#------------------------------------------------------------------------------
#$Date: 2016-03-21 09:30:05 +0200 (Mon, 21 Mar 2016) $
#$Revision: 178624 $
#$URL: svn://www.crystallography.net/cod/cif/4/07/35/4073528.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_4073528
loop_
_publ_author_name
'Balakrishna, Maravanji S.'
'Mague, Joel T.'
_publ_section_title
;
 Synthesis and Molecular Structure of
 1,3-Di-tert-butyl-2,4-bis(cyclodipentadienyl)iron(II)
 1,3,2,4-Diazadiphosphetidine, [Fe(η5-C5H4)2(PNtBu)2]
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4677
_journal_paper_doi               10.1021/om700423h
_journal_volume                  26
_journal_year                    2007
_chemical_formula_sum            'C18 H26 Fe N2 P2'
_chemical_formula_weight         388.20
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           43
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'F 2 -2d'
_symmetry_space_group_name_H-M   'F d d 2'
_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                   15.543(1)
_cell_length_b                   23.253(2)
_cell_length_c                   9.9437(7)
_cell_measurement_reflns_used    6830
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.29
_cell_measurement_theta_min      2.58
_cell_volume                     3593.9(5)
_computing_cell_refinement       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_collection       'Bruker SMART (Bruker-AXS, 2000)'
_computing_data_reduction        'Bruker SAINT+ (Bruker-AXS, 2004)'
_computing_molecular_graphics    'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_publication_material  'Bruker SHELXTL (Bruker-AXS, 2000a)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker-AXS Smart APEX 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  0.0270
_diffrn_reflns_av_sigmaI/netI    0.0185
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15478
_diffrn_reflns_theta_full        28.29
_diffrn_reflns_theta_max         28.29
_diffrn_reflns_theta_min         2.58
_exptl_absorpt_coefficient_mu    1.018
_exptl_absorpt_correction_T_max  0.9024
_exptl_absorpt_correction_T_min  0.8480
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 2002)'
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             1632
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.380
_refine_diff_density_min         -0.215
_refine_diff_density_rms         0.055
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.194(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.089
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     109
_refine_ls_number_reflns         2242
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.089
_refine_ls_R_factor_all          0.0209
_refine_ls_R_factor_gt           0.0208
_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)+(0.0329P)²+2.3064P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0531
_refine_ls_wR_factor_ref         0.0532
_reflns_number_gt                2233
_reflns_number_total             2242
_reflns_threshold_expression     >2σ(I)
_cod_data_source_file            om700423h-file001.cif
_cod_data_source_block           msb301
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' 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_values 1715 2011-07-08 13:25:40Z adriana 
;
_cod_original_cell_volume        3593.9(4)
_cod_original_sg_symbol_H-M      Fdd2
_cod_database_code               4073528
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'x+1/4, -y+1/4, z+1/4'
'-x+1/4, y+1/4, z+1/4'
'x, y+1/2, z+1/2'
'-x, -y+1/2, z+1/2'
'x+1/4, -y+3/4, z+3/4'
'-x+1/4, y+3/4, z+3/4'
'x+1/2, y, z+1/2'
'-x+1/2, -y, z+1/2'
'x+3/4, -y+1/4, z+3/4'
'-x+3/4, y+1/4, z+3/4'
'x+1/2, y+1/2, z'
'-x+1/2, -y+1/2, z'
'x+3/4, -y+3/4, z+1/4'
'-x+3/4, y+3/4, z+1/4'
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
Fe Fe 0.2500 0.7500 1.21718(2) 0.01164(7) Uani 1 2 d S
P P 0.26568(2) 0.803703(16) 0.90602(3) 0.01236(8) Uani 1 1 d .
N N 0.17530(8) 0.75961(5) 0.89805(14) 0.0134(2) Uani 1 1 d .
C1 C 0.10284(10) 0.77100(6) 0.80503(14) 0.0165(3) Uani 1 1 d .
C2 C 0.03841(11) 0.72188(7) 0.81856(18) 0.0249(4) Uani 1 1 d .
H2A H 0.0649 0.6860 0.7874 0.037 Uiso 1 1 calc R
H2B H -0.0126 0.7303 0.7640 0.037 Uiso 1 1 calc R
H2C H 0.0215 0.7178 0.9130 0.037 Uiso 1 1 calc R
C3 C 0.06160(11) 0.82751(7) 0.8504(2) 0.0259(3) Uani 1 1 d .
H3A H 0.0405 0.8234 0.9428 0.039 Uiso 1 1 calc R
H3B H 0.0134 0.8369 0.7907 0.039 Uiso 1 1 calc R
H3C H 0.1045 0.8584 0.8468 0.039 Uiso 1 1 calc R
C4 C 0.13246(11) 0.77614(8) 0.65923(18) 0.0291(4) Uani 1 1 d .
H4A H 0.1758 0.8066 0.6520 0.044 Uiso 1 1 calc R
H4B H 0.0831 0.7856 0.6020 0.044 Uiso 1 1 calc R
H4C H 0.1575 0.7395 0.6300 0.044 Uiso 1 1 calc R
C5 C 0.26809(9) 0.81560(6) 1.08710(15) 0.0118(3) Uani 1 1 d .
C6 C 0.34165(9) 0.80926(6) 1.17264(15) 0.0148(3) Uani 1 1 d .
