# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2019

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_1-048scb14
_database_code_depnum_ccdc_archive 'CCDC 1886439'
loop_
_audit_author_name
_audit_author_address
'Samantha C. Binding'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-02-27 downloaded from the CCDC.
;
_audit_creation_date             2018-12-20
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '048scb14 in P2(1)/n'
_chemical_name_systematic        ?
_chemical_melting_point          ?


_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;

_cell_length_a                   9.1531(3)
_cell_length_b                   15.1021(4)
_cell_length_c                   11.1714(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.768(3)
_cell_angle_gamma                90
_cell_volume                     1453.23(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  ?
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_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'


_cell_formula_units_Z            2

# Given Formula = C33 H30 Fe3 
# Dc =      1.36 Fooo =    608.00 Mu =    119.71 M =    297.07
# Found Formula = C34 H48 Fe2 
# Dc =      1.30 FOOO =    608.00 Mu =     81.32 M =    284.22

_chemical_formula_sum            'C34 H48 Fe2'
_chemical_formula_moiety         'C34 H48 Fe2'
_chemical_compound_source        ?
_chemical_formula_weight         568.45


_cell_measurement_reflns_used    3001
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       rod
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_max          0.300

_exptl_crystal_density_diffrn    1.299
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             608
_exptl_absorpt_coefficient_mu    8.132

# Sheldrick geometric approximatio 0.52 0.52 
_exptl_absorpt_correction_type   none
_diffrn_measurement_device_type  'Oxford Diffraction SuperNova'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54180
_diffrn_measurement_method       ω/2θ

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'SuperNova, (Oxford Diffraction, 2010)'
_computing_cell_refinement       'CrysAlis, (Oxford Diffraction, 2002)'
_computing_data_reduction        'CrysAlis, (Oxford Diffraction, 2002)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            7782
_reflns_number_total             3013
_diffrn_reflns_av_R_equivalents  0.044
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 3013 
# Theoretical number of reflections is about 6092 


_diffrn_reflns_theta_min         5.126
_diffrn_reflns_theta_max         76.290
_diffrn_measured_fraction_theta_max 0.990

_diffrn_reflns_theta_full        74.001
_diffrn_measured_fraction_theta_full 0.997


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       13
_reflns_limit_h_min              -11
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              18
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   2.87
_oxford_diffrn_Wilson_scale      0.02

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.45
_refine_diff_density_max         0.75


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3001
_refine_ls_number_restraints     0
_refine_ls_number_parameters     163
_oxford_refine_ls_R_factor_ref   0.0617
_refine_ls_wR_factor_ref         0.1173
_refine_ls_goodness_of_fit_ref   0.9784
_refine_ls_shift/su_max          0.0004947
_refine_ls_shift/su_mean         0.0000169


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3001
_refine_ls_R_factor_all          0.0617
_refine_ls_wR_factor_all         0.1173

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2281
_refine_ls_R_factor_gt           0.0442
_refine_ls_wR_factor_gt          0.1067

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.07P)² + 0.41P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
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 . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          5.67(15)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_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
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_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


_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                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_3-033scb13
_database_code_depnum_ccdc_archive 'CCDC 1886441'
loop_
_audit_author_name
_audit_author_address
'Samantha C. Binding'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-02-27 downloaded from the CCDC.
;
_audit_creation_date             13-06-03
_audit_creation_method           CRYSTALS_ver_14.40

_oxford_structure_analysis_title '033scb13 At 21: 5 on 3/ 6'
_chemical_name_systematic        
(bispentamethylcyclopentadienylnickel)-1,2,3,5,6,7-hexamethylbicyclooct[3.3.0]ane
_chemical_melting_point          .


_cell_length_a                   8.8663(3)
_cell_length_b                   15.1452(7)
_cell_length_c                   11.5069(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.974(3)
_cell_angle_gamma                90
_cell_volume                     1492.70(10)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
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_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 0.0033 0.0016 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'
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            2

# Given Formula = C34 H48 Ni2 
# Dc =      1.28 Fooo =    616.00 Mu =     12.81 M =    287.09
# Found Formula = C34 H48 Ni2 
# Dc =      1.28 FOOO =    616.00 Mu =     12.81 M =    287.09

_chemical_formula_sum            'C34 H48 Ni2'
_chemical_formula_moiety         'C34 H48 Ni2'
_chemical_compound_source        SYN
_chemical_formula_weight         574.17


_cell_measurement_reflns_used    3218
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       needle
_exptl_crystal_colour            'red brown'
_exptl_crystal_size_min          0.080
_exptl_crystal_size_mid          0.080
_exptl_crystal_size_max          0.200

_exptl_crystal_density_diffrn    1.277
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             616
_exptl_absorpt_coefficient_mu    1.281

# Sheldrick geometric approximatio 0.90 0.90 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.84
_exptl_absorpt_correction_T_max  0.90
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            13864
_reflns_number_total             5069
_diffrn_reflns_av_R_equivalents  0.027
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 5069 
# Theoretical number of reflections is about 6828 


_diffrn_reflns_theta_min         5.206
_diffrn_reflns_theta_max         27.456
_diffrn_measured_fraction_theta_max 0.992

_diffrn_reflns_theta_full        26.083
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_limit_l_max       14
_reflns_limit_h_min              -11
_reflns_limit_h_max              11
_reflns_limit_k_min              0
_reflns_limit_k_max              19
_reflns_limit_l_min              0
_reflns_limit_l_max              14

_oxford_diffrn_Wilson_B_factor   2.16
_oxford_diffrn_Wilson_scale      8.15

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.66


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>0.0\s(I)
_refine_ls_number_reflns         3387
_refine_ls_number_restraints     0
_refine_ls_number_parameters     163
_oxford_refine_ls_R_factor_ref   0.0656
_refine_ls_wR_factor_ref         0.1066
_refine_ls_goodness_of_fit_ref   0.9480
_refine_ls_shift/su_max          0.0006909
_refine_ls_shift/su_mean         0.0000228


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3387
_refine_ls_R_factor_all          0.0656
_refine_ls_wR_factor_all         0.1066

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2466
_refine_ls_R_factor_gt           0.0395
_refine_ls_wR_factor_gt          0.0838

