#------------------------------------------------------------------------------
#$Date: 2019-11-25 12:23:53 +0200 (Mon, 25 Nov 2019) $
#$Revision: 240856 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/04/4130417.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_4130417
loop_
_publ_author_name
'Lang, Georgette M.'
'Shima, Takanori'
'Wang, Leyong'
'Cluff, Kyle J.'
'Skopek, Katrin'
'Hampel, Frank'
'Blümel, Janet'
'Gladysz, John A.'
_publ_section_title
;
 Gyroscope-Like Complexes Based on Dibridgehead Diphosphine Cages That Are
 Accessed by Three-Fold Intramolecular Ring Closing Metatheses and Encase
 Fe(CO)3, Fe(CO)2(NO)(+), and Fe(CO)3(H)(+) Rotators.
;
_journal_issue                   24
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              7649
_journal_page_last               7663
_journal_paper_doi               10.1021/jacs.6b03178
_journal_volume                  138
_journal_year                    2016
_chemical_formula_sum            'C45 H84 Fe O3 P2'
_chemical_formula_weight         790.91
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 1 2/c 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                 122.839(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   21.5104(8)
_cell_length_b                   13.9765(6)
_cell_length_c                   18.3436(8)
_cell_measurement_reflns_used    5272
_cell_measurement_temperature    173(2)
_cell_volume                     4633.5(3)
_computing_cell_refinement       DENZO-SMN
_computing_data_collection       'Nonius Collect'
_computing_data_reduction        DENZO-SMN
_computing_molecular_graphics    'SHELXTL NT'
_computing_publication_material  'SHELXTL NT'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 9
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0478
_diffrn_reflns_av_sigmaI/netI    0.0680
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            10223
_diffrn_reflns_theta_full        27.49
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.25
_exptl_absorpt_coefficient_mu    0.430
_exptl_absorpt_correction_T_max  0.9583
_exptl_absorpt_correction_T_min  0.8642
_exptl_absorpt_correction_type   'empirical (Scalepack)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.134
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.241
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     232
_refine_ls_number_reflns         5304
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.0889
_refine_ls_R_factor_gt           0.0428
_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)+(0.0436P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0907
_refine_ls_wR_factor_ref         0.1036
_reflns_number_gt                3295
_reflns_number_total             5304
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja6b03178_si_002.cif
_cod_data_source_block           ts06
_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      C2/c
_cod_database_code               4130417
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -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
Fe1 Fe 0.5000 0.51235(3) -0.2500 0.03019(13) Uani 1 2 d S
P1 P 0.62201(2) 0.51391(4) -0.16982(3) 0.03056(14) Uani 1 1 d .
O1 O 0.5000 0.30318(14) -0.2500 0.0591(7) Uani 1 2 d S
C1 C 0.5000 0.3863(2) -0.2500 0.0379(7) Uani 1 2 d S
O2 O 0.49504(8) 0.61308(12) -0.11325(11) 0.0551(5) Uani 1 1 d .
C2 C 0.49714(10) 0.57353(14) -0.16773(15) 0.0377(5) Uani 1 1 d .
C11 C 0.66567(10) 0.42559(14) -0.08195(14) 0.0372(5) Uani 1 1 d .
H11A H 0.6586 0.3611 -0.1077 0.045 Uiso 1 1 calc R
H11B H 0.7195 0.4384 -0.0461 0.045 Uiso 1 1 calc R
C12 C 0.63575(12) 0.42518(15) -0.02311(15) 0.0445(6) Uani 1 1 d .
H12A H 0.6472 0.4876 0.0070 0.053 Uiso 1 1 calc R
H12B H 0.5812 0.4189 -0.0597 0.053 Uiso 1 1 calc R
C13 C 0.66655(13) 0.34565(16) 0.04484(16) 0.0498(6) Uani 1 1 d .
H13A H 0.7206 0.3547 0.0847 0.060 Uiso 1 1 calc R
H13B H 0.6440 0.3506 0.0795 0.060 Uiso 1 1 calc R
C14 C 0.65180(13) 0.24615(15) 0.00489(17) 0.0468(6) Uani 1 1 d .
H14A H 0.6883 0.2329 -0.0109 0.056 Uiso 1 1 calc R
H14B H 0.6020 0.2455 -0.0492 0.056 Uiso 1 1 calc R
C15 C 0.65594(13) 0.16610(17) 0.06403(17) 0.0532(7) Uani 1 1 d .
H15A H 0.6564 0.1039 0.0385 0.064 Uiso 1 1 calc R
H15B H 0.7033 0.1719 0.1209 0.064 Uiso 1 1 calc R
C17 C 0.59328(13) 0.16525(17) 0.07910(16) 0.0511(6) Uani 1 1 d .
H17A H 0.5935 0.2265 0.1064 0.061 Uiso 1 1 calc R
H17B H 0.6020 0.1131 0.1201 0.061 Uiso 1 1 calc R
C18 C 0.51750(13) 0.15135(18) -0.00387(16) 0.0508(6) Uani 1 1 d .
