#------------------------------------------------------------------------------
#$Date: 2019-11-25 01:38:59 +0200 (Mon, 25 Nov 2019) $
#$Revision: 239888 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/35/04/4350422.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_4350422
loop_
_publ_author_name
'Trovitch, Ryan J.'
'Lobkovsky, Emil'
'Chirik, Paul J.'
_publ_section_title
;
 Bis(diisopropylphosphino)pyridine iron dicarbonyl, dihydride, and silyl
 hydride complexes.
;
_journal_issue                   18
_journal_name_full               'Inorganic chemistry'
_journal_page_first              7252
_journal_page_last               7260
_journal_paper_doi               10.1021/ic0608647
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C26 H43 Fe N O P2 Si'
_chemical_formula_weight         531.49
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 105.723(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.2739(5)
_cell_length_b                   12.2884(5)
_cell_length_c                   17.7620(7)
_cell_measurement_reflns_used    9103
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      29.68
_cell_measurement_theta_min      2.48
_cell_volume                     2788.84(19)
_computing_cell_refinement       'Bruker SAINT+'
_computing_data_collection       'Bruker APEX2'
_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      173(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker X8 APEX II diffractometer'
_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  0.0415
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            43132
_diffrn_reflns_theta_full        30.51
_diffrn_reflns_theta_max         30.51
_diffrn_reflns_theta_min         1.59
_exptl_absorpt_coefficient_mu    0.717
_exptl_absorpt_correction_T_max  0.9318
_exptl_absorpt_correction_T_min  0.8699
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            dark
_exptl_crystal_density_diffrn    1.266
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1136
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.884
_refine_diff_density_min         -0.551
_refine_diff_density_rms         0.078
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     461
_refine_ls_number_reflns         8494
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_gt           0.0375
_refine_ls_shift/su_max          0.040
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[σ²(Fo²)+(0.0592P)²+0.2072P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0964
_refine_ls_wR_factor_ref         0.1033
_reflns_number_gt                6552
_reflns_number_total             8494
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0608647si20060518_032301.cif
_cod_data_source_block           rt11
_cod_depositor_comments
;
The following automatic conversions were performed:

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_sg_symbol_H-M      P2(1)/c
_cod_database_code               4350422
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -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
Fe1 Fe 0.244248(16) 0.858511(18) 0.163740(13) 0.01647(7) Uani 1 1 d D
H1FE H 0.1307(13) 0.890(2) 0.1544(13) 0.046(7) Uiso 1 1 d D
P1 P 0.17423(3) 0.77011(3) 0.05597(2) 0.01823(9) Uani 1 1 d .
P2 P 0.28271(3) 0.99047(3) 0.24900(2) 0.01660(9) Uani 1 1 d .
Si1 Si 0.19046(4) 0.74326(4) 0.24484(3) 0.02081(10) Uani 1 1 d .
H2SI H 0.0809(15) 0.7218(16) 0.2238(11) 0.026(5) Uiso 1 1 d .
H1SI H 0.2020(18) 0.7802(18) 0.3245(13) 0.041(6) Uiso 1 1 d .
O1 O 0.44585(10) 0.74741(11) 0.20377(8) 0.0307(3) Uani 1 1 d .
N1 N 0.26171(10) 0.98091(10) 0.08899(8) 0.0190(3) Uani 1 1 d .
C1 C 0.14347(14) 0.88110(14) -0.01678(11) 0.0243(3) Uani 1 1 d .
H1B H 0.0717(16) 0.9048(17) -0.0153(12) 0.029(5) Uiso 1 1 d .
H1A H 0.1409(16) 0.8624(16) -0.0686(13) 0.030(5) Uiso 1 1 d .
C2 C 0.21904(13) 0.97268(13) 0.01048(10) 0.0214(3) Uani 1 1 d .
C3 C 0.24196(15) 1.04661(15) -0.04158(11) 0.0280(4) Uani 1 1 d .
H3 H 0.2141(17) 1.0349(18) -0.0978(14) 0.037(6) Uiso 1 1 d .
C4 C 0.30677(17) 1.13333(16) -0.01274(12) 0.0334(4) Uani 1 1 d .
H4 H 0.3199(18) 1.183(2) -0.0468(14) 0.044(6) Uiso 1 1 d .
C5 C 0.34486(16) 1.14615(15) 0.06695(12) 0.0289(4) Uani 1 1 d .
H5 H 0.3841(18) 1.2029(19) 0.0886(13) 0.039(6) Uiso 1 1 d .
C6 C 0.32144(13) 1.06940(13) 0.11661(10) 0.0217(3) Uani 1 1 d .
C7 C 0.36008(14) 1.08007(14) 0.20322(10) 0.0231(3) Uani 1 1 d .
H7B H 0.3575(14) 1.1502(15) 0.2155(11) 0.016(4) Uiso 1 1 d .
H7A H 0.4305(18) 1.0538(18) 0.2210(13) 0.037(6) Uiso 1 1 d .
