109.5 . . ?
H82A C82 H82C 109.5 . . ?
H82B C82 H82C 109.5 . . ?
Si14 C14 Fe1 117.88(17) . . ?
Si14 C14 H14A 107.8 . . ?
Fe1 C14 H14A 107.8 . . ?
Si14 C14 H14B 107.8 . . ?
Fe1 C14 H14B 107.8 . . ?
H14A C14 H14B 107.2 . . ?
Si14 C24 H24A 109.5 . . ?
Si14 C24 H24B 109.5 . . ?
H24A C24 H24B 109.5 . . ?
Si14 C24 H24C 109.5 . . ?
H24A C24 H24C 109.5 . . ?
H24B C24 H24C 109.5 . . ?
Si14 C34 H34A 108(3) . . ?
Si14 C34 H34B 112(3) . . ?
H34A C34 H34B 109(4) . . ?
Si14 C34 H34 111(2) . . ?
H34A C34 H34 115(3) . . ?
H34B C34 H34 102(3) . . ?
Si14 C44 H44A 109.5 . . ?
Si14 C44 H44B 109.5 . . ?
H44A C44 H44B 109.5 . . ?
Si14 C44 H44C 109.5 . . ?
H44A C44 H44C 109.5 . . ?
H44B C44 H44C 109.5 . . ?
C14 Si14 C34 118.76(18) . . ?
C14 Si14 C44 120.92(16) . . ?
C34 Si14 C44 106.66(18) . . ?
C14 Si14 C24 92.03(19) . . ?
C34 Si14 C24 109.17(19) . . ?
C44 Si14 C24 107.27(17) . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 N11 1.859(2) . ?
Fe1 C14 2.019(3) . ?
N11 C21 1.344(2) . ?
N11 C12 1.436(2) . ?
C11 C21 1.515(2) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C21 C31 1.413(2) . ?
C31 C21 1.413(2) 4_575 ?
C31 C41 1.533(4) . ?
C41 H41A 0.9800 . ?
C41 H41B 0.9800 . ?
C41 H41C 0.9800 . ?
C12 C22 1.402(2) . ?
C12 C62 1.404(2) . ?
C22 C32 1.392(3) . ?
C22 C72 1.514(2) . ?
C32 C42 1.387(3) . ?
C32 H32 0.9500 . ?
C42 C52 1.382(3) . ?
C42 H42 0.9500 . ?
C52 C62 1.391(3) . ?
C52 H52 0.9500 . ?
C62 C82 1.508(3) . ?
C72 H72A 0.9800 . ?
C72 H72B 0.9800 . ?
C72 H72C 0.9800 . ?
C82 H82A 0.9800 . ?
C82 H82B 0.9800 . ?
C82 H82C 0.9800 . ?
C14 Si14 1.766(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C24 Si14 1.883(4) . ?
C24 H24A 0.9800 . ?
C24 H24B 0.9800 . ?
C24 H24C 0.9800 . ?
C34 Si14 1.867(4) . ?
C34 H34A 1.02(5) . ?
C34 H34B 0.96(5) . ?
C34 H34 0.93(4) . ?
C44 Si14 1.880(3) . ?
C44 H44A 0.9800 . ?
C44 H44B 0.9800 . ?
C44 H44C 0.9800 . ?
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_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
C14 Fe1 N11 C21 -160.68(17) . . . . ?
C14 Fe1 N11 C12 17.67(19) . . . . ?
C12 N11 C21 C31 173.67(15) . . . . ?
Fe1 N11 C21 C31 -8.1(2) . . . . ?
C12 N11 C21 C11 -4.3(2) . . . . ?
Fe1 N11 C21 C11 173.92(11) . . . . ?
N11 C21 C31 C21 -17.1(3) . . . 4_575 ?
C11 C21 C31 C21 160.80(15) . . . 4_575 ?
N11 C21 C31 C41 169.2(2) . . . . ?
C11 C21 C31 C41 -12.8(3) . . . . ?
C21 N11 C12 C22 -87.41(18) . . . . ?
Fe1 N11 C12 C22 94.08(14) . . . . ?
C21 N11 C12 C62 97.37(17) . . . . ?
Fe1 N11 C12 C62 -81.14(15) . . . . ?
C62 C12 C22 C32 -1.6(2) . . . . ?
N11 C12 C22 C32 -176.70(13) . . . . ?
C62 C12 C22 C72 178.35(15) . . . . ?
N11 C12 C22 C72 3.2(2) . . . . ?
C12 C22 C32 C42 1.1(2) . . . . ?
C72 C22 C32 C42 -178.83(15) . . . . ?
C22 C32 C42 C52 0.0(3) . . . . ?
C32 C42 C52 C62 -0.7(3) . . . . ?
C42 C52 C62 C12 0.3(3) . . . . ?
C42 C52 C62 C82 -179.88(17) . . . . ?
C22 C12 C62 C52 0.9(2) . . . . ?
N11 C12 C62 C52 176.06(14) . . . . ?
C22 C12 C62 C82 -178.95(15) . . . . ?
N11 C12 C62 C82 -3.8(2) . . . . ?
Fe1 C14 Si14 C34 -21.7(4) . . . . ?
Fe1 C14 Si14 C44 -156.9(2) . . . . ?
Fe1 C14 Si14 C24 91.5(3) . . . . ?