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 11.3 15.6 7.70 2.22 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 1.1676(3) 0.5599(2) 0.4837(3) 0.0273 1.0000 Uani . . . . . .
C2 C 1.1523(4) 0.5060(2) 0.3782(3) 0.0286 1.0000 Uani . . . . . .
C3 C 1.0181(3) 0.4489(2) 0.3632(3) 0.0271 1.0000 Uani . . . . . .
C4 C 0.9532(3) 0.46589(18) 0.4622(2) 0.0231 1.0000 Uani . . . . . .
C5 C 1.2970(4) 0.6240(2) 0.5340(3) 0.0380 1.0000 Uani . . . . . .
C6 C 1.2677(4) 0.5026(3) 0.3035(3) 0.0405 1.0000 Uani . . . . . .
C7 C 0.9676(5) 0.3794(2) 0.2685(3) 0.0400 1.0000 Uani . . . . . .
C8 C 0.9023(4) 0.7236(2) 0.3307(3) 0.0368 1.0000 Uani . . . . . .
C9 C 0.9722(4) 0.7057(2) 0.2366(3) 0.0388 1.0000 Uani . . . . . .
C10 C 0.8803(4) 0.6410(2) 0.1608(3) 0.0395 1.0000 Uani . . . . . .
C11 C 0.7536(4) 0.6183(2) 0.2096(3) 0.0349 1.0000 Uani . . . . . .
C12 C 0.7686(4) 0.6683(2) 0.3153(3) 0.0328 1.0000 Uani . . . . . .
C13 C 0.9561(6) 0.7892(3) 0.4312(4) 0.0659 1.0000 Uani . . . . . .
C14 C 1.1171(5) 0.7490(4) 0.2177(5) 0.0728 1.0000 Uani . . . . . .
C15 C 0.9091(7) 0.6068(4) 0.0459(4) 0.0732 1.0000 Uani . . . . . .
C16 C 0.6266(5) 0.5516(3) 0.1605(4) 0.0608 1.0000 Uani . . . . . .
C17 C 0.6610(5) 0.6650(3) 0.3969(4) 0.0557 1.0000 Uani . . . . . .
Ni1 Ni 0.96911(4) 0.58746(3) 0.33853(3) 0.0251 1.0000 Uani . . . . . .
H63 H 1.2596 0.6724 0.5725 0.0569 1.0000 Uiso R . . . . .
H62 H 1.3797 0.5957 0.5916 0.0575 1.0000 Uiso R . . . . .
H61 H 1.3355 0.6473 0.4695 0.0573 1.0000 Uiso R . . . . .
H73 H 1.3083 0.5609 0.2961 0.0612 1.0000 Uiso R . . . . .
H72 H 1.3531 0.4649 0.3417 0.0608 1.0000 Uiso R . . . . .
H71 H 1.2196 0.4797 0.2248 0.0612 1.0000 Uiso R . . . . .
H83 H 0.8595 0.3651 0.2575 0.0603 1.0000 Uiso R . . . . .
H82 H 1.0279 0.3267 0.2923 0.0605 1.0000 Uiso R . . . . .
H81 H 0.9836 0.3987 0.1935 0.0606 1.0000 Uiso R . . . . .
H143 H 1.1803 0.7048 0.1919 0.1096 1.0000 Uiso R . . . . .
H142 H 1.0902 0.7947 0.1570 0.1088 1.0000 Uiso R . . . . .
H141 H 1.1756 0.7746 0.2932 0.1094 1.0000 Uiso R . . . . .
H153 H 1.0197 0.5959 0.0578 0.1100 1.0000 Uiso R . . . . .
H152 H 0.8761 0.6496 -0.0182 0.1100 1.0000 Uiso R . . . . .
H151 H 0.8504 0.5521 0.0241 0.1100 1.0000 Uiso R . . . . .
H163 H 0.6557 0.5180 0.0978 0.0912 1.0000 Uiso R . . . . .
H162 H 0.5286 0.5814 0.1274 0.0911 1.0000 Uiso R . . . . .
H161 H 0.6144 0.5124 0.2238 0.0911 1.0000 Uiso R . . . . .
H173 H 0.6242 0.6054 0.4004 0.0843 1.0000 Uiso R . . . . .
H172 H 0.5733 0.7034 0.3675 0.0844 1.0000 Uiso R . . . . .
H171 H 0.7187 0.6844 0.4758 0.0844 1.0000 Uiso R . . . . .
H183 H 1.0658 0.8016 0.4431 0.0993 1.0000 Uiso R . . . . .
H182 H 0.8991 0.8438 0.4133 0.0990 1.0000 Uiso R . . . . .
H181 H 0.9404 0.7648 0.5051 0.0995 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.3428(4)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C4 2_766 1.425(4) yes
C1 . C2 . 1.440(4) yes
C1 . C5 . 1.500(4) yes
C1 . Ni1 . 2.132(3) yes
C2 . C3 . 1.444(4) yes
C2 . C6 . 1.498(4) yes
C2 . Ni1 . 1.997(3) yes
C3 . C4 . 1.426(4) yes
C3 . C7 . 1.498(4) yes
C3 . Ni1 . 2.146(3) yes
C4 . Ni1 2_766 2.360(3) yes
C4 . C4 2_766 1.463(5) yes
C4 . Ni1 . 2.353(3) yes
C5 . H63 . 0.959 no
C5 . H62 . 0.954 no
C5 . H61 . 0.960 no
C6 . H73 . 0.966 no
C6 . H72 . 0.959 no
C6 . H71 . 0.960 no
C7 . H83 . 0.959 no
C7 . H82 . 0.960 no
C7 . H81 . 0.956 no
C8 . C9 . 1.407(5) yes
C8 . C12 . 1.425(5) yes
C8 . C13 . 1.506(5) yes
C8 . Ni1 . 2.142(3) yes
C9 . C10 . 1.421(5) yes
C9 . C14 . 1.507(5) yes
C9 . Ni1 . 2.145(3) yes
C10 . C11 . 1.422(5) yes
C10 . C15 . 1.501(5) yes
C10 . Ni1 . 2.152(3) yes
C11 . C12 . 1.409(5) yes
C11 . C16 . 1.510(5) yes
C11 . Ni1 . 2.146(3) yes
C12 . C17 . 1.502(5) yes
C12 . Ni1 . 2.118(3) yes
C13 . H183 . 0.965 no
C13 . H182 . 0.963 no
C13 . H181 . 0.969 no
C14 . H143 . 0.967 no
C14 . H142 . 0.968 no
C14 . H141 . 0.971 no
C15 . H153 . 0.969 no
C15 . H152 . 0.968 no
C15 . H151 . 0.977 no
C16 . H163 . 0.971 no
C16 . H162 . 0.966 no
C16 . H161 . 0.966 no
C17 . H173 . 0.965 no
C17 . H172 . 0.960 no
C17 . H171 . 0.965 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 2_766 C1 . C2 . 107.1(3) yes
C4 2_766 C1 . C5 . 126.5(3) yes
C2 . C1 . C5 . 126.0(3) yes
C4 2_766 C1 . Ni1 . 80.47(17) yes
C2 . C1 . Ni1 . 64.63(16) yes
C5 . C1 . Ni1 . 124.7(2) yes
C1 . C2 . C3 . 109.6(3) yes
C1 . C2 . C6 . 125.0(3) yes
C3 . C2 . C6 . 125.1(3) yes
C1 . C2 . Ni1 . 74.70(18) yes
C3 . C2 . Ni1 . 75.28(18) yes
C6 . C2 . Ni1 . 121.7(2) yes
C2 . C3 . C4 . 106.6(3) yes
C2 . C3 . C7 . 126.1(3) yes
C4 . C3 . C7 . 126.9(3) yes
C2 . C3 . Ni1 . 64.13(17) yes
C4 . C3 . Ni1 . 79.63(18) yes
C7 . C3 . Ni1 . 125.4(2) yes
Ni1 2_766 C4 . C4 2_766 71.7(2) yes
Ni1 2_766 C4 . C3 . 129.6(2) yes
C4 2_766 C4 . C3 . 108.6(3) yes
Ni1 2_766 C4 . C1 2_766 62.97(16) yes
C4 2_766 C4 . C1 2_766 108.0(3) yes
C3 . C4 . C1 2_766 143.4(3) yes
Ni1 2_766 C4 . Ni1 . 143.84(13) yes
C4 2_766 C4 . Ni1 . 72.2(2) yes
C3 . C4 . Ni1 . 63.79(16) yes
C1 2_766 C4 . Ni1 . 130.3(2) yes
C1 . C5 . H63 . 110.5 no
C1 . C5 . H62 . 110.5 no
H63 . C5 . H62 . 108.6 no
C1 . C5 . H61 . 109.2 no
H63 . C5 . H61 . 108.0 no
H62 . C5 . H61 . 109.9 no
C2 . C6 . H73 . 110.2 no
C2 . C6 . H72 . 109.5 no
H73 . C6 . H72 . 108.4 no
C2 . C6 . H71 . 110.6 no
H73 . C6 . H71 . 109.3 no
H72 . C6 . H71 . 108.9 no
C3 . C7 . H83 . 110.9 no
C3 . C7 . H82 . 109.7 no
H83 . C7 . H82 . 108.3 no
C3 . C7 . H81 . 110.8 no
H83 . C7 . H81 . 109.1 no
H82 . C7 . H81 . 108.0 no
C9 . C8 . C12 . 108.0(3) yes
C9 . C8 . C13 . 127.1(4) yes
C12 . C8 . C13 . 124.9(4) yes
C9 . C8 . Ni1 . 71.0(2) yes
C12 . C8 . Ni1 . 69.55(18) yes
C13 . C8 . Ni1 . 125.0(2) yes
C8 . C9 . C10 . 108.0(3) yes
C8 . C9 . C14 . 126.1(4) yes
C10 . C9 . C14 . 125.9(4) yes
C8 . C9 . Ni1 . 70.69(18) yes
C10 . C9 . Ni1 . 70.92(19) yes
C14 . C9 . Ni1 . 125.0(2) yes
C9 . C10 . C11 . 108.1(3) yes
C9 . C10 . C15 . 125.2(4) yes
C11 . C10 . C15 . 126.6(4) yes
C9 . C10 . Ni1 . 70.46(18) yes
C11 . C10 . Ni1 . 70.47(18) yes
C15 . C10 . Ni1 . 127.1(3) yes
C10 . C11 . C12 . 107.7(3) yes
C10 . C11 . C16 . 127.1(4) yes
C12 . C11 . C16 . 125.2(4) yes
C10 . C11 . Ni1 . 70.89(19) yes
C12 . C11 . Ni1 . 69.62(18) yes
C16 . C11 . Ni1 . 123.9(3) yes
C8 . C12 . C11 . 108.2(3) yes
C8 . C12 . C17 . 125.7(4) yes
C11 . C12 . C17 . 126.0(4) yes
C8 . C12 . Ni1 . 71.35(18) yes
C11 . C12 . Ni1 . 71.78(19) yes
C17 . C12 . Ni1 . 123.4(2) yes
C8 . C13 . H183 . 110.2 no
C8 . C13 . H182 . 110.9 no
H183 . C13 . H182 . 108.6 no
C8 . C13 . H181 . 109.4 no
H183 . C13 . H181 . 108.5 no
H182 . C13 . H181 . 109.2 no
C9 . C14 . H143 . 109.0 no
C9 . C14 . H142 . 110.8 no
H143 . C14 . H142 . 109.1 no
C9 . C14 . H141 . 108.8 no
H143 . C14 . H141 . 109.4 no
H142 . C14 . H141 . 109.6 no
C10 . C15 . H153 . 109.3 no
C10 . C15 . H152 . 110.7 no
H153 . C15 . H152 . 108.5 no
C10 . C15 . H151 . 108.6 no
H153 . C15 . H151 . 110.2 no
H152 . C15 . H151 . 109.5 no
C11 . C16 . H163 . 108.3 no
C11 . C16 . H162 . 110.1 no
H163 . C16 . H162 . 109.6 no
C11 . C16 . H161 . 110.3 no
H163 . C16 . H161 . 110.0 no
H162 . C16 . H161 . 108.6 no
C12 . C17 . H173 . 109.5 no
C12 . C17 . H172 . 110.3 no
H173 . C17 . H172 . 109.3 no
C12 . C17 . H171 . 108.0 no
H173 . C17 . H171 . 110.4 no
H172 . C17 . H171 . 109.3 no
C4 2_766 Ni1 . C4 . 36.16(13) yes
C4 2_766 Ni1 . C10 . 174.89(12) yes
C4 . Ni1 . C10 . 143.64(13) yes
C4 2_766 Ni1 . C3 . 62.52(10) yes
C4 . Ni1 . C3 . 36.58(10) yes
C10 . Ni1 . C3 . 120.39(13) yes
C4 2_766 Ni1 . C11 . 136.92(12) yes
C4 . Ni1 . C11 . 114.00(11) yes
C10 . Ni1 . C11 . 38.64(13) yes
C3 . Ni1 . C11 . 114.70(12) yes
C4 2_766 Ni1 . C9 . 140.85(13) yes
C4 . Ni1 . C9 . 174.35(13) yes
C10 . Ni1 . C9 . 38.62(15) yes
C3 . Ni1 . C9 . 149.06(13) yes
C11 . Ni1 . C9 . 64.85(13) yes
C4 2_766 Ni1 . C8 . 112.25(12) yes
C4 . Ni1 . C8 . 136.04(12) yes
C10 . Ni1 . C8 . 64.39(13) yes
C3 . Ni1 . C8 . 172.45(13) yes
C11 . Ni1 . C8 . 64.78(13) yes
C4 2_766 Ni1 . C1 . 36.56(10) yes
C4 . Ni1 . C1 . 62.55(10) yes
C10 . Ni1 . C1 . 147.59(13) yes
C3 . Ni1 . C1 . 66.86(12) yes
C11 . Ni1 . C1 . 172.68(13) yes
C4 2_766 Ni1 . C12 . 110.19(11) yes
C4 . Ni1 . C12 . 110.43(11) yes
C10 . Ni1 . C12 . 64.73(13) yes
C3 . Ni1 . C12 . 135.74(13) yes
C11 . Ni1 . C12 . 38.60(13) yes
C4 2_766 Ni1 . C2 . 63.26(11) yes
C4 . Ni1 . C2 . 63.27(11) yes
C10 . Ni1 . C2 . 121.79(13) yes
C3 . Ni1 . C2 . 40.59(12) yes
C11 . Ni1 . C2 . 144.99(13) yes
C9 . Ni1 . C8 . 38.31(14) yes
C9 . Ni1 . C1 . 117.87(13) yes
C8 . Ni1 . C1 . 112.65(12) yes
C9 . Ni1 . C12 . 65.00(13) yes
C8 . Ni1 . C12 . 39.09(13) yes
C1 . Ni1 . C12 . 135.10(13) yes
C9 . Ni1 . C2 . 121.11(13) yes
C8 . Ni1 . C2 . 143.61(13) yes
C1 . Ni1 . C2 . 40.67(12) yes
C12 . Ni1 . C2 . 173.16(12) yes