H18A H 0.5072 0.2062 -0.0431 0.061 Uiso 1 1 calc R
H18B H 0.5185 0.0927 -0.0335 0.061 Uiso 1 1 calc R
C19 C 0.45524(13) 0.14297(17) 0.01193(17) 0.0506(6) Uani 1 1 d .
H19A H 0.4537 0.2022 0.0405 0.061 Uiso 1 1 calc R
H19B H 0.4662 0.0891 0.0522 0.061 Uiso 1 1 calc R
C20 C 0.37926(13) 0.12700(17) -0.07053(17) 0.0532(7) Uani 1 1 d .
H20A H 0.3426 0.1189 -0.0542 0.064 Uiso 1 1 calc R
H20B H 0.3805 0.0666 -0.0979 0.064 Uiso 1 1 calc R
C21 C 0.35266(13) 0.20768(16) -0.13809(17) 0.0493(6) Uani 1 1 d .
H21A H 0.3865 0.2115 -0.1589 0.059 Uiso 1 1 calc R
H21B H 0.3029 0.1911 -0.1884 0.059 Uiso 1 1 calc R
C22 C 0.34891(13) 0.30489(16) -0.10457(16) 0.0484(6) Uani 1 1 d .
H22A H 0.3997 0.3249 -0.0589 0.058 Uiso 1 1 calc R
H22B H 0.3199 0.2993 -0.0774 0.058 Uiso 1 1 calc R
C23 C 0.31423(12) 0.38250(16) -0.17404(16) 0.0449(6) Uani 1 1 d .
H23A H 0.2633 0.3628 -0.2195 0.054 Uiso 1 1 calc R
H23B H 0.3107 0.4423 -0.1475 0.054 Uiso 1 1 calc R
C24 C 0.35730(11) 0.40273(15) -0.21626(15) 0.0393(5) Uani 1 1 d .
H24A H 0.3528 0.3470 -0.2521 0.047 Uiso 1 1 calc R
H24B H 0.4103 0.4104 -0.1703 0.047 Uiso 1 1 calc R
C25 C 0.33090(10) 0.49206(14) -0.27315(14) 0.0360(5) Uani 1 1 d .
H25A H 0.3384 0.5483 -0.2364 0.043 Uiso 1 1 calc R
H25B H 0.2771 0.4861 -0.3166 0.043 Uiso 1 1 calc R
C31 C 0.66314(10) 0.62679(14) -0.11293(14) 0.0365(5) Uani 1 1 d .
H31A H 0.6516 0.6357 -0.0679 0.044 Uiso 1 1 calc R
H31B H 0.7176 0.6223 -0.0831 0.044 Uiso 1 1 calc R
C32 C 0.63635(11) 0.71444(14) -0.17197(15) 0.0411(5) Uani 1 1 d .
H32A H 0.6583 0.7131 -0.2075 0.049 Uiso 1 1 calc R
H32B H 0.5819 0.7105 -0.2121 0.049 Uiso 1 1 calc R
C33 C 0.65568(11) 0.80922(14) -0.12376(15) 0.0383(5) Uani 1 1 d .
H33A H 0.6369 0.8091 -0.0850 0.046 Uiso 1 1 calc R
H33B H 0.7102 0.8160 -0.0871 0.046 Uiso 1 1 calc R
C34 C 0.62321(12) 0.89438(14) -0.18482(15) 0.0415(5) Uani 1 1 d .
H34A H 0.6441 0.8959 -0.2214 0.050 Uiso 1 1 calc R
H34B H 0.5691 0.8851 -0.2238 0.050 Uiso 1 1 calc R
C35 C 0.63750(13) 0.99047(14) -0.13957(16) 0.0474(6) Uani 1 1 d .
H35A H 0.6915 0.9989 -0.0991 0.057 Uiso 1 1 calc R
H35B H 0.6149 0.9901 -0.1048 0.057 Uiso 1 1 calc R
C36 C 0.60698(14) 1.07505(15) -0.20177(17) 0.0544(7) Uani 1 1 d .
H36A H 0.6185 1.1345 -0.1673 0.065 Uiso 1 1 calc R
H36B H 0.6331 1.0784 -0.2325 0.065 Uiso 1 1 calc R
C37 C 0.52410(14) 1.07231(15) -0.26909(16) 0.0512(6) Uani 1 1 d .
H37A H 0.5127 1.0142 -0.3051 0.061 Uiso 1 1 calc R
H37B H 0.5107 1.1285 -0.3077 0.061 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'
O O 0.0106 0.0060 '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
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
C1 Fe1 C2 118.99(7) . 2_654
C1 Fe1 C2 118.99(7) . .
C2 Fe1 C2 122.02(14) 2_654 .
C1 Fe1 P1 90.565(17) . .
C2 Fe1 P1 89.13(6) 2_654 .
C2 Fe1 P1 90.32(6) . .
C1 Fe1 P1 90.565(17) . 2_654
C2 Fe1 P1 90.32(6) 2_654 2_654
C2 Fe1 P1 89.13(6) . 2_654
P1 Fe1 P1 178.87(3) . 2_654
C31 P1 C11 102.71(10) . .
