#------------------------------------------------------------------------------
#$Date: 2015-10-06 08:33:04 +0300 (Tue, 06 Oct 2015) $
#$Revision: 160442 $
#$URL: svn://www.crystallography.net/cod/cif/4/08/63/4086302.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_4086302
loop_
_publ_author_name
'Billow, Brennan S.'
'Bemowski, Ross D.'
'DiFranco, Stephen A.'
'Staples, Richard J.'
'Odom, Aaron L.'
_publ_section_title
;
 Synthesis and Structure of Chromium(VI) Nitrido Cyclopentadienyl
 Complexes
;
_journal_issue                   18
_journal_name_full               Organometallics
_journal_page_first              4567
_journal_paper_doi               10.1021/acs.organomet.5b00661
_journal_volume                  34
_journal_year                    2015
_chemical_formula_moiety         'C12 H10 Fe O2'
_chemical_formula_sum            'C12 H10 Fe O2'
_chemical_formula_weight         242.05
_chemical_name_systematic
;
 ?
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2015-06-30
_audit_creation_method
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_cell_angle_alpha                90
_cell_angle_beta                 98.154(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.5220(16)
_cell_length_b                   7.4596(9)
_cell_length_c                   11.2323(14)
_cell_measurement_reflns_used    4059
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      25.37
_cell_measurement_theta_min      3.19
_cell_volume                     1038.6(2)
_computing_cell_refinement       'SAINT v8.27A (Bruker, 2012)'
_computing_data_reduction        'SAINT v8.27A (Bruker, 2012)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_diffrn_ambient_temperature      173(2)
_diffrn_detector_area_resol_mean 836.6
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0345
_diffrn_reflns_av_unetI/netI     0.0291
_diffrn_reflns_laue_measured_fraction_full 0.998
_diffrn_reflns_laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            8231
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.391
_diffrn_reflns_theta_min         3.187
_diffrn_source                   'sealed tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.425
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6322
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0602 before and 0.0440 after correction. The Ratio of minimum to maximum transmission is 0.8484. The λ/2 correction factor is 0.0015.'
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.548
_exptl_crystal_description       plate
_exptl_crystal_F_000             496
_exptl_crystal_recrystallization_method 'used as received'
_exptl_crystal_size_max          0.262
_exptl_crystal_size_mid          0.193
_exptl_crystal_size_min          0.046
_refine_diff_density_max         0.292
_refine_diff_density_min         -0.267
_refine_diff_density_rms         0.057
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.037
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     140
