#------------------------------------------------------------------------------
#$Date: 2019-11-24 05:03:49 +0200 (Sun, 24 Nov 2019) $
#$Revision: 236789 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/08/74/4087417.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_4087417
loop_
_publ_author_name
'Ito, Jun-ichi'
'Hosokawa, Satomi'
'Khalid, Hairuzana Binti'
'Nishiyama, Hisao'
_publ_section_title
;
 Preparation, Characterization, and Catalytic Reactions of NCN Pincer Iron
 Complexes Containing Stannyl, Silyl, Methyl, and Phenyl Ligands
;
_journal_issue                   7
_journal_name_full               Organometallics
_journal_page_first              1377
_journal_paper_doi               10.1021/acs.organomet.5b00082
_journal_volume                  34
_journal_year                    2015
_chemical_formula_sum            'C21 H28 Fe N2 O4 Si'
_chemical_formula_weight         456.39
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/m 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                 96.899(7)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.427(3)
_cell_length_b                   12.448(5)
_cell_length_c                   10.577(4)
_cell_measurement_reflns_used    4617
_cell_measurement_temperature    123(2)
_cell_measurement_theta_max      28.25
_cell_measurement_theta_min      2.43
_cell_volume                     1101.5(7)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      123(2)
_diffrn_detector_area_resol_mean 8.366
_diffrn_measured_fraction_theta_full 0.992
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_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  0.0260
_diffrn_reflns_av_sigmaI/netI    0.0286
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            8047
_diffrn_reflns_theta_full        28.31
_diffrn_reflns_theta_max         28.31
_diffrn_reflns_theta_min         1.94
_exptl_absorpt_coefficient_mu    0.768
_exptl_absorpt_correction_T_max  0.9272
_exptl_absorpt_correction_T_min  0.8024
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.376
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.584
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.065
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     149
_refine_ls_number_reflns         2837
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.065
_refine_ls_R_factor_all          0.0346
_refine_ls_R_factor_gt           0.0314
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0469P)²+0.3909P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0821
_refine_ls_wR_factor_ref         0.0843
_reflns_number_gt                2610
_reflns_number_total             2837
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om5b00082_si_002.cif
_cod_data_source_block           5a
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_absorpt_correction_type' value 'Empirical' was
changed to 'empirical' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

data item '_symmetry_cell_setting' value 'Monoclinic' was changed to
'monoclinic' in accordance with the
/home/saulius/struct/COD-crude-data/automatic-downloads/DataCite-retrospective/ACS/depositions/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 last updated on
2011-04-26.

Automatic conversion script
Id: cif_fix_values 6909 2019-04-08 15:41:33Z antanas 
;
_cod_original_cell_volume        1101.6(7)
_cod_original_sg_symbol_H-M      P2(1)/m
_cod_database_code               4087417
loop_
_symmetry_equiv_pos_as_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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
Fe1 Fe 0.15788(3) 0.2500 0.23833(2) 0.01395(9) Uani 1 2 d S
N1 N 0.18036(14) 0.09165(9) 0.20675(11) 0.0177(2) Uani 1 1 d .
O1 O 0.25305(14) -0.03805(8) 0.07523(11) 0.0285(3) Uani 1 1 d .
O2 O -0.16497(19) 0.2500 0.09377(17) 0.0306(4) Uani 1 2 d S
O3 O 0.0592(2) 0.2500 0.49617(15) 0.0328(4) Uani 1 2 d S
Si1 Si 0.43003(6) 0.2500 0.33628(5) 0.01910(13) Uani 1 2 d S
C1 C 0.2664(2) 0.2500 0.08879(18) 0.0170(4) Uani 1 2 d S
C2 C 0.30166(16) 0.15315(11) 0.03116(13) 0.0191(3) Uani 1 1 d .
C3 C 0.37722(17) 0.15214(12) -0.07962(14) 0.0238(3) Uani 1 1 d .
H3 H 0.4025 0.0862 -0.1176 0.029 Uiso 1 1 calc R
C4 C 0.4146(3) 0.2500 -0.1331(2) 0.0268(4) Uani 1 2 d S
H4 H 0.4669 0.2500 -0.2078 0.032 Uiso 1 2 calc SR
C5 C 0.24559(16) 0.06680(11) 0.10556(14) 0.0200(3) Uani 1 1 d .
C6 C 0.1803(3) -0.09527(14) 0.1736(2) 0.0464(5) Uani 1 1 d .
H6A H 0.2591 -0.1437 0.2214 0.056 Uiso 1 1 calc R
H6B H 0.0886 -0.1388 0.1351 0.056 Uiso 1 1 calc R
C7 C 0.12352(18) -0.00909(11) 0.26296(15) 0.0221(3) Uani 1 1 d .
C8 C -0.05736(19) -0.00663(14) 0.25695(18) 0.0334(4) Uani 1 1 d .