C8 C 0.04937(13) 0.69372(15) 0.03821(11) 0.0260(4) Uani 1 1 d .
H8 H 0.0631(16) 0.6391(16) 0.0746(13) 0.029(5) Uiso 1 1 d .
C9 C 0.01427(17) 0.63777(18) -0.04114(13) 0.0352(4) Uani 1 1 d .
H9C H 0.0601(18) 0.582(2) -0.0476(13) 0.041(6) Uiso 1 1 d .
H9B H 0.0102(16) 0.6835(18) -0.0817(13) 0.026(5) Uiso 1 1 d .
H9A H -0.055(2) 0.605(2) -0.0433(15) 0.058(7) Uiso 1 1 d .
C10 C -0.03909(15) 0.76473(18) 0.05095(14) 0.0368(5) Uani 1 1 d .
H10C H -0.0201(18) 0.809(2) 0.1017(14) 0.041(6) Uiso 1 1 d .
H10B H -0.0617(17) 0.8171(19) 0.0108(14) 0.037(6) Uiso 1 1 d .
H10A H -0.099(2) 0.720(2) 0.0505(15) 0.050(7) Uiso 1 1 d .
C11 C 0.25583(14) 0.68046(15) 0.01265(11) 0.0255(3) Uani 1 1 d .
H11 H 0.2130(17) 0.6641(17) -0.0367(12) 0.032(6) Uiso 1 1 d .
C12 C 0.35225(15) 0.74134(17) 0.00309(12) 0.0316(4) Uani 1 1 d .
H12B H 0.3941(14) 0.7709(14) 0.0514(11) 0.015(4) Uiso 1 1 d .
H12A H 0.3294(18) 0.806(2) -0.0325(14) 0.042(6) Uiso 1 1 d .
H12 H 0.397(2) 0.695(2) -0.0192(15) 0.054(7) Uiso 1 1 d .
C13 C 0.28418(17) 0.57565(16) 0.05892(13) 0.0327(4) Uani 1 1 d .
H13C H 0.3219(15) 0.5905(16) 0.1116(12) 0.022(5) Uiso 1 1 d .
H13B H 0.2157(19) 0.5353(19) 0.0603(14) 0.045(6) Uiso 1 1 d .
H13A H 0.3177(18) 0.5236(19) 0.0325(14) 0.043(6) Uiso 1 1 d .
C14 C 0.17774(13) 1.08186(14) 0.26167(11) 0.0241(3) Uani 1 1 d .
H14 H 0.2127(16) 1.1426(16) 0.2930(12) 0.024(5) Uiso 1 1 d .
C15 C 0.10683(16) 1.11920(17) 0.18288(13) 0.0344(4) Uani 1 1 d .
H15C H 0.0570(19) 1.169(2) 0.1954(14) 0.044(6) Uiso 1 1 d .
H15B H 0.069(2) 1.052(2) 0.1518(15) 0.056(7) Uiso 1 1 d .
H15A H 0.1471(19) 1.158(2) 0.1533(14) 0.046(7) Uiso 1 1 d .
C16 C 0.11429(18) 1.02820(19) 0.31104(16) 0.0392(5) Uani 1 1 d .
H16B H 0.059(2) 1.079(2) 0.3176(14) 0.051(7) Uiso 1 1 d .
H16A H 0.078(2) 0.963(2) 0.2838(15) 0.055(8) Uiso 1 1 d .
H16C H 0.156(2) 1.017(2) 0.3616(18) 0.058(8) Uiso 1 1 d .
C17 C 0.36574(13) 0.97575(13) 0.35066(10) 0.0207(3) Uani 1 1 d .
H17 H 0.3215(15) 0.9349(17) 0.3756(11) 0.027(5) Uiso 1 1 d .
C18 C 0.39454(17) 1.08378(16) 0.39358(12) 0.0321(4) Uani 1 1 d .
H18C H 0.4277(19) 1.0689(19) 0.4424(15) 0.043(7) Uiso 1 1 d .
H18B H 0.3276(17) 1.1227(17) 0.3962(13) 0.034(6) Uiso 1 1 d .
H18A H 0.431(2) 1.130(2) 0.3679(15) 0.050(7) Uiso 1 1 d .
C19 C 0.46401(15) 0.90892(17) 0.35442(12) 0.0299(4) Uani 1 1 d .
H19C H 0.5039(17) 0.9033(17) 0.4110(13) 0.033(5) Uiso 1 1 d .
H19B H 0.5038(18) 0.9445(19) 0.3259(14) 0.042(6) Uiso 1 1 d .
H19A H 0.4461(19) 0.837(2) 0.3365(14) 0.046(7) Uiso 1 1 d .
C20 C 0.24823(13) 0.60098(13) 0.26372(10) 0.0229(3) Uani 1 1 d .
C21 C 0.34942(14) 0.58241(15) 0.31111(12) 0.0293(4) Uani 1 1 d .
H21 H 0.387(2) 0.644(2) 0.3369(15) 0.049(7) Uiso 1 1 d .