H6 H 0.3988 0.8005 1.1487 0.018 Uiso 1 1 d R
C7 C 0.31468(10) 0.81645(6) 1.30846(16) 0.0180(3) Uani 1 1 d .
H7 H 0.3471 0.8148 1.3857 0.022 Uiso 1 1 d R
C8 C 0.22486(11) 0.82757(6) 1.30836(15) 0.0177(3) Uani 1 1 d .
H8 H 0.1896 0.8317 1.3863 0.021 Uiso 1 1 d R
C9 C 0.19583(10) 0.82715(6) 1.17255(15) 0.0152(3) Uani 1 1 d .
H9 H 0.1393 0.8321 1.1507 0.018 Uiso 1 1 d 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'
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
C5 Fe C5 100.35(8) . 14_565
C5 Fe C6 41.43(6) . .
C5 Fe C6 118.06(6) 14_565 .
C5 Fe C6 118.06(6) . 14_565
C5 Fe C6 41.43(6) 14_565 14_565
C6 Fe C6 154.80(8) . 14_565
C5 Fe C9 41.46(6) . .
C5 Fe C9 118.01(6) 14_565 .
C6 Fe C9 69.13(6) . .
C6 Fe C9 105.12(6) 14_565 .
C5 Fe C9 118.01(6) . 14_565
C5 Fe C9 41.46(6) 14_565 14_565
C6 Fe C9 105.13(6) . 14_565
C6 Fe C9 69.13(6) 14_565 14_565
C9 Fe C9 154.76(8) . 14_565
C5 Fe C7 69.32(6) . .
C5 Fe C7 156.78(6) 14_565 .
C6 Fe C7 40.79(6) . .
C6 Fe C7 161.77(6) 14_565 .
C9 Fe C7 68.60(6) . .
C9 Fe C7 123.92(6) 14_565 .
C5 Fe C7 156.78(6) . 14_565
C5 Fe C7 69.32(6) 14_565 14_565
C6 Fe C7 161.77(6) . 14_565
C6 Fe C7 40.79(6) 14_565 14_565
C9 Fe C7 123.91(6) . 14_565
C9 Fe C7 68.59(6) 14_565 14_565
C7 Fe C7 127.57(9) . 14_565
C5 Fe C8 156.70(6) . 14_565
C5 Fe C8 69.29(6) 14_565 14_565
C6 Fe C8 123.92(6) . 14_565
C6 Fe C8 68.55(6) 14_565 14_565
C9 Fe C8 161.81(6) . 14_565
C9 Fe C8 40.77(6) 14_565 14_565
C7 Fe C8 111.83(6) . 14_565
C7 Fe C8 40.41(6) 14_565 14_565
C5 Fe C8 69.29(6) . .
C5 Fe C8 156.70(6) 14_565 .
C6 Fe C8 68.55(6) . .
C6 Fe C8 123.92(6) 14_565 .
C9 Fe C8 40.77(6) . .
C9 Fe C8 161.81(6) 14_565 .
C7 Fe C8 40.41(6) . .
C7 Fe C8 111.83(6) 14_565 .
C8 Fe C8 127.67(9) 14_565 .
N P N 85.70(6) 14_565 .
N P C5 99.38(6) 14_565 .
N P C5 98.69(7) . .
N P P 43.04(4) 14_565 14_565
N P P 42.90(4) . 14_565
C5 P P 98.80(4) . 14_565
C1 N P 125.58(10) . 14_565
C1 N P 122.45(10) . .
P N P 94.07(6) 14_565 .
N C1 C2 108.07(12) . .
N C1 C4 112.20(13) . .
C2 C1 C4 109.91(13) . .
N C1 C3 106.75(12) . .
C2 C1 C3 110.01(14) . .
C4 C1 C3 109.84(14) . .
C6 C5 C9 107.01(13) . .
C6 C5 P 125.98(11) . .
C9 C5 P 126.73(11) . .
C6 C5 Fe 69.70(8) . .
C9 C5 Fe 69.69(8) . .
P C5 Fe 121.02(7) . .
C7 C6 C5 108.43(13) . .
C7 C6 Fe 70.51(9) . .
C5 C6 Fe 68.88(8) . .
C8 C7 C6 108.07(13) . .
C8 C7 Fe 69.85(8) . .
C6 C7 Fe 68.70(8) . .
C7 C8 C9 108.12(13) . .
C7 C8 Fe 69.74(8) . .
C9 C8 Fe 68.66(8) . .
C8 C9 C5 108.37(13) . .
C8 C9 Fe 70.57(8) . .
C5 C9 Fe 68.86(8) . .
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
Fe C5 2.0198(14) .
Fe C5 2.0198(14) 14_565
Fe C6 2.0308(14) .
Fe C6 2.0308(14) 14_565
Fe C9 2.0309(14) .
Fe C9 2.0309(14) 14_565
Fe C7 2.0547(15) .
Fe C7 2.0548(15) 14_565
Fe C8 2.0562(14) 14_565
Fe C8 2.0562(14) .
P N 1.7364(12) 14_565
P N 1.7410(12) .
P C5 1.8221(15) .
P P 2.5446(7) 14_565
N C1 1.4812(18) .
N P 1.7364(12) 14_565
C1 C2 1.525(2) .
C1 C4 1.526(2) .
C1 C3 1.530(2) .
C5 C6 1.4326(19) .
C5 C9 1.4338(19) .
C6 C7 1.424(2) .
C7 C8 1.420(2) .
C8 C9 1.424(2) .