_iucr_refine_instruction_details_constraints 
;
#
# Punched on 03/06/13 at 21:21:18
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   5,X'S) H   (  63,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE C   (   6,X'S) H   (  73,X'S) H   (  72,X'S) H   (  71,X'S) 
RIDE C   (   7,X'S) H   (  83,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (  13,X'S) H   ( 183,X'S) H   ( 182,X'S) H   ( 181,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_instruction_details_restraints 
;
#
# Punched on 03/06/13 at 21:21:18
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_4-062scb15
_database_code_depnum_ccdc_archive 'CCDC 1886442'
loop_
_audit_author_name
_audit_author_address
'Samantha C. Binding'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-02-27 downloaded from the CCDC.
;
_audit_creation_date             2015-01-06
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '062scb15 At 10: 3 on 6/ 1'
_chemical_name_systematic        bis(cyclopentadienylcobalt)pentalenyl
_chemical_melting_point          'not measured'


_cell_length_a                   7.9066(2)
_cell_length_b                   8.1643(2)
_cell_length_c                   9.3165(4)
_cell_angle_alpha                67.9417(14)
_cell_angle_beta                 83.4571(14)
_cell_angle_gamma                61.8652(17)
_cell_volume                     490.05(3)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 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'


_cell_formula_units_Z            1

# Given Formula = C24 H28 Co2 
# Dc =      1.47 Fooo =    226.00 Mu =     16.96 M =    217.18
# Found Formula = C24 H28 Co2 
# Dc =      1.47 FOOO =    226.00 Mu =     16.96 M =    217.18

_chemical_formula_sum            'C24 H28 Co2'
_chemical_formula_moiety         'C24 H28 Co2'
_chemical_compound_source        SYN
_chemical_formula_weight         434.35


_cell_measurement_reflns_used    1955
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            black
_exptl_crystal_size_min          0.40
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_max          0.42

_exptl_crystal_density_diffrn    1.472
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             226
_exptl_absorpt_coefficient_mu    1.696

# Sheldrick geometric approximatio 0.51 0.51 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.43
_exptl_absorpt_correction_T_max  0.51
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            6663
_reflns_number_total             2232
_diffrn_reflns_av_R_equivalents  0.019
# Number of reflections without Friedels Law is 3741 
# Number of reflections with Friedels Law is 2232 
# Theoretical number of reflections is about 2251 


_diffrn_reflns_theta_min         5.117
_diffrn_reflns_theta_max         27.498
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        26.948
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       10
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              -9
_reflns_limit_k_max              10
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   1.40
_oxford_diffrn_Wilson_scale      1.51

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.39
_refine_diff_density_max         0.50


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2232
_refine_ls_number_restraints     0
_refine_ls_number_parameters     118
_oxford_refine_ls_R_factor_ref   0.0350
_refine_ls_wR_factor_ref         0.0655
_refine_ls_goodness_of_fit_ref   0.8884
_refine_ls_shift/su_max          0.0003598
_refine_ls_shift/su_mean         0.0000147


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2232
_refine_ls_R_factor_all          0.0350
_refine_ls_wR_factor_all         0.0655

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2013
_refine_ls_R_factor_gt           0.0292
_refine_ls_wR_factor_gt          0.0603