C22 C 0.39156(17) 0.47846(17) 0.32378(14) 0.0380(5) Uani 1 1 d .
H22 H 0.457(2) 0.4659(19) 0.3592(14) 0.046(7) Uiso 1 1 d .
C23 C 0.33423(19) 0.39034(17) 0.28929(14) 0.0410(5) Uani 1 1 d .
H23 H 0.364(2) 0.322(2) 0.2918(17) 0.068(9) Uiso 1 1 d .
C24 C 0.2336(2) 0.40539(16) 0.24283(14) 0.0420(5) Uani 1 1 d .
H24 H 0.191(2) 0.349(2) 0.2167(15) 0.050(7) Uiso 1 1 d .
C25 C 0.19125(16) 0.50949(16) 0.23078(12) 0.0329(4) Uani 1 1 d .
H25 H 0.1163(18) 0.5136(19) 0.1986(14) 0.042(6) Uiso 1 1 d .
C26 C 0.36739(12) 0.79547(13) 0.18704(9) 0.0197(3) Uani 1 1 d .
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'
P P 0.1023 0.0942 '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
H1FE Fe1 C26 166.2(9)
H1FE Fe1 N1 91.3(9)
C26 Fe1 N1 102.36(6)
H1FE Fe1 P1 81.8(9)
C26 Fe1 P1 97.79(5)
N1 Fe1 P1 83.89(4)
H1FE Fe1 P2 85.6(9)
C26 Fe1 P2 97.85(5)
N1 Fe1 P2 81.88(4)
P1 Fe1 P2 160.761(19)
H1FE Fe1 Si1 75.9(9)
C26 Fe1 Si1 90.46(5)
N1 Fe1 Si1 167.02(4)
P1 Fe1 Si1 96.539(18)
P2 Fe1 Si1 94.469(18)
C1 P1 C11 101.06(8)
C1 P1 C8 103.69(8)
C11 P1 C8 102.97(8)
C1 P1 Fe1 101.97(6)
C11 P1 Fe1 120.23(6)
C8 P1 Fe1 123.40(6)
C7 P2 C14 102.68(8)
C7 P2 C17 103.50(8)
C14 P2 C17 102.10(8)
C7 P2 Fe1 101.05(6)
C14 P2 Fe1 119.54(6)
C17 P2 Fe1 124.71(5)
C20 Si1 Fe1 120.30(5)
C2 N1 C6 118.08(14)
C2 N1 Fe1 121.23(11)
C6 N1 Fe1 120.59(11)
C2 C1 P1 109.08(12)
N1 C2 C3 121.96(16)
N1 C2 C1 116.35(14)
C3 C2 C1 121.66(16)
C4 C3 C2 119.08(18)
C5 C4 C3 119.27(17)
C4 C5 C6 119.62(17)
N1 C6 C5 121.75(16)
N1 C6 C7 116.61(14)
C5 C6 C7 121.64(16)
C6 C7 P2 109.07(11)
C9 C8 C10 109.88(16)
C9 C8 P1 114.89(14)
C10 C8 P1 111.87(13)
C13 C11 C12 112.47(16)
C13 C11 P1 111.50(13)
C12 C11 P1 110.85(13)
C16 C14 C15 110.97(17)
C16 C14 P2 111.09(12)
C15 C14 P2 111.57(13)
C18 C17 C19 110.51(15)
C18 C17 P2 113.85(12)
C19 C17 P2 111.76(12)
C25 C20 C21 116.44(17)
C25 C20 Si1 121.40(14)
C21 C20 Si1 122.15(13)
C22 C21 C20 121.83(19)
C23 C22 C21 120.3(2)
C22 C23 C24 119.50(19)
C23 C24 C25 120.1(2)
C24 C25 C20 121.8(2)
O1 C26 Fe1 175.39(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 H1FE 1.522(15)
Fe1 C26 1.7541(16)
Fe1 N1 2.0605(13)
Fe1 P1 2.1780(5)
Fe1 P2 2.1827(4)
Fe1 Si1 2.2689(5)
P1 C1 1.8469(17)
P1 C11 1.8523(17)
P1 C8 1.8558(17)
P2 C7 1.8387(17)
P2 C14 1.8502(16)
P2 C17 1.8518(17)
Si1 C20 1.9021(17)
O1 C26 1.1635(19)
N1 C2 1.359(2)
N1 C6 1.357(2)
C1 C2 1.498(2)
C2 C3 1.388(2)
C3 C4 1.378(3)
C4 C5 1.377(3)
C5 C6 1.383(2)
C6 C7 1.490(2)
C8 C9 1.523(3)
C8 C10 1.528(3)
C11 C13 1.519(3)
C11 C12 1.531(3)
C14 C16 1.521(3)
C14 C15 1.530(3)
C17 C18 1.527(2)
C17 C19 1.527(2)
C20 C25 1.392(3)
C20 C21 1.397(3)
C21 C22 1.388(3)
C22 C23 1.369(3)
C23 C24 1.380(3)
C24 C25 1.390(3)
