#------------------------------------------------------------------------------
#$Date: 2016-03-23 00:23:57 +0200 (Wed, 23 Mar 2016) $
#$Revision: 179108 $
#$URL: svn://www.crystallography.net/cod/cif/4/30/70/4307068.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_4307068
loop_
_publ_author_name
'John D. Gilbertson'
'Nathaniel K. Szymczak'
'Justin L. Crossland'
'Warren K. Miller'
'David K. Lyon'
'Bruce M. Foxman'
'Joclyn Davis'
'David R. Tyler'
_publ_section_title
;
Coordination Chemistry of H2 and N2 in Aqueous Solution. Reactivity and
Mechanistic Studies Using trans-FeII(P2)2X2-Type Complexes (P2= a Chelating,
Water-Solubilizing Phosphine)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1205
_journal_page_last               1214
_journal_paper_doi               10.1021/ic061570o
_journal_volume                  46
_journal_year                    2007
_chemical_formula_sum            'C40 H86 F12 Fe N2 O8 P6'
_chemical_formula_weight         1192.78
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 106.481(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.8015(13)
_cell_length_b                   11.9842(12)
_cell_length_c                   18.8456(19)
_cell_measurement_reflns_used    2524
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      25.94
_cell_measurement_theta_min      2.25
_cell_volume                     2772.4(5)
_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      153(2)
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.0441
_diffrn_reflns_av_sigmaI/netI    0.0604
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16007
_diffrn_reflns_theta_full        27.11
_diffrn_reflns_theta_max         27.11
_diffrn_reflns_theta_min         1.66
_exptl_absorpt_coefficient_mu    0.532
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.429
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1256
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.535
_refine_diff_density_min         -0.274
_refine_diff_density_rms         0.068
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.987
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     318
_refine_ls_number_reflns         6081
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0737
_refine_ls_R_factor_gt           0.0419
_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)+(0.0473P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0867
_refine_ls_wR_factor_ref         0.0976
_reflns_number_gt                4239
_reflns_number_total             6081
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic061570osi20060818_015204.cif
_cod_data_source_block           jdg11
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_database_code               4307068
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
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.0000 0.5000 0.0000 0.01499(12) Uani 1 2 d S . .
P1 P -0.05715(5) 0.67964(5) 0.01080(3) 0.01661(14) Uani 1 1 d . . .
P2 P 0.16588(5) 0.56487(5) 0.06816(3) 0.01671(14) Uani 1 1 d . . .
N1 N -0.03311(15) 0.45937(16) 0.08971(10) 0.0172(4) Uani 1 1 d . . .
O1 O -0.26974(14) 0.61826(16) 0.16773(10) 0.0346(5) Uani 1 1 d . . .
O2 O -0.29549(15) 0.93346(16) -0.12967(10) 0.0357(5) Uani 1 1 d . . .
O3 O 0.47544(15) 0.38603(16) 0.19514(10) 0.0351(5) Uani 1 1 d . . .
O4 O 0.46863(16) 0.6988(2) 0.01179(11) 0.0543(7) Uani 1 1 d . . .
C1 C 0.13741(19) 0.6855(2) 0.12034(12) 0.0206(5) Uani 1 1 d . . .
H1A H 0.1032 0.6606 0.1586 0.025 Uiso 1 1 calc R . .
H1B H 0.2058 0.7255 0.1450 0.025 Uiso 1 1 calc R . .
C2 C 0.06016(18) 0.7618(2) 0.06472(12) 0.0196(5) Uani 1 1 d . . .
H2A H 0.0986 0.7953 0.0312 0.024 Uiso 1 1 calc R . .
H2B H 0.0348 0.8229 0.0911 0.024 Uiso 1 1 calc R . .
C3 C -0.16039(19) 0.7045(2) 0.05973(12) 0.0214(5) Uani 1 1 d . . .
H3A H -0.1989 0.7746 0.0405 0.026 Uiso 1 1 calc R . .