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 11.5 15.0 6.86 1.69 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.6598(3) 0.7702(3) 0.1486(2) 0.0190 1.0000 Uani . . . . . .
C2 C 0.6374(3) 0.8948(3) 0.2326(2) 0.0196 1.0000 Uani . . . . . .
C3 C 0.4962(3) 1.0956(3) 0.1462(2) 0.0192 1.0000 Uani . . . . . .
C4 C 0.5501(3) 0.9007(3) 0.0007(2) 0.0169 1.0000 Uani . . . . . .
C5 C 0.8001(3) 0.5532(3) 0.1931(3) 0.0276 1.0000 Uani . . . . . .
C6 C 0.7468(3) 0.8270(4) 0.3835(3) 0.0279 1.0000 Uani . . . . . .
C7 C 0.4344(4) 1.2757(4) 0.1872(3) 0.0278 1.0000 Uani . . . . . .
C8 C 0.1315(3) 1.0108(3) 0.3203(3) 0.0224 1.0000 Uani . . . . . .
C9 C 0.2535(3) 0.8171(3) 0.4255(2) 0.0212 1.0000 Uani . . . . . .
C10 C 0.3004(3) 0.6821(3) 0.3491(3) 0.0219 1.0000 Uani . . . . . .
C11 C 0.1993(3) 0.7916(4) 0.1988(3) 0.0249 1.0000 Uani . . . . . .
C12 C 0.0930(3) 0.9947(3) 0.1816(3) 0.0259 1.0000 Uani . . . . . .
Co1 Co 0.38498(4) 0.89829(4) 0.21423(3) 0.0161 1.0000 Uani . . . . . .
H101 H 0.3863 0.5372 0.3928 0.0272 1.0000 Uiso R . . . . .
H91 H 0.3037 0.7842 0.5298 0.0267 1.0000 Uiso R . . . . .
H81 H 0.0792 1.1333 0.3415 0.0272 1.0000 Uiso R . . . . .
H121 H 0.0106 1.1081 0.0886 0.0319 1.0000 Uiso R . . . . .
H111 H 0.2025 0.7364 0.1201 0.0306 1.0000 Uiso R . . . . .
H73 H 0.4434 1.2360 0.2983 0.0431 1.0000 Uiso R . . . . .
H72 H 0.5178 1.3367 0.1447 0.0430 1.0000 Uiso R . . . . .
H71 H 0.3020 1.3732 0.1472 0.0437 1.0000 Uiso R . . . . .
H63 H 0.6676 0.9117 0.4402 0.0430 1.0000 Uiso R . . . . .
H62 H 0.8631 0.8409 0.3613 0.0435 1.0000 Uiso R . . . . .
H61 H 0.7782 0.6879 0.4448 0.0431 1.0000 Uiso R . . . . .
H53 H 0.8240 0.4922 0.3045 0.0430 1.0000 Uiso R . . . . .
H52 H 0.9192 0.5388 0.1458 0.0435 1.0000 Uiso R . . . . .
H51 H 0.7462 0.4877 0.1568 0.0431 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.7912(17)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C2 . 1.441(3) yes
C1 . C4 . 1.444(3) yes
C1 . C5 . 1.497(3) yes
C1 . Co1 . 2.055(2) yes
C2 . C3 . 1.439(3) yes
C2 . C6 . 1.507(3) yes
C2 . Co1 . 2.008(2) yes
C3 . C4 2_675 1.442(3) yes
C3 . C7 . 1.499(3) yes
C3 . Co1 . 2.053(2) yes
C4 . Co1 2_675 2.2491(19) yes
C4 . C4 2_675 1.426(4) yes
C4 . Co1 . 2.2508(19) yes
C5 . H53 . 0.964 no
C5 . H52 . 0.967 no
C5 . H51 . 0.982 no
C6 . H63 . 0.970 no
C6 . H62 . 0.968 no
C6 . H61 . 0.978 no
C7 . H73 . 0.961 no
C7 . H72 . 0.970 no
C7 . H71 . 0.974 no
C8 . C9 . 1.416(3) yes
C8 . C12 . 1.427(3) yes
C8 . Co1 . 2.081(2) yes
C8 . H81 . 0.975 no
C9 . C10 . 1.416(3) yes
C9 . Co1 . 2.144(2) yes
C9 . H91 . 0.982 no
C10 . C11 . 1.428(3) yes
C10 . Co1 . 2.097(2) yes
C10 . H101 . 0.985 no
C11 . C12 . 1.414(3) yes
C11 . Co1 . 2.070(2) yes
C11 . H111 . 0.987 no
C12 . Co1 . 2.075(2) yes
C12 . H121 . 0.994 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . C1 . C4 . 107.03(17) yes
C2 . C1 . C5 . 126.0(2) yes
C4 . C1 . C5 . 126.03(19) yes
C2 . C1 . Co1 . 67.50(11) yes
C4 . C1 . Co1 . 77.91(12) yes
C5 . C1 . Co1 . 128.54(15) yes
C1 . C2 . C3 . 108.41(18) yes
C1 . C2 . C6 . 125.7(2) yes
C3 . C2 . C6 . 125.8(2) yes
C1 . C2 . Co1 . 70.99(12) yes
C3 . C2 . Co1 . 70.90(12) yes
C6 . C2 . Co1 . 125.01(14) yes
C4 2_675 C3 . C2 . 107.28(17) yes
C4 2_675 C3 . C7 . 125.34(19) yes
C2 . C3 . C7 . 126.5(2) yes
C4 2_675 C3 . Co1 . 77.96(12) yes
C2 . C3 . Co1 . 67.61(11) yes
C7 . C3 . Co1 . 127.89(15) yes
Co1 2_675 C4 . C1 . 130.65(14) yes
Co1 2_675 C4 . C3 2_675 63.20(10) yes
C1 . C4 . C3 2_675 143.26(19) yes
Co1 2_675 C4 . C4 2_675 71.59(14) yes
C1 . C4 . C4 2_675 108.5(2) yes
C3 2_675 C4 . C4 2_675 108.3(2) yes
Co1 2_675 C4 . Co1 . 143.05(9) yes
C1 . C4 . Co1 . 63.23(10) yes
C3 2_675 C4 . Co1 . 130.49(14) yes
C4 2_675 C4 . Co1 . 71.46(14) yes
C1 . C5 . H53 . 109.2 no
C1 . C5 . H52 . 109.6 no
H53 . C5 . H52 . 109.7 no
C1 . C5 . H51 . 109.5 no
H53 . C5 . H51 . 109.5 no
H52 . C5 . H51 . 109.4 no
C2 . C6 . H63 . 108.8 no
C2 . C6 . H62 . 109.1 no
H63 . C6 . H62 . 108.7 no
C2 . C6 . H61 . 109.6 no
H63 . C6 . H61 . 110.0 no
H62 . C6 . H61 . 110.5 no
C3 . C7 . H73 . 109.4 no
C3 . C7 . H72 . 110.3 no
H73 . C7 . H72 . 108.2 no
C3 . C7 . H71 . 110.6 no
H73 . C7 . H71 . 109.0 no
H72 . C7 . H71 . 109.4 no
C9 . C8 . C12 . 108.56(19) yes
C9 . C8 . Co1 . 72.85(12) yes
C12 . C8 . Co1 . 69.72(12) yes
C9 . C8 . H81 . 125.3 no
C12 . C8 . H81 . 126.1 no
Co1 . C8 . H81 . 125.1 no
C8 . C9 . C10 . 107.56(19) yes
C8 . C9 . Co1 . 68.03(11) yes
C10 . C9 . Co1 . 68.71(11) yes
C8 . C9 . H91 . 126.0 no
C10 . C9 . H91 . 126.3 no
Co1 . C9 . H91 . 125.4 no
C9 . C10 . C11 . 108.26(19) yes
C9 . C10 . Co1 . 72.32(12) yes
C11 . C10 . Co1 . 68.94(12) yes
C9 . C10 . H101 . 125.8 no
C11 . C10 . H101 . 125.9 no
Co1 . C10 . H101 . 125.3 no
C10 . C11 . C12 . 107.98(19) yes
C10 . C11 . Co1 . 70.99(12) yes
C12 . C11 . Co1 . 70.28(13) yes
C10 . C11 . H111 . 126.4 no
C12 . C11 . H111 . 125.6 no
Co1 . C11 . H111 . 124.2 no
C8 . C12 . C11 . 107.53(19) yes
C8 . C12 . Co1 . 70.14(12) yes
C11 . C12 . Co1 . 69.84(12) yes
C8 . C12 . H121 . 125.5 no
C11 . C12 . H121 . 127.0 no
Co1 . C12 . H121 . 123.4 no
C9 . Co1 . C4 2_675 157.75(8) yes
C9 . Co1 . C4 . 165.17(8) yes
C4 2_675 Co1 . C4 . 36.95(9) yes
C9 . Co1 . C10 . 38.97(8) yes
C4 2_675 Co1 . C10 . 158.00(8) yes
C4 . Co1 . C10 . 126.88(8) yes
C9 . Co1 . C8 . 39.12(8) yes
C4 2_675 Co1 . C8 . 120.78(8) yes
C4 . Co1 . C8 . 150.95(8) yes
C10 . Co1 . C8 . 66.29(8) yes
C9 . Co1 . C12 . 66.28(8) yes
C4 2_675 Co1 . C12 . 104.27(8) yes
C4 . Co1 . C12 . 115.91(8) yes
C10 . Co1 . C12 . 66.85(9) yes
C8 . Co1 . C12 . 40.14(9) yes
C9 . Co1 . C11 . 66.26(8) yes
C4 2_675 Co1 . C11 . 120.33(8) yes
C4 . Co1 . C11 . 105.39(8) yes
C10 . Co1 . C11 . 40.07(8) yes
C8 . Co1 . C11 . 67.00(9) yes
C9 . Co1 . C1 . 132.84(8) yes
C4 2_675 Co1 . C1 . 65.32(8) yes
C4 . Co1 . C1 . 38.85(8) yes
C10 . Co1 . C1 . 111.57(8) yes
C8 . Co1 . C1 . 169.47(9) yes
C9 . Co1 . C3 . 127.40(8) yes
C4 2_675 Co1 . C3 . 38.84(8) yes
C4 . Co1 . C3 . 65.20(8) yes
C10 . Co1 . C3 . 162.89(8) yes
C8 . Co1 . C3 . 109.53(8) yes
C9 . Co1 . C2 . 117.14(8) yes
C4 2_675 Co1 . C2 . 65.76(8) yes
C4 . Co1 . C2 . 65.70(8) yes
C10 . Co1 . C2 . 127.70(8) yes
C8 . Co1 . C2 . 130.82(9) yes
C12 . Co1 . C11 . 39.88(9) yes
C12 . Co1 . C1 . 149.73(9) yes
C11 . Co1 . C1 . 118.61(9) yes
C12 . Co1 . C3 . 121.59(9) yes
C11 . Co1 . C3 . 155.59(9) yes
C1 . Co1 . C3 . 69.30(8) yes
C12 . Co1 . C2 . 162.27(9) yes
C11 . Co1 . C2 . 157.69(9) yes
C1 . Co1 . C2 . 41.51(8) yes
C3 . Co1 . C2 . 41.48(8) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 06/01/15 at 10:24:46
#
#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   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 06/01/15 at 10:24:46
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-035scb13
_database_code_depnum_ccdc_archive 'CCDC 1886440'
loop_
_audit_author_name
_audit_author_address
'Samantha C. Binding'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-02-27 downloaded from the CCDC.
;
_audit_creation_date             2015-02-10
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '035scb13 At 0:11 on 30/ 6'
_chemical_name_systematic        
bis(pentamethylcyclopentadienylcobalt)pentalene
_chemical_melting_point          'not measured'


_cell_length_a                   16.7219(4)
_cell_length_b                   8.6986(2)
_cell_length_c                   20.5957(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.8732(10)
_cell_angle_gamma                90
_cell_volume                     2895.42(12)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c '
_symmetry_space_group_name_Hall  '-C 2yc'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,y+1/2,z
-x+1/2,-y+1/2,-z
x,-y,z+1/2
-x,y,-z+1/2
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

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 0.0033 0.0016 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'
Co 0.3494 0.9721 12.2841 4.2791 7.3409 0.2784 4.0034 13.5359 2.3488 71.1692
1.0118 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C34 H33 Co2 
# Dc =      1.28 Fooo =   1224.00 Mu =     11.65 M =    279.75
# Found Formula = C34 H48 Co2 
# Dc =      1.32 FOOO =   1224.00 Mu =     11.66 M =    287.31

_chemical_formula_sum            'C34 H48 Co2'
_chemical_formula_moiety         'C34 H48 Co2'
_chemical_compound_source        SYN
_chemical_formula_weight         574.62


_cell_measurement_reflns_used    3399
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            'dark brown'
_exptl_crystal_size_min          0.05
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_max          0.16

_exptl_crystal_density_diffrn    1.318
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             1224
_exptl_absorpt_coefficient_mu    1.166