_refine_ls_number_reflns         1900
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.037
_refine_ls_R_factor_all          0.0375
_refine_ls_R_factor_gt           0.0271
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0319P)²+0.3677P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0627
_refine_ls_wR_factor_ref         0.0686
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1534
_reflns_number_total             1900
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            om5b00661_si_002.cif
_cod_data_source_block           fecpco173
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'Multi-scan' changed to
'multi-scan' according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 3271 2015-04-21 07:52:19Z andrius 
;
_cod_database_code               4086302
_shelxl_version_number           2013-3
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.937
_shelx_estimated_absorpt_t_min   0.707
_olex2_refinement_description
;
1. Others
 Fixed Uiso: H2(0.033) H3(0.039) H4(0.044) H5(0.039) H6(0.043) H7(0.037)
 H8(0.04) H9(0.046) H10(0.047)
 Fixed X: H2(0.8155) H3(0.9949) H4(0.9817) H5(0.7934) H6(0.813001) H7(0.9042)
 H8(0.7927) H9(0.6324) H10(0.6441)
 Fixed Y: H2(0.609) H3(0.653201) H4(0.8777) H5(0.972799) H6(0.9615) H7(1.0399)
 H8(1.276499) H9(1.348201) H10(1.153301)
 Fixed Z: H2(0.9598) H3(0.902699) H4(0.73) H5(0.6795) H6(1.1497) H7(0.9697)
 H8(0.8491) H9(0.9561) H10(1.1407)
;
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method 'mounted on nylon loop with paratone oil'
_olex2_submission_original_sample_id 'Fe(CP)2(CO)2 173 10s'
_olex2_submission_special_instructions 'No special instructions were received'
loop_
_space_group_symop_operation_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_site_symmetry_order
_atom_site_calc_flag
Fe1 Fe 0.68316(2) 0.99210(4) 0.93048(2) 0.02183(12) Uani 1 1 d
O1 O 0.57932(13) 0.6914(2) 1.03320(14) 0.0368(4) Uani 1 1 d
O2 O 0.50691(14) 1.0580(3) 0.73707(15) 0.0441(4) Uani 1 1 d
C1 C 0.75450(18) 0.8032(3) 0.82340(19) 0.0256(5) Uani 1 1 d
H1 H 0.6936(18) 0.745(3) 0.7880(19) 0.030(6) Uiso 1 1 d
C2 C 0.83233(18) 0.6876(3) 0.89854(19) 0.0274(5) Uani 1 1 d
H2 H 0.8155 0.6090 0.9598 0.033 Uiso 1 1 d
C3 C 0.93075(18) 0.7109(3) 0.8667(2) 0.0326(5) Uani 1 1 d
H3 H 0.9949 0.6532 0.9027 0.039 Uiso 1 1 d
C4 C 0.92338(19) 0.8381(3) 0.7688(2) 0.0370(6) Uani 1 1 d
H4 H 0.9817 0.8777 0.7300 0.044 Uiso 1 1 d
C5 C 0.8199(2) 0.8913(3) 0.74167(19) 0.0326(5) Uani 1 1 d
H5 H 0.7934 0.9728 0.6795 0.039 Uiso 1 1 d
C6 C 0.7885(2) 1.0472(3) 1.0895(2) 0.0360(6) Uani 1 1 d
H6 H 0.8130 0.9615 1.1497 0.043 Uiso 1 1 d
C7 C 0.83931(17) 1.0911(3) 0.9889(2) 0.0309(5) Uani 1 1 d
H7 H 0.9042 1.0399 0.9697 0.037 Uiso 1 1 d
C8 C 0.77722(19) 1.2233(3) 0.9216(2) 0.0330(5) Uani 1 1 d
H8 H 0.7927 1.2765 0.8491 0.040 Uiso 1 1 d
C9 C 0.68742(19) 1.2631(3) 0.9814(2) 0.0385(6) Uani 1 1 d
H9 H 0.6324 1.3482 0.9561 0.046 Uiso 1 1 d
C10 C 0.6939(2) 1.1548(3) 1.0844(2) 0.0391(6) Uani 1 1 d
H10 H 0.6441 1.1533 1.1407 0.047 Uiso 1 1 d