H3B H -0.2145 0.6434 0.0467 0.026 Uiso 1 1 calc R . .
C4 C -0.1208(2) 0.7129(2) 0.14423(13) 0.0247(6) Uani 1 1 d . . .
H4A H -0.0768 0.6461 0.1644 0.030 Uiso 1 1 calc R . .
H4B H -0.0734 0.7793 0.1584 0.030 Uiso 1 1 calc R . .
C5 C -0.2145(2) 0.7218(2) 0.17771(14) 0.0301(6) Uani 1 1 d . . .
H5A H -0.1870 0.7395 0.2311 0.036 Uiso 1 1 calc R . .
H5B H -0.2648 0.7820 0.1531 0.036 Uiso 1 1 calc R . .
C6 C -0.3707(2) 0.6248(3) 0.18464(16) 0.0458(8) Uani 1 1 d . . .
H6A H -0.3583 0.6512 0.2356 0.069 Uiso 1 1 calc R . .
H6B H -0.4045 0.5507 0.1796 0.069 Uiso 1 1 calc R . .
H6C H -0.4190 0.6768 0.1505 0.069 Uiso 1 1 calc R . .
C7 C -0.1116(2) 0.7639(2) -0.07289(12) 0.0218(5) Uani 1 1 d . . .
H7A H -0.0716 0.7440 -0.1090 0.026 Uiso 1 1 calc R . .
H7B H -0.1888 0.7429 -0.0950 0.026 Uiso 1 1 calc R . .
C8 C -0.1058(2) 0.8907(2) -0.06225(13) 0.0240(6) Uani 1 1 d . . .
H8A H -0.1230 0.9099 -0.0157 0.029 Uiso 1 1 calc R . .
H8B H -0.0307 0.9165 -0.0579 0.029 Uiso 1 1 calc R . .
C9 C -0.1850(2) 0.9502(2) -0.12662(14) 0.0290(6) Uani 1 1 d . . .
H9A H -0.1691 1.0312 -0.1226 0.035 Uiso 1 1 calc R . .
H9B H -0.1731 0.9235 -0.1734 0.035 Uiso 1 1 calc R . .
C10 C -0.3290(3) 0.9995(3) -0.07725(16) 0.0487(8) Uani 1 1 d . . .
H10A H -0.2911 0.9743 -0.0271 0.073 Uiso 1 1 calc R . .
H10B H -0.4078 0.9917 -0.0857 0.073 Uiso 1 1 calc R . .
H10C H -0.3113 1.0779 -0.0829 0.073 Uiso 1 1 calc R . .
C11 C 0.25788(18) 0.4760(2) 0.13728(12) 0.0193(5) Uani 1 1 d . . .
H11A H 0.2147 0.4372 0.1659 0.023 Uiso 1 1 calc R . .
H11B H 0.2880 0.4182 0.1110 0.023 Uiso 1 1 calc R . .
C12 C 0.35276(19) 0.5356(2) 0.19168(13) 0.0229(6) Uani 1 1 d . . .
H12A H 0.3919 0.5814 0.1637 0.028 Uiso 1 1 calc R . .
H12B H 0.3239 0.5865 0.2230 0.028 Uiso 1 1 calc R . .
C13 C 0.4316(2) 0.4553(2) 0.24052(14) 0.0292(6) Uani 1 1 d . . .
H13A H 0.4908 0.4970 0.2758 0.035 Uiso 1 1 calc R . .
H13B H 0.3936 0.4093 0.2691 0.035 Uiso 1 1 calc R . .
C14 C 0.5599(3) 0.3166(3) 0.23667(19) 0.0573(10) Uani 1 1 d . . .
H14A H 0.6226 0.3626 0.2622 0.086 Uiso 1 1 calc R . .
H14B H 0.5814 0.2642 0.2034 0.086 Uiso 1 1 calc R . .
H14C H 0.5342 0.2749 0.2732 0.086 Uiso 1 1 calc R . .