# Sheldrick geometric approximatio 0.83 0.94 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.87
_exptl_absorpt_correction_T_max  0.94
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'Superflip (Palatinus & Chapuis, 2007)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            17044
_reflns_number_total             3296
_diffrn_reflns_av_R_equivalents  0.029
# Number of reflections without Friedels Law is 6003 
# Number of reflections with Friedels Law is 3296 
# Theoretical number of reflections is about 3336 


_diffrn_reflns_theta_min         5.116
_diffrn_reflns_theta_max         27.531
_diffrn_measured_fraction_theta_max 0.987

_diffrn_reflns_theta_full        26.430
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_limit_l_max       26
_reflns_limit_h_min              -21
_reflns_limit_h_max              20
_reflns_limit_k_min              0
_reflns_limit_k_max              11
_reflns_limit_l_min              0
_reflns_limit_l_max              26

_oxford_diffrn_Wilson_B_factor   2.07
_oxford_diffrn_Wilson_scale      28.61

_atom_sites_solution_primary     Other #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.58
_refine_diff_density_max         0.86


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         3296
_refine_ls_number_restraints     0
_refine_ls_number_parameters     163
_oxford_refine_ls_R_factor_ref   0.0582
_refine_ls_wR_factor_ref         0.0978
_refine_ls_goodness_of_fit_ref   0.9421
_refine_ls_shift/su_max          0.0003994
_refine_ls_shift/su_mean         0.0000286


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        3296
_refine_ls_R_factor_all          0.0582
_refine_ls_wR_factor_all         0.0978

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2456
_refine_ls_R_factor_gt           0.0355
_refine_ls_wR_factor_gt          0.0758