C31 P1 C25 102.86(10) . 2_654
C11 P1 C25 102.20(9) . 2_654
C31 P1 Fe1 114.88(7) . .
C11 P1 Fe1 115.89(7) . .
C25 P1 Fe1 116.33(7) 2_654 .
O1 C1 Fe1 180.000(1) . .
O2 C2 Fe1 179.3(2) . .
C12 C11 P1 114.36(14) . .
C13 C12 C11 114.64(18) . .
C14 C13 C12 112.8(2) . .
C13 C14 C15 114.2(2) . .
C17 C15 C14 114.85(19) . .
C15 C17 C18 113.2(2) . .
C19 C18 C17 113.3(2) . .
C18 C19 C20 113.8(2) . .
C19 C20 C21 114.95(19) . .
C22 C21 C20 114.2(2) . .
C21 C22 C23 114.2(2) . .
C24 C23 C22 113.61(17) . .
C23 C24 C25 113.37(17) . .
C24 C25 P1 114.24(14) . 2_654
C32 C31 P1 114.02(15) . .
C33 C32 C31 114.07(18) . .
C34 C33 C32 112.47(18) . .
C35 C34 C33 114.42(19) . .
C34 C35 C36 113.6(2) . .
C37 C36 C35 115.32(18) . .
C36 C37 C37 114.4(3) . 2_654
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 C1 1.761(3) .
Fe1 C2 1.764(2) 2_654
Fe1 C2 1.764(2) .
Fe1 P1 2.2056(5) .
Fe1 P1 2.2056(5) 2_654
P1 C31 1.8329(19) .
P1 C11 1.834(2) .
P1 C25 1.834(2) 2_654
O1 C1 1.162(3) .
O2 C2 1.164(3) .
C11 C12 1.527(3) .
C12 C13 1.527(3) .
C13 C14 1.523(3) .
C14 C15 1.527(3) .
C15 C17 1.516(3) .
C17 C18 1.523(3) .
C18 C19 1.520(3) .
C19 C20 1.526(3) .
C20 C21 1.538(3) .
C21 C22 1.511(3) .
C22 C23 1.525(3) .
C23 C24 1.522(3) .
C24 C25 1.526(3) .
C25 P1 1.834(2) 2_654
C31 C32 1.526(3) .
C32 C33 1.520(3) .
C33 C34 1.520(3) .
C34 C35 1.520(3) .
C35 C36 1.522(3) .
C36 C37 1.522(3) .
C37 C37 1.534(5) 2_654
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_4
C1 Fe1 P1 C31 -160.78(8) . .
C2 Fe1 P1 C31 80.24(11) 2_654 .
C2 Fe1 P1 C31 -41.78(11) . .
P1 Fe1 P1 C31 19.23(9) 2_654 .
C1 Fe1 P1 C11 -41.14(8) . .
C2 Fe1 P1 C11 -160.12(11) 2_654 .
C2 Fe1 P1 C11 77.86(11) . .
P1 Fe1 P1 C11 138.87(8) 2_654 .
C1 Fe1 P1 C25 79.01(7) . 2_654
C2 Fe1 P1 C25 -39.97(10) 2_654 2_654
C2 Fe1 P1 C25 -162.00(10) . 2_654
P1 Fe1 P1 C25 -100.99(8) 2_654 2_654
C2 Fe1 C1 O1 0(100) 2_654 .
C2 Fe1 C1 O1 0(100) . .
P1 Fe1 C1 O1 0(100) . .
P1 Fe1 C1 O1 0(100) 2_654 .
C1 Fe1 C2 O2 -16(20) . .
C2 Fe1 C2 O2 164(100) 2_654 .
P1 Fe1 C2 O2 -107(20) . .
P1 Fe1 C2 O2 74(20) 2_654 .
C31 P1 C11 C12 74.90(17) . .
C25 P1 C11 C12 -178.71(15) 2_654 .
Fe1 P1 C11 C12 -51.17(18) . .
P1 C11 C12 C13 174.47(15) . .
C11 C12 C13 C14 -58.3(3) . .
C12 C13 C14 C15 -159.3(2) . .
C13 C14 C15 C17 70.3(3) . .
C14 C15 C17 C18 61.3(3) . .
C15 C17 C18 C19 175.7(2) . .
C17 C18 C19 C20 -178.82(19) . .
C18 C19 C20 C21 -61.3(3) . .
C19 C20 C21 C22 -57.6(3) . .
C20 C21 C22 C23 -173.32(19) . .
C21 C22 C23 C24 -62.6(3) . .
C22 C23 C24 C25 -169.37(19) . .
C23 C24 C25 P1 -176.38(15) . 2_654
C11 P1 C31 C32 179.64(15) . .
C25 P1 C31 C32 73.76(17) 2_654 .
Fe1 P1 C31 C32 -53.63(17) . .
P1 C31 C32 C33 166.38(15) . .
C31 C32 C33 C34 -175.75(18) . .
C32 C33 C34 C35 176.82(19) . .
C33 C34 C35 C36 177.87(19) . .
C34 C35 C36 C37 58.2(3) . .
C35 C36 C37 C37 61.3(2) . 2_654