C15 C 0.25507(19) 0.6331(2) 0.02011(13) 0.0215(5) Uani 1 1 d . . .
H15A H 0.2082 0.6776 -0.0210 0.026 Uiso 1 1 calc R . .
H15B H 0.3019 0.6864 0.0552 0.026 Uiso 1 1 calc R . .
C16 C 0.3289(2) 0.5617(2) -0.01185(14) 0.0287(6) Uani 1 1 d . . .
H16A H 0.3756 0.5144 0.0277 0.034 Uiso 1 1 calc R . .
H16B H 0.2840 0.5120 -0.0506 0.034 Uiso 1 1 calc R . .
C17 C 0.3999(2) 0.6345(3) -0.04484(15) 0.0373(7) Uani 1 1 d . . .
H17A H 0.4440 0.5874 -0.0685 0.045 Uiso 1 1 calc R . .
H17B H 0.3537 0.6841 -0.0831 0.045 Uiso 1 1 calc R . .
C18 C 0.5238(3) 0.7825(3) -0.0162(2) 0.0711(12) Uani 1 1 d . . .
H18A H 0.5710 0.7476 -0.0427 0.107 Uiso 1 1 calc R . .
H18B H 0.5681 0.8273 0.0248 0.107 Uiso 1 1 calc R . .
H18C H 0.4705 0.8306 -0.0502 0.107 Uiso 1 1 calc R . .
C19 C -0.05876(19) 0.4344(2) 0.14032(13) 0.0211(5) Uani 1 1 d . . .
C20 C -0.0956(2) 0.4041(2) 0.20439(13) 0.0284(6) Uani 1 1 d . . .
H20A H -0.1672 0.4375 0.1995 0.043 Uiso 1 1 calc R . .
H20B H -0.0433 0.4317 0.2496 0.043 Uiso 1 1 calc R . .
H20C H -0.1011 0.3227 0.2070 0.043 Uiso 1 1 calc R . .
P3 P 0.16195(6) 0.56959(6) 0.34625(4) 0.02855(17) Uani 1 1 d . . .
F1 F 0.09587(16) 0.47770(13) 0.37750(9) 0.0497(5) Uani 1 1 d . . .
F2 F 0.17135(15) 0.64369(15) 0.41748(9) 0.0553(5) Uani 1 1 d . . .
F3 F 0.22646(14) 0.66207(14) 0.31452(9) 0.0470(4) Uani 1 1 d . . .
F4 F 0.15011(14) 0.49531(15) 0.27428(8) 0.0478(5) Uani 1 1 d . . .
F5 F 0.04975(13) 0.62987(15) 0.30592(10) 0.0509(5) Uani 1 1 d . . .
F6 F 0.27323(15) 0.50849(17) 0.38570(10) 0.0616(6) 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'
F F 0.0171 0.0103 '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
_geom_angle_publ_flag
N1 Fe1 N1 180.0 . 3_565 ?
N1 Fe1 P2 90.38(6) . 3_565 ?
N1 Fe1 P2 89.62(6) 3_565 3_565 ?
N1 Fe1 P2 89.62(6) . . ?
N1 Fe1 P2 90.38(6) 3_565 . ?
P2 Fe1 P2 180.0 3_565 . ?
N1 Fe1 P1 89.76(6) . 3_565 ?
N1 Fe1 P1 90.24(6) 3_565 3_565 ?
P2 Fe1 P1 84.26(2) 3_565 3_565 ?
P2 Fe1 P1 95.74(2) . 3_565 ?
N1 Fe1 P1 90.24(6) . . ?
N1 Fe1 P1 89.76(6) 3_565 . ?
P2 Fe1 P1 95.74(2) 3_565 . ?
P2 Fe1 P1 84.26(2) . . ?
P1 Fe1 P1 180.0 3_565 . ?
C7 P1 C3 100.95(11) . . ?