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 15.4 22.1 10.6 2.70 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.21875(16) 0.8532(3) 0.56514(13) 0.0250 1.0000 Uani . . . . . .
C2 C 0.19888(16) 0.7038(3) 0.58662(13) 0.0256 1.0000 Uani . . . . . .
C3 C 0.22494(16) 0.5886(3) 0.54605(13) 0.0253 1.0000 Uani . . . . . .
C4 C 0.25188(16) 0.6697(3) 0.49412(13) 0.0232 1.0000 Uani . . . . . .
C5 C 0.20057(19) 1.0046(3) 0.59339(15) 0.0342 1.0000 Uani . . . . . .
C6 C 0.15455(19) 0.6728(4) 0.63977(15) 0.0352 1.0000 Uani . . . . . .
C7 C 0.21390(19) 0.4189(3) 0.55033(15) 0.0340 1.0000 Uani . . . . . .
C8 C 0.41820(18) 0.8488(4) 0.65528(16) 0.0378 1.0000 Uani . . . . . .
C9 C 0.39104(17) 0.7516(4) 0.70149(14) 0.0366 1.0000 Uani . . . . . .
C10 C 0.39863(17) 0.5987(4) 0.68227(14) 0.0333 1.0000 Uani . . . . . .
C11 C 0.43224(17) 0.6000(3) 0.62438(14) 0.0314 1.0000 Uani . . . . . .
C12 C 0.44613(16) 0.7546(4) 0.60904(14) 0.0330 1.0000 Uani . . . . . .
C13 C 0.4226(2) 1.0216(4) 0.6580(2) 0.0576 1.0000 Uani . . . . . .
C14 C 0.3598(2) 0.8024(5) 0.76053(17) 0.0560 1.0000 Uani . . . . . .
C15 C 0.3791(2) 0.4570(5) 0.71689(19) 0.0513 1.0000 Uani . . . . . .
C16 C 0.4530(2) 0.4604(4) 0.58923(19) 0.0483 1.0000 Uani . . . . . .
C17 C 0.48272(19) 0.8079(5) 0.55357(17) 0.0486 1.0000 Uani . . . . . .
Co1 Co 0.32119(2) 0.71736(4) 0.602031(18) 0.0246 1.0000 Uani . . . . . .
H73 H 0.2589 0.3668 0.5384 0.0528 1.0000 Uiso R . . . . .
H72 H 0.2140 0.3909 0.5951 0.0530 1.0000 Uiso R . . . . .
H71 H 0.1637 0.3879 0.5201 0.0526 1.0000 Uiso R . . . . .
H83 H 0.1651 0.7548 0.6713 0.0547 1.0000 Uiso R . . . . .
H82 H 0.1738 0.5790 0.6622 0.0550 1.0000 Uiso R . . . . .
H81 H 0.0968 0.6651 0.6194 0.0548 1.0000 Uiso R . . . . .
H143 H 0.3324 0.4765 0.7350 0.0762 1.0000 Uiso R . . . . .
H142 H 0.4257 0.4302 0.7530 0.0762 1.0000 Uiso R . . . . .
H141 H 0.3672 0.3743 0.6856 0.0755 1.0000 Uiso R . . . . .
H153 H 0.3204 0.7298 0.7681 0.0796 1.0000 Uiso R . . . . .
H152 H 0.4054 0.8083 0.7997 0.0803 1.0000 Uiso R . . . . .
H151 H 0.3355 0.9015 0.7508 0.0796 1.0000 Uiso R . . . . .
H163 H 0.3815 1.0607 0.6788 0.0846 1.0000 Uiso R . . . . .
H162 H 0.4768 1.0506 0.6854 0.0854 1.0000 Uiso R . . . . .
H161 H 0.4156 1.0616 0.6131 0.0842 1.0000 Uiso R . . . . .
H173 H 0.4660 0.9104 0.5424 0.0707 1.0000 Uiso R . . . . .
H172 H 0.5422 0.8051 0.5693 0.0714 1.0000 Uiso R . . . . .
H171 H 0.4655 0.7423 0.5157 0.0707 1.0000 Uiso R . . . . .
H183 H 0.4152 0.3793 0.5905 0.0716 1.0000 Uiso R . . . . .
H182 H 0.5083 0.4273 0.6115 0.0725 1.0000 Uiso R . . . . .
H181 H 0.4508 0.4860 0.5438 0.0718 1.0000 Uiso R . . . . .
H513 H 0.2399 1.0802 0.5877 0.0538 1.0000 Uiso R . . . . .
H512 H 0.2044 0.9920 0.6405 0.0541 1.0000 Uiso R . . . . .
H511 H 0.1460 1.0366 0.5706 0.0540 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.18503(11)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C4 4_566 1.442(3) yes
C1 . C2 . 1.439(4) yes
C1 . C5 . 1.502(4) yes
C1 . Co1 . 2.059(3) yes
C2 . C3 . 1.442(4) yes
C2 . C6 . 1.496(3) yes
C2 . Co1 . 1.991(3) yes
C3 . C4 . 1.446(3) yes
C3 . C7 . 1.493(4) yes
C3 . Co1 . 2.055(3) yes
C4 . Co1 4_566 2.267(3) yes
C4 . C4 4_566 1.422(5) yes
C4 . Co1 . 2.266(3) yes
C5 . H513 . 0.958 no
C5 . H512 . 0.962 no
C5 . H511 . 0.955 no
C6 . H83 . 0.950 no
C6 . H82 . 0.953 no
C6 . H81 . 0.952 no
C7 . H73 . 0.962 no
C7 . H72 . 0.953 no
C7 . H71 . 0.947 no
C8 . C9 . 1.432(4) yes
C8 . C12 . 1.423(4) yes
C8 . C13 . 1.505(5) yes
C8 . Co1 . 2.056(3) yes
C9 . C10 . 1.402(4) yes
C9 . C14 . 1.508(4) yes
C9 . Co1 . 2.103(3) yes
C10 . C11 . 1.443(4) yes
C10 . C15 . 1.502(5) yes
C10 . Co1 . 2.091(3) yes
C11 . C12 . 1.414(4) yes
C11 . C16 . 1.499(4) yes
C11 . Co1 . 2.065(3) yes
C12 . C17 . 1.501(4) yes
C12 . Co1 . 2.082(3) yes
C13 . H163 . 0.961 no
C13 . H162 . 0.970 no
C13 . H161 . 0.965 no
C14 . H153 . 0.954 no
C14 . H152 . 0.959 no
C14 . H151 . 0.952 no
C15 . H143 . 0.963 no
C15 . H142 . 0.958 no
C15 . H141 . 0.952 no
C16 . H183 . 0.953 no
C16 . H182 . 0.965 no
C16 . H181 . 0.952 no
C17 . H173 . 0.945 no
C17 . H172 . 0.965 no
C17 . H171 . 0.949 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 4_566 C1 . C2 . 106.9(2) yes
C4 4_566 C1 . C5 . 126.6(2) yes
C2 . C1 . C5 . 126.0(2) yes
C4 4_566 C1 . Co1 . 78.54(15) yes
C2 . C1 . Co1 . 66.69(14) yes
C5 . C1 . Co1 . 126.3(2) yes
C1 . C2 . C3 . 108.7(2) yes
C1 . C2 . C6 . 125.8(2) yes
C3 . C2 . C6 . 125.4(2) yes
C1 . C2 . Co1 . 71.74(14) yes
C3 . C2 . Co1 . 71.50(15) yes
C6 . C2 . Co1 . 125.2(2) yes
C2 . C3 . C4 . 106.7(2) yes
C2 . C3 . C7 . 126.3(2) yes
C4 . C3 . C7 . 126.3(2) yes
C2 . C3 . Co1 . 66.78(15) yes
C4 . C3 . Co1 . 78.55(15) yes
C7 . C3 . Co1 . 126.6(2) yes
Co1 4_566 C4 . C3 . 131.08(19) yes
Co1 4_566 C4 . C1 4_566 62.90(14) yes
C3 . C4 . C1 4_566 142.9(3) yes
Co1 4_566 C4 . C4 4_566 71.7(2) yes
C3 . C4 . C4 4_566 108.5(3) yes
C1 4_566 C4 . C4 4_566 108.6(3) yes
