#------------------------------------------------------------------------------
#$Date: 2019-11-08 00:28:22 +0200 (Fri, 08 Nov 2019) $
#$Revision: 224266 $
#$URL: file:///home/coder/svn-repositories/cod/cif/7/04/91/7049180.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_7049180
loop_
_publ_author_name
'Binding, Samantha C.'
'Green, Jennifer C.'
'Turner, Zoë R'
'Buffet, Jean-Charles'
'O'Hare, Dermot'
_publ_section_title
;
 Synthesis, characterisation and redox properties of anti-bimetallic
 permethylpentalene complexes.
;
_journal_issue                   13
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4263
_journal_page_last               4273
_journal_paper_doi               10.1039/c8dt05054f
_journal_volume                  48
_journal_year                    2019
_chemical_formula_moiety         'C34 H48 Fe2'
_chemical_formula_sum            'C34 H48 Fe2'
_chemical_formula_weight         568.45
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_audit_creation_date             2018-12-20
_audit_creation_method           CRYSTALS_ver_14.43
_audit_update_record
;
2018-12-20 deposited with the CCDC.    2019-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 109.768(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   9.1531(3)
_cell_length_b                   15.1021(4)
_cell_length_c                   11.1714(3)
_cell_measurement_reflns_used    3001
_cell_measurement_temperature    150
_cell_measurement_theta_max      27
_cell_measurement_theta_min      5
_cell_volume                     1453.23(8)
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_diffrn_ambient_temperature      150
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_device       Area
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_method       ω/2θ
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_reflns_av_R_equivalents  0.044
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            7782
_diffrn_reflns_theta_full        74.001
_diffrn_reflns_theta_max         76.290
_diffrn_reflns_theta_min         5.126
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    8.132
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            black
_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       rod
_exptl_crystal_F_000             608
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_min          0.080
_refine_diff_density_max         0.75
_refine_diff_density_min         -0.45
_refine_ls_extinction_method     None
_refine_ls_goodness_of_fit_ref   0.9784
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     163
_refine_ls_number_reflns         3001
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0617
_refine_ls_R_factor_gt           0.0442
_refine_ls_shift/su_max          0.0004947
_refine_ls_shift/su_mean         0.0000169
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 0.41P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1173
_refine_ls_wR_factor_gt          0.1067
_refine_ls_wR_factor_ref         0.1173
_reflns_limit_h_max              10
_reflns_limit_h_min              -11
_reflns_limit_k_max              18
_reflns_limit_k_min              0
_reflns_limit_l_max              14
_reflns_limit_l_min              0
_reflns_number_gt                2281
_reflns_number_total             3013
_reflns_threshold_expression     I>2.0σ(I)
_oxford_diffrn_Wilson_B_factor   2.87
_oxford_diffrn_Wilson_scale      0.02
_oxford_refine_ls_r_factor_ref   0.0617
_oxford_refine_ls_scale          5.67(15)
_oxford_reflns_number_all        3001
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_oxford_structure_analysis_title '048scb14 in P2(1)/n'
_cod_data_source_file            c8dt05054f2.cif
_cod_data_source_block           1-048scb14
_cod_depositor_comments
'Adding full bibliography for 7049180--7049184.cif.'
_cod_original_cell_volume        1453.23(7)
_cod_original_sg_symbol_H-M      'P 1 21/n 1 '
_cod_database_code               7049180
_iucr_refine_instructions_details_constraints
;
#
# Punched on 20/12/18 at 10:19:18
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   5,X'S) H   (  53,X'S) H   (  52,X'S) H   (  51,X'S) 
RIDE C   (   6,X'S) H   (  63,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (  13,X'S) H   ( 133,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  15,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 173,X'S) H   ( 172,X'S) H   ( 171,X'S) 
END                                                                             
;
_iucr_refine_instructions_details_restraints
;
#
# Punched on 20/12/18 at 10:19:18
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
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_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
C1 C 0.5411(3) 0.45461(18) 0.3655(3) 0.0319 1.0000 Uani .
C2 C 0.6780(3) 0.50840(19) 0.4091(3) 0.0336 1.0000 Uani .
C3 C 0.6745(3) 0.56173(18) 0.5156(3) 0.0318 1.0000 Uani .
C4 C 0.4585(3) 0.46702(17) 0.4536(2) 0.0288 1.0000 Uani .
C5 C 0.5029(4) 0.3885(2) 0.2591(3) 0.0438 1.0000 Uani .
C6 C 0.8052(4) 0.5083(2) 0.3534(3) 0.0460 1.0000 Uani .