C11 C 0.61931(17) 0.8101(3) 0.99174(18) 0.0262(5) Uani 1 1 d
C12 C 0.57753(19) 1.0295(3) 0.8117(2) 0.0289(5) 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 0.0030 0.0020 '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'
Fe Fe 0.3460 0.8440 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0110 0.0060 '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
C6 Fe1 C1 110.24(10)
C6 Fe1 C7 39.18(9)
C7 Fe1 C1 87.85(9)
C8 Fe1 C1 103.52(9)
C8 Fe1 C6 65.88(9)
C8 Fe1 C7 39.11(9)
C8 Fe1 C9 39.56(9)
C8 Fe1 C10 66.01(9)
C9 Fe1 C1 142.61(9)
C9 Fe1 C6 65.92(10)
C9 Fe1 C7 65.86(9)
C9 Fe1 C10 39.04(10)
C10 Fe1 C1 149.77(10)
C10 Fe1 C6 39.61(10)
C10 Fe1 C7 65.99(9)
C11 Fe1 C1 87.74(9)
C11 Fe1 C6 94.79(9)
C11 Fe1 C7 126.90(10)
C11 Fe1 C8 159.94(10)
C11 Fe1 C9 129.06(10)
C11 Fe1 C10 95.93(10)
C12 Fe1 C1 90.40(9)
C12 Fe1 C6 157.52(10)
C12 Fe1 C7 138.09(10)
C12 Fe1 C8 101.54(10)
C12 Fe1 C9 92.37(10)
C12 Fe1 C10 119.01(10)
C12 Fe1 C11 94.83(10)
Fe1 C1 H1 99.7(13)
C2 C1 Fe1 111.10(14)
C2 C1 H1 114.4(14)
C5 C1 Fe1 111.87(15)
C5 C1 H1 116.3(13)
C5 C1 C2 103.73(18)
C1 C2 H2 125.4(2)
C3 C2 C1 109.20(19)
C3 C2 H2 125.4(2)
C2 C3 H3 125.5(2)
C2 C3 C4 109.0(2)
C4 C3 H3 125.5(2)
C3 C4 H4 125.7(2)
C5 C4 C3 108.7(2)
C5 C4 H4 125.6(3)
C1 C5 H5 125.3(2)
C4 C5 C1 109.3(2)
C4 C5 H5 125.4(2)
Fe1 C6 H6 124.96(18)
C7 C6 Fe1 70.45(13)
C7 C6 H6 126.1(3)
C7 C6 C10 107.7(2)
C10 C6 Fe1 70.03(13)
C10 C6 H6 126.2(3)
Fe1 C7 H7 125.11(17)
C6 C7 Fe1 70.37(13)
C6 C7 H7 125.9(2)
C8 C7 Fe1 70.16(13)
C8 C7 C6 108.3(2)
C8 C7 H7 125.8(2)
Fe1 C8 H8 124.61(18)
C7 C8 Fe1 70.72(13)
C7 C8 H8 126.0(2)
C7 C8 C9 107.9(2)
C9 C8 Fe1 70.27(13)
C9 C8 H8 126.1(2)
Fe1 C9 H9 124.91(19)
C8 C9 Fe1 70.18(13)
C8 C9 H9 126.0(3)
C10 C9 Fe1 70.51(13)
C10 C9 C8 108.2(2)
C10 C9 H9 125.9(3)
Fe1 C10 H10 124.78(18)
C6 C10 Fe1 70.36(13)
C6 C10 H10 126.0(3)
C9 C10 Fe1 70.45(13)
C9 C10 C6 107.9(2)
C9 C10 H10 126.1(3)
O1 C11 Fe1 178.8(2)
O2 C12 Fe1 177.4(2)
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
Fe1 C1 2.130(2)
Fe1 C6 2.105(2)
Fe1 C7 2.106(2)
Fe1 C8 2.099(2)
Fe1 C9 2.100(2)
Fe1 C10 2.101(2)
Fe1 C11 1.764(2)
Fe1 C12 1.763(3)
O1 C11 1.148(3)
O2 C12 1.149(3)
C1 H1 0.92(2)
C1 C2 1.474(3)
C1 C5 1.470(3)
C2 H2 0.950(2)
C2 C3 1.342(3)
C3 H3 0.950(2)
C3 C4 1.445(3)
C4 H4 0.949(2)
C4 C5 1.348(3)
C5 H5 0.950(2)
C6 H6 0.950(2)
C6 C7 1.412(3)
C6 C10 1.425(4)
C7 H7 0.950(2)
C7 C8 1.407(3)
C8 H8 0.951(2)
C8 C9 1.421(3)
C9 H9 0.950(2)
C9 C10 1.404(4)
C10 H10 0.949(2)
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
Fe1 C1 C2 C3 -118.52(17)
Fe1 C1 C5 C4 117.97(19)
Fe1 C6 C7 C8 60.16(16)
Fe1 C6 C10 C9 -60.72(16)
Fe1 C7 C8 C9 60.74(16)
Fe1 C8 C9 C10 60.55(16)
Fe1 C9 C10 C6 60.66(16)
C1 C2 C3 C4 -1.2(3)
C2 C1 C5 C4 -1.9(2)
C2 C3 C4 C5 0.0(3)
C3 C4 C5 C1 1.2(3)
C5 C1 C2 C3 1.8(2)
C6 C7 C8 Fe1 -60.29(16)
C6 C7 C8 C9 0.5(3)
C7 C6 C10 Fe1 60.68(16)
C7 C6 C10 C9 0.0(3)
C7 C8 C9 Fe1 -61.04(16)
C7 C8 C9 C10 -0.5(3)
C8 C9 C10 Fe1 -60.34(16)
C8 C9 C10 C6 0.3(3)
C10 C6 C7 Fe1 -60.42(16)
C10 C6 C7 C8 -0.3(3)