Co1 4_566 C4 . Co1 . 143.42(13) yes
C3 . C4 . Co1 . 62.73(14) yes
C1 4_566 C4 . Co1 . 131.01(18) yes
C4 4_566 C4 . Co1 . 71.75(19) yes
C1 . C5 . H513 . 110.0 no
C1 . C5 . H512 . 108.9 no
H513 . C5 . H512 . 109.3 no
C1 . C5 . H511 . 109.2 no
H513 . C5 . H511 . 109.8 no
H512 . C5 . H511 . 109.7 no
C2 . C6 . H83 . 109.0 no
C2 . C6 . H82 . 109.9 no
H83 . C6 . H82 . 109.3 no
C2 . C6 . H81 . 109.1 no
H83 . C6 . H81 . 110.1 no
H82 . C6 . H81 . 109.4 no
C3 . C7 . H73 . 109.5 no
C3 . C7 . H72 . 109.9 no
H73 . C7 . H72 . 108.6 no
C3 . C7 . H71 . 110.2 no
H73 . C7 . H71 . 108.4 no
H72 . C7 . H71 . 110.2 no
C9 . C8 . C12 . 108.6(3) yes
C9 . C8 . C13 . 125.9(3) yes
C12 . C8 . C13 . 125.3(3) yes
C9 . C8 . Co1 . 71.61(17) yes
C12 . C8 . Co1 . 70.88(17) yes
C13 . C8 . Co1 . 126.8(2) yes
C8 . C9 . C10 . 107.8(3) yes
C8 . C9 . C14 . 126.7(3) yes
C10 . C9 . C14 . 125.5(3) yes
C8 . C9 . Co1 . 68.14(16) yes
C10 . C9 . Co1 . 70.04(17) yes
C14 . C9 . Co1 . 127.3(2) yes
C9 . C10 . C11 . 108.0(3) yes
C9 . C10 . C15 . 126.7(3) yes
C11 . C10 . C15 . 125.2(3) yes
C9 . C10 . Co1 . 70.90(17) yes
C11 . C10 . Co1 . 68.71(16) yes
C15 . C10 . Co1 . 127.9(2) yes
C10 . C11 . C12 . 108.2(3) yes
C10 . C11 . C16 . 125.5(3) yes
C12 . C11 . C16 . 126.2(3) yes
C10 . C11 . Co1 . 70.67(16) yes
C12 . C11 . Co1 . 70.72(16) yes
C16 . C11 . Co1 . 126.8(2) yes
C8 . C12 . C11 . 107.3(3) yes
C8 . C12 . C17 . 126.8(3) yes
C11 . C12 . C17 . 125.9(3) yes
C8 . C12 . Co1 . 68.91(16) yes
C11 . C12 . Co1 . 69.40(16) yes
C17 . C12 . Co1 . 126.4(2) yes
C8 . C13 . H163 . 109.6 no
C8 . C13 . H162 . 108.1 no
H163 . C13 . H162 . 108.4 no
C8 . C13 . H161 . 109.4 no
H163 . C13 . H161 . 112.0 no
H162 . C13 . H161 . 109.3 no
C9 . C14 . H153 . 109.6 no
C9 . C14 . H152 . 109.3 no
H153 . C14 . H152 . 109.3 no
C9 . C14 . H151 . 108.3 no
H153 . C14 . H151 . 111.0 no
H152 . C14 . H151 . 109.4 no
C10 . C15 . H143 . 109.6 no
C10 . C15 . H142 . 109.6 no
H143 . C15 . H142 . 108.7 no
C10 . C15 . H141 . 109.5 no
H143 . C15 . H141 . 110.2 no
H142 . C15 . H141 . 109.3 no
C11 . C16 . H183 . 110.4 no
C11 . C16 . H182 . 109.0 no
H183 . C16 . H182 . 109.1 no
C11 . C16 . H181 . 109.3 no
H183 . C16 . H181 . 110.0 no
H182 . C16 . H181 . 109.1 no
C12 . C17 . H173 . 108.9 no
C12 . C17 . H172 . 108.9 no
H173 . C17 . H172 . 108.7 no
C12 . C17 . H171 . 110.1 no
H173 . C17 . H171 . 111.0 no
H172 . C17 . H171 . 109.3 no
C4 . Co1 . C4 4_566 36.58(13) yes
C4 . Co1 . C9 . 176.44(10) yes
C4 4_566 Co1 . C9 . 146.09(11) yes
C4 . Co1 . C10 . 137.90(11) yes
C4 4_566 Co1 . C10 . 171.81(10) yes
C9 . Co1 . C10 . 39.06(12) yes
C4 . Co1 . C12 . 110.37(10) yes
C4 4_566 Co1 . C12 . 107.42(10) yes
C9 . Co1 . C12 . 67.28(11) yes
C10 . Co1 . C12 . 67.37(11) yes
C4 . Co1 . C11 . 109.42(10) yes
C4 4_566 Co1 . C11 . 131.40(10) yes
C9 . Co1 . C11 . 67.04(11) yes
C10 . Co1 . C11 . 40.62(11) yes
C12 . Co1 . C11 . 39.88(12) yes
C4 . Co1 . C1 . 64.87(10) yes
C4 4_566 Co1 . C1 . 38.56(9) yes
C9 . Co1 . C1 . 118.68(11) yes
C10 . Co1 . C1 . 149.59(11) yes
C12 . Co1 . C1 . 131.40(11) yes
C4 . Co1 . C8 . 139.45(11) yes
C4 4_566 Co1 . C8 . 113.54(11) yes
C9 . Co1 . C8 . 40.25(12) yes
C10 . Co1 . C8 . 67.00(13) yes
C12 . Co1 . C8 . 40.21(12) yes
C4 . Co1 . C3 . 38.73(9) yes
C4 4_566 Co1 . C3 . 64.98(10) yes
C9 . Co1 . C3 . 141.55(11) yes
C10 . Co1 . C3 . 114.30(12) yes
C12 . Co1 . C3 . 138.69(11) yes
C4 . Co1 . C2 . 65.60(10) yes
C4 4_566 Co1 . C2 . 65.49(10) yes
C9 . Co1 . C2 . 117.05(11) yes
C10 . Co1 . C2 . 119.94(11) yes
C12 . Co1 . C2 . 172.56(11) yes
C11 . Co1 . C1 . 168.93(11) yes
C11 . Co1 . C8 . 67.35(13) yes
C1 . Co1 . C8 . 110.21(12) yes
C11 . Co1 . C3 . 112.68(11) yes
C1 . Co1 . C3 . 69.39(10) yes
C8 . Co1 . C3 . 178.18(12) yes
C11 . Co1 . C2 . 146.55(12) yes
C1 . Co1 . C2 . 41.57(11) yes
C8 . Co1 . C2 . 139.07(12) yes
C3 . Co1 . C2 . 41.72(10) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 10/02/15 at 19:44:05
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   5,X'S) H   ( 513,X'S) H   ( 512,X'S) H   ( 511,X'S) 
RIDE C   (   6,X'S) H   (  83,X'S) H   (  82,X'S) H   (  81,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   ( 163,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  14,X'S) H   ( 153,X'S) H   ( 152,X'S) H   ( 151,X'S) 
RIDE C   (  15,X'S) H   ( 143,X'S) H   ( 142,X'S) H   ( 141,X'S) 
RIDE C   (  16,X'S) H   ( 183,X'S) H   ( 182,X'S) H   ( 181,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 10/02/15 at 19:44:05
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5-044scb14
_database_code_depnum_ccdc_archive 'CCDC 1886443'
loop_
_audit_author_name
_audit_author_address
'Samantha C. Binding'
;University of Oxford
United Kingdom
;
_audit_update_record             
;
2018-12-20 deposited with the CCDC.	2019-02-27 downloaded from the CCDC.
;
_audit_creation_date             2014-06-02
_audit_creation_method           CRYSTALS_ver_14.43