C7 C 0.7971(3) 0.6243(2) 0.5917(3) 0.0413 1.0000 Uani .
C8 C 0.3173(4) 0.6137(2) 0.1832(3) 0.0447 1.0000 Uani .
C9 C 0.4589(4) 0.6517(2) 0.1847(3) 0.0462 1.0000 Uani .
C10 C 0.5098(3) 0.7113(2) 0.2879(3) 0.0407 1.0000 Uani .
C11 C 0.3966(3) 0.71188(19) 0.3512(3) 0.0372 1.0000 Uani .
C12 C 0.2768(3) 0.6516(2) 0.2850(3) 0.0409 1.0000 Uani .
C13 C 0.2219(5) 0.5469(3) 0.0888(4) 0.0667 1.0000 Uani .
C14 C 0.5406(5) 0.6354(3) 0.0899(4) 0.0662 1.0000 Uani .
C15 C 0.6530(4) 0.7682(3) 0.3233(4) 0.0560 1.0000 Uani .
C16 C 0.4018(4) 0.7682(2) 0.4626(3) 0.0533 1.0000 Uani .
C17 C 0.1349(4) 0.6315(3) 0.3182(4) 0.0605 1.0000 Uani .
Fe1 Fe 0.48834(5) 0.58696(3) 0.35494(4) 0.0320 1.0000 Uani .
H53 H 0.3912 0.3792 0.2272 0.0647 1.0000 Uiso R
H52 H 0.5383 0.4095 0.1924 0.0651 1.0000 Uiso R
H51 H 0.5524 0.3331 0.2913 0.0649 1.0000 Uiso R
H63 H 0.8553 0.5649 0.3661 0.0691 1.0000 Uiso R
H62 H 0.7643 0.4953 0.2636 0.0685 1.0000 Uiso R
H61 H 0.8805 0.4642 0.3959 0.0687 1.0000 Uiso R
H73 H 0.7512 0.6744 0.6175 0.0614 1.0000 Uiso R
H72 H 0.8575 0.6445 0.5417 0.0620 1.0000 Uiso R
H71 H 0.8626 0.5946 0.6662 0.0618 1.0000 Uiso R
H133 H 0.1714 0.5082 0.1318 0.1021 1.0000 Uiso R
H132 H 0.1455 0.5769 0.0204 0.1017 1.0000 Uiso R
H131 H 0.2889 0.5129 0.0543 0.1020 1.0000 Uiso R
H143 H 0.6514 0.6398 0.1290 0.0988 1.0000 Uiso R
H142 H 0.5066 0.6776 0.0218 0.0985 1.0000 Uiso R
H141 H 0.5136 0.5775 0.0540 0.0992 1.0000 Uiso R
H153 H 0.6882 0.7808 0.4134 0.0839 1.0000 Uiso R
H152 H 0.6310 0.8230 0.2767 0.0842 1.0000 Uiso R
H151 H 0.7347 0.7382 0.3035 0.0840 1.0000 Uiso R
H163 H 0.3360 0.7435 0.5061 0.0803 1.0000 Uiso R
H162 H 0.3673 0.8273 0.4338 0.0796 1.0000 Uiso R
H161 H 0.5068 0.7711 0.5200 0.0799 1.0000 Uiso R
H173 H 0.1581 0.6341 0.4099 0.0891 1.0000 Uiso R
H172 H 0.0538 0.6738 0.2800 0.0889 1.0000 Uiso R
H171 H 0.0954 0.5737 0.2867 0.0893 1.0000 Uiso R
loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0181 0.0091 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe -1.1336 3.1974 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 C4 . 107.1(2) yes
C2 . C1 C5 . 126.1(3) yes
C4 . C1 C5 . 126.3(3) yes
C2 . C1 Fe1 . 68.22(16) yes
C4 . C1 Fe1 . 75.22(16) yes
C5 . C1 Fe1 . 128.0(2) yes
C1 . C2 C3 . 109.5(2) yes
C1 . C2 C6 . 125.0(3) yes
C3 . C2 C6 . 125.5(3) yes
C1 . C2 Fe1 . 70.53(15) yes
C3 . C2 Fe1 . 70.29(15) yes
C6 . C2 Fe1 . 126.0(2) yes
C2 . C3 C4 2_666 106.6(2) yes
C2 . C3 C7 . 126.8(3) yes
C4 2_666 C3 C7 . 126.0(3) yes
C2 . C3 Fe1 . 68.07(15) yes
