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#$Date: 2016-03-21 08:17:57 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178601 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/12/4071294.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_4071294
loop_
_publ_author_name
'Allen, Olivia R.'
'Dalgarno, Scott J.'
'Field, Leslie D.'
'Jensen, Paul'
'Turnbull, Anthony J.'
'Willis, Anthony C.'
_publ_section_title
;
 Addition of CO2to Alkyl Iron Complexes, Fe(PP)2Me2
;
_journal_issue                   9
_journal_name_full               Organometallics
_journal_page_first              2092
_journal_paper_doi               10.1021/om800091a
_journal_volume                  27
_journal_year                    2008
_chemical_formula_moiety         'C22 H51 Fe O2 P4, C24 H20 B'
_chemical_formula_sum            'C46 H71 B Fe O2 P4'
_chemical_formula_weight         846.57
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           73
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-I 2b 2c'
_symmetry_space_group_name_H-M   'I b c a'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   17.3563(4)
_cell_length_b                   22.1987(6)
_cell_length_c                   24.0438(6)
_cell_measurement_temperature    223(2)
_cell_volume                     9263.8(4)
_computing_cell_refinement       'Bruker Apex2'
_computing_data_collection       'Bruker Apex2'
_computing_data_reduction        'Bruker Apex2'
_computing_molecular_graphics    XSEED
_computing_publication_material  XSEED
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      223(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker-Nonius Kappa ApexII'
_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  0.0268
_diffrn_reflns_av_sigmaI/netI    0.0112
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            88581
_diffrn_reflns_theta_full        27.59
_diffrn_reflns_theta_max         27.59
_diffrn_reflns_theta_min         2.66
_exptl_absorpt_coefficient_mu    0.499
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.857
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.214
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             3632
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.37
_exptl_crystal_size_min          0.25
_refine_diff_density_max         0.993
_refine_diff_density_min         -0.841
_refine_diff_density_rms         0.063
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.088
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     251
_refine_ls_number_reflns         5357
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0567
_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)+(0.0509P)²+25.5722P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1325
_refine_ls_wR_factor_ref         0.1545
_reflns_number_gt                4144
_reflns_number_total             5357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            om800091a-file002.cif
_cod_data_source_block           a7_05
_cod_original_sg_symbol_H-M      Ibca
_cod_database_code               4071294
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y+1/2, z'
'x, -y, -z+1/2'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1, z+1/2'
'x+1/2, -y+1/2, -z+1'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y-1/2, -z'
'-x, y, z-1/2'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y, -z+1/2'
'-x+1/2, y+1/2, 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 0.5000 0.2500 0.31093(2) 0.03841(15) Uani 1 2 d S
P1 P 0.49703(4) 0.35299(3) 0.30770(3) 0.04628(19) Uani 1 1 d .
P2 P 0.40022(5) 0.25802(4) 0.36657(3) 0.0541(2) Uani 1 1 d .
O1 O 0.43800(11) 0.25482(9) 0.23828(8) 0.0479(5) Uani 1 1 d .
C1 C 0.5300(3) 0.46881(15) 0.35533(19) 0.0827(12) Uani 1 1 d .
H1A H 0.5453 0.4845 0.3193 0.124 Uiso 1 1 calc R
H1B H 0.5586 0.4893 0.3843 0.124 Uiso 1 1 calc R
H1C H 0.4752 0.4755 0.3608 0.124 Uiso 1 1 calc R
C2 C 0.5469(2) 0.40134(14) 0.35782(14) 0.0618(8) Uani 1 1 d .
H2A H 0.5342 0.3871 0.3953 0.074 Uiso 1 1 calc R
H2B H 0.6025 0.3958 0.3527 0.074 Uiso 1 1 calc R
C3 C 0.5166(2) 0.38995(16) 0.24116(15) 0.0639(9) Uani 1 1 d .
H3A H 0.4886 0.3686 0.2118 0.077 Uiso 1 1 calc R
H3B H 0.4966 0.4312 0.2427 0.077 Uiso 1 1 calc R
C4 C 0.6016(2) 0.39233(18) 0.22554(17) 0.0796(12) Uani 1 1 d .
H4A H 0.6294 0.4161 0.2528 0.119 Uiso 1 1 calc R
H4B H 0.6072 0.4106 0.1891 0.119 Uiso 1 1 calc R
H4C H 0.6224 0.3518 0.2247 0.119 Uiso 1 1 calc R
C5 C 0.3958(2) 0.37057(16) 0.32075(19) 0.0724(11) Uani 1 1 d .
H5A H 0.3888 0.4141 0.3254 0.087 Uiso 1 1 calc R
H5B H 0.3637 0.3570 0.2896 0.087 Uiso 1 1 calc R
C6 C 0.3736(2) 0.33723(17) 0.37415(19) 0.0794(12) Uani 1 1 d .