C7 P1 C2 103.40(11) . . ?
C3 P1 C2 103.10(11) . . ?
C7 P1 Fe1 119.43(8) . . ?
C3 P1 Fe1 119.20(8) . . ?
C2 P1 Fe1 108.60(8) . . ?
C11 P2 C15 104.21(11) . . ?
C11 P2 C1 105.19(11) . . ?
C15 P2 C1 99.10(11) . . ?
C11 P2 Fe1 120.67(8) . . ?
C15 P2 Fe1 118.86(8) . . ?
C1 P2 Fe1 105.91(8) . . ?
C19 N1 Fe1 176.00(19) . . ?
C5 O1 C6 112.0(2) . . ?
C9 O2 C10 112.9(2) . . ?
C14 O3 C13 112.5(2) . . ?
C17 O4 C18 112.1(2) . . ?
C2 C1 P2 106.95(15) . . ?
C1 C2 P1 109.12(16) . . ?
C4 C3 P1 117.33(17) . . ?
C5 C4 C3 111.8(2) . . ?
O1 C5 C4 108.0(2) . . ?
C8 C7 P1 116.15(16) . . ?
C9 C8 C7 111.3(2) . . ?
O2 C9 C8 113.5(2) . . ?
C12 C11 P2 115.74(16) . . ?
C13 C12 C11 112.3(2) . . ?
O3 C13 C12 108.49(19) . . ?
C16 C15 P2 119.19(18) . . ?
C17 C16 C15 110.6(2) . . ?
O4 C17 C16 108.9(2) . . ?
N1 C19 C20 178.0(3) . . ?
F2 P3 F6 91.11(10) . . ?
F2 P3 F4 178.94(11) . . ?
F6 P3 F4 89.83(10) . . ?
F2 P3 F5 89.51(10) . . ?
F6 P3 F5 179.35(11) . . ?
F4 P3 F5 89.55(10) . . ?
F2 P3 F3 90.30(10) . . ?
F6 P3 F3 90.28(11) . . ?
F4 P3 F3 90.20(9) . . ?
F5 P3 F3 89.92(10) . . ?
F2 P3 F1 89.70(10) . . ?
F6 P3 F1 90.46(11) . . ?
F4 P3 F1 89.79(9) . . ?
F5 P3 F1 89.34(10) . . ?
F3 P3 F1 179.26(11) . . ?
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 N1 1.9188(19) . ?
Fe1 N1 1.9189(19) 3_565 ?
Fe1 P2 2.2839(6) 3_565 ?
Fe1 P2 2.2839(6) . ?
Fe1 P1 2.3013(6) 3_565 ?
Fe1 P1 2.3013(6) . ?
P1 C7 1.836(2) . ?
P1 C3 1.838(2) . ?
P1 C2 1.841(2) . ?
P2 C11 1.830(2) . ?
P2 C15 1.838(2) . ?
P2 C1 1.842(2) . ?
N1 C19 1.133(3) . ?
O1 C5 1.413(3) . ?
O1 C6 1.418(3) . ?
O2 C9 1.414(3) . ?
O2 C10 1.423(3) . ?
O3 C14 1.411(3) . ?
O3 C13 1.418(3) . ?
O4 C17 1.404(3) . ?
O4 C18 1.412(4) . ?
C1 C2 1.524(3) . ?
C3 C4 1.531(3) . ?
C4 C5 1.510(3) . ?
C7 C8 1.532(3) . ?
C8 C9 1.520(3) . ?
C11 C12 1.527(3) . ?
C12 C13 1.504(3) . ?
C15 C16 1.521(3) . ?
C16 C17 1.515(3) . ?
C19 C20 1.461(3) . ?
P3 F2 1.5854(16) . ?
P3 F6 1.5866(18) . ?
P3 F4 1.5932(16) . ?
P3 F5 1.5948(18) . ?
P3 F3 1.5962(17) . ?
P3 F1 1.5993(17) . ?