C4 2_666 C3 Fe1 . 75.28(15) yes
C7 . C3 Fe1 . 128.5(2) yes
Fe1 2_666 C4 C4 2_666 70.58(19) yes
Fe1 2_666 C4 C1 . 128.70(19) yes
C4 2_666 C4 C1 . 107.9(3) yes
Fe1 2_666 C4 C3 2_666 65.13(15) yes
C4 2_666 C4 C3 2_666 108.4(3) yes
C1 . C4 C3 2_666 143.6(3) yes
Fe1 2_666 C4 Fe1 . 141.14(13) yes
C4 2_666 C4 Fe1 . 70.6(2) yes
C1 . C4 Fe1 . 65.14(15) yes
C3 2_666 C4 Fe1 . 129.12(19) yes
C1 . C5 H53 . 108.7 no
C1 . C5 H52 . 110.2 no
H53 . C5 H52 . 110.7 no
C1 . C5 H51 . 109.2 no
H53 . C5 H51 . 108.4 no
H52 . C5 H51 . 109.7 no
C2 . C6 H63 . 109.8 no
C2 . C6 H62 . 110.5 no
H63 . C6 H62 . 109.5 no
C2 . C6 H61 . 109.0 no
H63 . C6 H61 . 108.6 no
H62 . C6 H61 . 109.5 no
C3 . C7 H73 . 110.5 no
C3 . C7 H72 . 109.9 no
H73 . C7 H72 . 108.9 no
C3 . C7 H71 . 109.1 no
H73 . C7 H71 . 108.6 no
H72 . C7 H71 . 109.9 no
C9 . C8 C12 . 108.1(3) yes
C9 . C8 C13 . 126.4(4) yes
C12 . C8 C13 . 125.4(4) yes
C9 . C8 Fe1 . 70.38(19) yes
C12 . C8 Fe1 . 70.03(17) yes
C13 . C8 Fe1 . 126.7(2) yes
C8 . C9 C10 . 108.5(3) yes
C8 . C9 C14 . 126.5(4) yes
C10 . C9 C14 . 124.9(3) yes
C8 . C9 Fe1 . 69.73(19) yes
C10 . C9 Fe1 . 69.34(18) yes
C14 . C9 Fe1 . 128.7(3) yes
C9 . C10 C11 . 108.2(3) yes
C9 . C10 C15 . 126.7(3) yes
C11 . C10 C15 . 125.1(3) yes
C9 . C10 Fe1 . 70.70(19) yes
C11 . C10 Fe1 . 69.70(17) yes
C15 . C10 Fe1 . 127.5(2) yes
C10 . C11 C12 . 107.3(3) yes
C10 . C11 C16 . 126.0(3) yes
C12 . C11 C16 . 126.7(3) yes
C10 . C11 Fe1 . 69.39(17) yes
C12 . C11 Fe1 . 70.27(17) yes
C16 . C11 Fe1 . 127.3(2) yes
C8 . C12 C11 . 107.9(3) yes
C8 . C12 C17 . 126.6(3) yes
C11 . C12 C17 . 125.5(3) yes
C8 . C12 Fe1 . 69.53(17) yes
C11 . C12 Fe1 . 69.38(16) yes
C17 . C12 Fe1 . 126.1(2) yes
C8 . C13 H133 . 108.5 no
C8 . C13 H132 . 109.6 no
H133 . C13 H132 . 109.9 no
C8 . C13 H131 . 109.6 no
H133 . C13 H131 . 110.4 no
H132 . C13 H131 . 108.8 no
C9 . C14 H143 . 111.5 no
C9 . C14 H142 . 110.1 no
H143 . C14 H142 . 108.9 no
C9 . C14 H141 . 108.8 no
H143 . C14 H141 . 109.6 no
H142 . C14 H141 . 107.8 no
C10 . C15 H153 . 109.9 no
C10 . C15 H152 . 110.2 no
H153 . C15 H152 . 109.2 no
C10 . C15 H151 . 110.2 no
H153 . C15 H151 . 108.7 no
H152 . C15 H151 . 108.5 no
C11 . C16 H163 . 110.4 no
C11 . C16 H162 . 109.6 no
H163 . C16 H162 . 109.6 no
C11 . C16 H161 . 109.0 no
H163 . C16 H161 . 109.5 no
H162 . C16 H161 . 108.8 no
C12 . C17 H173 . 110.7 no
C12 . C17 H172 . 110.9 no
H173 . C17 H172 . 107.5 no
C12 . C17 H171 . 110.0 no
H173 . C17 H171 . 110.1 no
H172 . C17 H171 . 107.6 no
C4 . Fe1 C4 2_666 38.86(13) yes