H6A H 0.3181 0.3408 0.3806 0.095 Uiso 1 1 calc R
H6B H 0.4007 0.3549 0.4060 0.095 Uiso 1 1 calc R
C7 C 0.4032(3) 0.2290(2) 0.43897(16) 0.0889(13) Uani 1 1 d .
H7A H 0.4299 0.1901 0.4384 0.107 Uiso 1 1 calc R
H7B H 0.4349 0.2567 0.4611 0.107 Uiso 1 1 calc R
C8 C 0.3310(4) 0.2209(3) 0.4676(2) 0.131(2) Uani 1 1 d .
H8A H 0.3011 0.2578 0.4654 0.196 Uiso 1 1 calc R
H8B H 0.3407 0.2112 0.5063 0.196 Uiso 1 1 calc R
H8C H 0.3025 0.1883 0.4503 0.196 Uiso 1 1 calc R
C9 C 0.31586(19) 0.22346(18) 0.33319(17) 0.0662(9) Uani 1 1 d .
H9A H 0.3268 0.2207 0.2933 0.079 Uiso 1 1 calc R
H9B H 0.3117 0.1821 0.3472 0.079 Uiso 1 1 calc R
C10 C 0.2378(2) 0.2524(2) 0.3394(3) 0.0964(15) Uani 1 1 d .
H10A H 0.2230 0.2524 0.3783 0.145 Uiso 1 1 calc R
H10B H 0.2002 0.2299 0.3180 0.145 Uiso 1 1 calc R
H10C H 0.2399 0.2935 0.3259 0.145 Uiso 1 1 calc R
C11 C 0.5000 0.2500 0.21157(17) 0.0486(9) Uani 1 2 d S
C12 C 0.5000 0.2500 0.1493(2) 0.0791(17) Uani 1 2 d S
H12A H 0.4473 0.2491 0.1358 0.119 Uiso 0.50 1 calc PR
H12B H 0.5273 0.2148 0.1358 0.119 Uiso 0.50 1 calc PR
H12C H 0.5254 0.2861 0.1358 0.119 Uiso 0.50 1 calc PR
C13 C 0.26560(16) 0.51802(14) 0.44431(12) 0.0486(7) Uani 1 1 d .
C14 C 0.2441(2) 0.49959(18) 0.39101(14) 0.0650(9) Uani 1 1 d .
H14 H 0.2147 0.4643 0.3872 0.078 Uiso 1 1 calc R
C15 C 0.2644(3) 0.5310(2) 0.34359(17) 0.0853(12) Uani 1 1 d .
H15 H 0.2491 0.5168 0.3085 0.102 Uiso 1 1 calc R
C16 C 0.3067(3) 0.5828(2) 0.34753(19) 0.0884(14) Uani 1 1 d .
H16 H 0.3206 0.6041 0.3153 0.106 Uiso 1 1 calc R
C17 C 0.3288(2) 0.60361(19) 0.3991(2) 0.0806(12) Uani 1 1 d .
H17 H 0.3576 0.6393 0.4023 0.097 Uiso 1 1 calc R
C18 C 0.3083(2) 0.57148(16) 0.44652(16) 0.0628(8) Uani 1 1 d .
H18 H 0.3236 0.5863 0.4814 0.075 Uiso 1 1 calc R
C19 C 0.17355(15) 0.43453(13) 0.48964(11) 0.0428(6) Uani 1 1 d .
C20 C 0.17741(17) 0.38106(16) 0.45902(15) 0.0600(8) Uani 1 1 d .
H20 H 0.2259 0.3676 0.4469 0.072 Uiso 1 1 calc R
C21 C 0.1131(2) 0.34708(18) 0.44576(17) 0.0710(10) Uani 1 1 d .
H21 H 0.1186 0.3114 0.4250 0.085 Uiso 1 1 calc R
C22 C 0.04104(18) 0.36532(16) 0.46286(15) 0.0618(8) Uani 1 1 d .
H22 H -0.0029 0.3428 0.4534 0.074 Uiso 1 1 calc R
C23 C 0.03461(16) 0.41694(14) 0.49395(14) 0.0519(7) Uani 1 1 d .
H23 H -0.0141 0.4298 0.5062 0.062 Uiso 1 1 calc R
C24 C 0.09955(15) 0.45018(12) 0.50741(12) 0.0433(6) Uani 1 1 d .
H24 H 0.0936 0.4848 0.5295 0.052 Uiso 1 1 calc R
B1 B 0.2500 0.4767(2) 0.5000 0.0430(9) Uani 1 2 d S
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'
B B 0.0013 0.0007 '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
O1 Fe1 O1 63.52(11) . 2_655
O1 Fe1 P2 95.78(6) . .