H8A H -0.0891 0.0520 0.3104 0.050 Uiso 1 1 calc R
H8B H -0.0951 -0.0751 0.2879 0.050 Uiso 1 1 calc R
H8C H -0.1045 0.0048 0.1687 0.050 Uiso 1 1 calc R
C9 C 0.1984(2) -0.02403(14) 0.39984(17) 0.0336(4) Uani 1 1 d .
H9A H 0.3151 -0.0236 0.4031 0.050 Uiso 1 1 calc R
H9B H 0.1637 -0.0928 0.4323 0.050 Uiso 1 1 calc R
H9C H 0.1647 0.0346 0.4524 0.050 Uiso 1 1 calc R
C10 C -0.0421(2) 0.2500 0.15089(19) 0.0187(4) Uani 1 2 d S
C11 C 0.0989(2) 0.2500 0.3952(2) 0.0201(4) Uani 1 2 d S
C12 C 0.4516(3) 0.2500 0.5173(2) 0.0322(5) Uani 1 2 d S
H12A H 0.4132 0.3186 0.5476 0.048 Uiso 0.50 1 calc PR
H12B H 0.5644 0.2404 0.5506 0.048 Uiso 0.50 1 calc PR
H12C H 0.3885 0.1911 0.5471 0.048 Uiso 0.50 1 calc PR
C13 C 0.55578(18) 0.13154(13) 0.29641(16) 0.0283(3) Uani 1 1 d .
H13A H 0.5656 0.1318 0.2050 0.043 Uiso 1 1 calc R
H13B H 0.5046 0.0647 0.3189 0.043 Uiso 1 1 calc R
H13C H 0.6623 0.1369 0.3447 0.043 Uiso 1 1 calc R
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'
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
C11 Fe1 C10 97.35(9) . .
C11 Fe1 C1 167.79(8) . .
C10 Fe1 C1 94.86(9) . .
C11 Fe1 N1 101.32(3) . 4_565
C10 Fe1 N1 90.89(4) . 4_565
C1 Fe1 N1 78.44(3) . 4_565
C11 Fe1 N1 101.32(3) . .
C10 Fe1 N1 90.89(4) . .
C1 Fe1 N1 78.44(3) . .
N1 Fe1 N1 156.87(7) 4_565 .
C11 Fe1 Si1 87.53(7) . .
C10 Fe1 Si1 175.12(6) . .
C1 Fe1 Si1 80.26(6) . .
N1 Fe1 Si1 88.14(3) 4_565 .
N1 Fe1 Si1 88.14(3) . .
C5 N1 C7 108.45(12) . .
C5 N1 Fe1 115.34(9) . .
C7 N1 Fe1 135.77(9) . .
C5 O1 C6 105.55(12) . .
C13 Si1 C13 102.35(11) . 4_565
C13 Si1 C12 103.64(7) . .
C13 Si1 C12 103.64(7) 4_565 .
C13 Si1 Fe1 115.80(5) . .
C13 Si1 Fe1 115.80(5) 4_565 .
C12 Si1 Fe1 113.93(8) . .
C2 C1 C2 119.03(18) 4_565 .
C2 C1 Fe1 120.42(9) 4_565 .
C2 C1 Fe1 120.42(9) . .
C1 C2 C3 120.97(14) . .
C1 C2 C5 107.66(13) . .
C3 C2 C5 131.37(13) . .
C4 C3 C2 118.64(14) . .
C3 C4 C3 121.68(19) . 4_565
N1 C5 O1 117.63(13) . .
N1 C5 C2 118.06(12) . .
O1 C5 C2 124.29(13) . .
O1 C6 C7 106.61(13) . .
N1 C7 C8 109.59(12) . .
N1 C7 C9 111.48(12) . .
C8 C7 C9 110.02(14) . .
N1 C7 C6 101.68(12) . .
C8 C7 C6 111.82(15) . .
C9 C7 C6 112.00(15) . .
O2 C10 Fe1 178.33(18) . .
O3 C11 Fe1 179.31(19) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C11 1.789(2) .
Fe1 C10 1.823(2) .
Fe1 C1 1.920(2) .
Fe1 N1 2.0121(13) 4_565
Fe1 N1 2.0121(13) .
Fe1 Si1 2.4006(10) .
N1 C5 1.2980(18) .
N1 C7 1.4913(18) .
O1 C5 1.3473(17) .
O1 C6 1.456(2) .
O2 C10 1.134(3) .
O3 C11 1.156(3) .
Si1 C13 1.8928(16) .
Si1 C13 1.8928(16) 4_565
Si1 C12 1.902(2) .
C1 C2 1.3989(17) 4_565
C1 C2 1.3990(17) .
C2 C3 1.399(2) .
C2 C5 1.445(2) .
C3 C4 1.3950(19) .
C4 C3 1.3950(19) 4_565
C6 C7 1.543(2) .
C7 C8 1.518(2) .
C7 C9 1.520(2) .