C4 . Fe1 C9 . 148.66(13) yes
C4 2_666 Fe1 C9 . 172.24(13) yes
C4 . Fe1 C12 . 108.70(11) yes
C4 2_666 Fe1 C12 . 114.56(11) yes
C9 . Fe1 C12 . 67.44(13) yes
C4 . Fe1 C8 . 116.49(12) yes
C4 2_666 Fe1 C8 . 146.17(12) yes
C9 . Fe1 C8 . 39.90(14) yes
C12 . Fe1 C8 . 40.44(14) yes
C4 . Fe1 C11 . 130.54(11) yes
C4 2_666 Fe1 C11 . 108.43(11) yes
C9 . Fe1 C11 . 67.87(13) yes
C12 . Fe1 C11 . 40.35(12) yes
C8 . Fe1 C11 . 68.05(13) yes
C4 . Fe1 C10 . 170.00(12) yes
C4 2_666 Fe1 C10 . 132.89(12) yes
C9 . Fe1 C10 . 39.96(14) yes
C12 . Fe1 C10 . 67.93(12) yes
C8 . Fe1 C10 . 67.57(13) yes
C4 . Fe1 C1 . 39.64(10) yes
C4 2_666 Fe1 C1 . 67.03(10) yes
C9 . Fe1 C1 . 117.90(12) yes
C12 . Fe1 C1 . 130.78(12) yes
C8 . Fe1 C1 . 109.50(12) yes
C4 . Fe1 C3 . 67.24(10) yes
C4 2_666 Fe1 C3 . 39.59(10) yes
C9 . Fe1 C3 . 134.63(12) yes
C12 . Fe1 C3 . 144.33(13) yes
C8 . Fe1 C3 . 173.98(13) yes
C4 . Fe1 C2 . 66.64(10) yes
C4 2_666 Fe1 C2 . 66.63(11) yes
C9 . Fe1 C2 . 112.57(12) yes
C12 . Fe1 C2 . 171.64(13) yes
C8 . Fe1 C2 . 134.26(13) yes
C11 . Fe1 C10 . 40.92(12) yes
C11 . Fe1 C1 . 168.70(12) yes
C10 . Fe1 C1 . 149.52(12) yes
C11 . Fe1 C3 . 113.62(12) yes
C10 . Fe1 C3 . 109.59(12) yes
C1 . Fe1 C3 . 70.04(11) yes
C11 . Fe1 C2 . 147.94(12) yes
C10 . Fe1 C2 . 117.86(12) yes
C1 . Fe1 C2 . 41.25(11) yes
C3 . Fe1 C2 . 41.63(12) yes
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 C2 . 1.434(4) yes
C1 C4 . 1.442(4) yes
C1 C5 . 1.500(4) yes
C1 Fe1 . 2.050(3) yes
C2 C3 . 1.446(4) yes
C2 C6 . 1.494(4) yes
C2 Fe1 . 2.019(3) yes
C3 C4 2_666 1.440(4) yes
C3 C7 . 1.494(4) yes
C3 Fe1 . 2.049(3) yes
C4 Fe1 2_666 2.185(3) yes
C4 C4 2_666 1.453(5) yes
C4 Fe1 . 2.185(3) yes
C5 H53 . 0.972 no
C5 H52 . 0.961 no
C5 H51 . 0.962 no
C6 H63 . 0.958 no
C6 H62 . 0.965 no
C6 H61 . 0.961 no
C7 H73 . 0.956 no
C7 H72 . 0.959 no
C7 H71 . 0.957 no
C8 C9 . 1.412(5) yes
C8 C12 . 1.430(5) yes
C8 C13 . 1.507(5) yes
C8 Fe1 . 2.065(3) yes
C9 C10 . 1.411(5) yes
C9 C14 . 1.510(5) yes
C9 Fe1 . 2.073(3) yes
C10 C11 . 1.438(4) yes
C10 C15 . 1.504(4) yes
C10 Fe1 . 2.055(3) yes
C11 C12 . 1.425(4) yes
C11 C16 . 1.495(5) yes
C11 Fe1 . 2.060(3) yes
C12 C17 . 1.498(4) yes
C12 Fe1 . 2.071(3) yes
C13 H133 . 0.967 no
C13 H132 . 0.957 no
C13 H131 . 0.974 no
C14 H143 . 0.961 no
C14 H142 . 0.959 no
C14 H141 . 0.960 no
C15 H153 . 0.966 no
C15 H152 . 0.962 no
C15 H151 . 0.962 no
C16 H163 . 0.968 no
C16 H162 . 0.965 no
C16 H161 . 0.959 no
C17 H173 . 0.973 no
C17 H172 . 0.963 no
C17 H171 . 0.965 no