O1 Fe1 P2 159.30(6) 2_655 .
O1 Fe1 P2 159.30(6) . 2_655
O1 Fe1 P2 95.78(6) 2_655 2_655
P2 Fe1 P2 104.92(5) . 2_655
O1 Fe1 P1 92.00(6) . 2_655
O1 Fe1 P1 84.68(6) 2_655 2_655
P2 Fe1 P1 96.87(3) . 2_655
P2 Fe1 P1 85.52(3) 2_655 2_655
O1 Fe1 P1 84.68(6) . .
O1 Fe1 P1 92.00(6) 2_655 .
P2 Fe1 P1 85.52(3) . .
P2 Fe1 P1 96.87(3) 2_655 .
P1 Fe1 P1 176.10(5) 2_655 .
O1 Fe1 C11 31.76(5) . .
O1 Fe1 C11 31.76(5) 2_655 .
P2 Fe1 C11 127.54(3) . .
P2 Fe1 C11 127.54(3) 2_655 .
P1 Fe1 C11 88.05(2) 2_655 .
P1 Fe1 C11 88.05(2) . .
C5 P1 C3 103.48(18) . .
C5 P1 C2 102.51(18) . .
C3 P1 C2 102.98(17) . .
C5 P1 Fe1 103.25(12) . .
C3 P1 Fe1 118.27(12) . .
C2 P1 Fe1 123.54(11) . .
C6 P2 C9 104.13(19) . .
C6 P2 C7 104.3(2) . .
C9 P2 C7 106.7(2) . .
C6 P2 Fe1 109.76(12) . .
C9 P2 Fe1 109.18(12) . .
C7 P2 Fe1 121.39(17) . .
C11 O1 Fe1 88.93(19) . .
C1 C2 P1 117.2(3) . .
C4 C3 P1 114.3(3) . .
C6 C5 P1 106.4(3) . .
C5 C6 P2 108.5(2) . .
C8 C7 P2 117.8(4) . .
C10 C9 P2 119.7(3) . .
O1 C11 O1 118.6(4) 2_655 .
O1 C11 C12 120.70(18) 2_655 .
O1 C11 C12 120.70(18) . .
O1 C11 Fe1 59.30(18) 2_655 .
O1 C11 Fe1 59.30(18) . .
C12 C11 Fe1 180.0 . .
C14 C13 C18 115.1(3) . .
C14 C13 B1 122.7(3) . .
C18 C13 B1 121.9(3) . .
C15 C14 C13 122.8(4) . .
C16 C15 C14 120.3(4) . .
C15 C16 C17 119.6(4) . .
C16 C17 C18 119.6(4) . .
C17 C18 C13 122.6(4) . .
C24 C19 C20 114.6(3) . .
C24 C19 B1 123.6(2) . .
C20 C19 B1 121.7(2) . .
C21 C20 C19 123.0(3) . .
C22 C21 C20 120.2(3) . .
C23 C22 C21 118.8(3) . .
C22 C23 C24 120.4(3) . .
C23 C24 C19 122.9(3) . .
C19 B1 C19 110.5(3) 4_556 .
C19 B1 C13 107.95(13) 4_556 .
C19 B1 C13 109.09(14) . .
C19 B1 C13 109.09(14) 4_556 4_556
C19 B1 C13 107.95(13) . 4_556
C13 B1 C13 112.3(3) . 4_556
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe1 O1 2.0546(19) .
Fe1 O1 2.0546(19) 2_655
Fe1 P2 2.1956(8) .
Fe1 P2 2.1956(8) 2_655
Fe1 P1 2.2881(7) 2_655
Fe1 P1 2.2881(7) .
Fe1 C11 2.389(4) .
P1 C5 1.827(3) .
P1 C3 1.830(3) .
P1 C2 1.832(3) .
P2 C6 1.827(4) .
P2 C9 1.838(4) .
P2 C7 1.857(4) .
O1 C11 1.258(3) .
C1 C2 1.528(5) .
C3 C4 1.523(5) .
C5 C6 1.531(6) .
C7 C8 1.441(7) .
C9 C10 1.507(5) .
C11 O1 1.258(3) 2_655
C11 C12 1.497(6) .
C13 C14 1.396(4) .
C13 C18 1.400(5) .
C13 B1 1.645(4) .
C14 C15 1.382(5) .
C15 C16 1.367(7) .
C16 C17 1.378(7) .
C17 C18 1.391(5) .
C19 C24 1.397(4) .
C19 C20 1.398(4) .
C19 B1 1.643(4) .
C20 C21 1.385(5) .
C21 C22 1.377(5) .
C22 C23 1.373(5) .
C23 C24 1.386(4) .
B1 C19 1.643(4) 4_556
B1 C13 1.645(4) 4_556