_oxford_structure_analysis_title '044scb14 At 18:16 on 2/ 6'
_chemical_name_systematic        bis(cyclopentadienylnickel)pentalenyl
_chemical_melting_point          'not measured'

_cell_length_a                   7.6274(4)
_cell_length_b                   8.2173(4)
_cell_length_c                   9.6561(7)
_cell_angle_alpha                68.600(3)
_cell_angle_beta                 87.710(3)
_cell_angle_gamma                62.426(4)
_cell_volume                     493.35(5)

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1 '
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z

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
Ni 0.3393 1.1124 12.8376 3.8785 7.2920 0.2565 4.4438 12.1763 2.3800 66.3421
1.0341 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
C 0.0033 0.0016 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'


_cell_formula_units_Z            1

# Given Formula = C24 H28 Ni2 
# Dc =      1.46 Fooo =    228.00 Mu =     19.12 M =    216.95
# Found Formula = C24 H28 Ni2 
# Dc =      1.46 FOOO =    228.00 Mu =     19.12 M =    216.95

_chemical_formula_sum            'C24 H28 Ni2'
_chemical_formula_moiety         'C24 H28 Ni2'
_chemical_compound_source        SYN
_chemical_formula_weight         433.91


_cell_measurement_reflns_used    1880
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            'brown black'
_exptl_crystal_size_min          0.10
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_max          0.16

_exptl_crystal_density_diffrn    1.460
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             228
_exptl_absorpt_coefficient_mu    1.912

# Sheldrick geometric approximatio 0.74 0.83 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.74
_exptl_absorpt_correction_T_max  0.83
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

# If a reference occurs more than once, delete the author 
# and date from subsequent references. 
_computing_data_collection       'COLLECT (Nonius, 2001).'
_computing_cell_refinement       'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_data_reduction        'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_computing_structure_solution    'SIR92 (Altomare et al., 1994)'
_computing_structure_refinement  'CRYSTALS (Betteridge et al., 2003)'
_computing_publication_material  'CRYSTALS (Betteridge et al., 2003)'
_computing_molecular_graphics    'CAMERON (Watkin et al., 1996)'

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            6788
_reflns_number_total             2245
_diffrn_reflns_av_R_equivalents  0.029
# Number of reflections without Friedels Law is 3707 
# Number of reflections with Friedels Law is 2245 
# Theoretical number of reflections is about 2355 


_diffrn_reflns_theta_min         5.246
_diffrn_reflns_theta_max         27.516
_diffrn_measured_fraction_theta_max 0.986

_diffrn_reflns_theta_full        25.039
_diffrn_measured_fraction_theta_full 0.991


_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_reflns_limit_h_min              -9
_reflns_limit_h_max              9
_reflns_limit_k_min              -9
_reflns_limit_k_max              10
_reflns_limit_l_min              0
_reflns_limit_l_max              12

_oxford_diffrn_Wilson_B_factor   2.66
_oxford_diffrn_Wilson_scale      0.33

_atom_sites_solution_primary     direct #heavy,direct,difmap,geom
# _atom_sites_solution_secondary  difmap
_atom_sites_solution_hydrogens   difmap

_refine_diff_density_min         -0.64
_refine_diff_density_max         0.87


# The current dictionary definitions do not cover the 
# situation where the reflections used for refinement were 
# selected by a user-defined sigma threshold 


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2245
_refine_ls_number_restraints     0
_refine_ls_number_parameters     119
_oxford_refine_ls_R_factor_ref   0.0441
_refine_ls_wR_factor_ref         0.1017
_refine_ls_goodness_of_fit_ref   0.8807
_refine_ls_shift/su_max          0.0007542
_refine_ls_shift/su_mean         0.0000170


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        2245
_refine_ls_R_factor_all          0.0441
_refine_ls_wR_factor_all         0.1017

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                2099
_refine_ls_R_factor_gt           0.0403
_refine_ls_wR_factor_gt          0.0984

# choose from: rm (reference molecule of known chirality), 
# ad (anomolous dispersion - Flack), rmad (rm and ad), 
# syn (from synthesis), unk (unknown) or . (not applicable). 
_chemical_absolute_configuration .


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method, part 1, Chebychev polynomial, (Watkin, 1994, Prince, 1982) 
 [weight] = 1.0/[A₀*T₀(x)+A₁*T₁(x) ... +Aₙ₋₁]*Tₙ₋₁(x)] 
 where Ai are the Chebychev coefficients listed below and x= Fcalc/Fmax 
 Method = Robust Weighting (Prince, 1982) 
 W = [weight] * [1-(deltaF/6*sigmaF)²]² 
 Ai are: 
 101. 162. 98.0 40.8 9.70 
;

# Uequiv = arithmetic mean of Ui i.e. Ueqiv = (U1+U2+U3)/3

# Replace last . with number of unfound hydrogen atoms attached to an atom.

# ..._refinement_flags_... 
# . no refinement constraints           S special position constraint on site
# G rigid group refinement of site      R riding atom
# D distance or angle restraint on site T thermal displacement constraints
# U Uiso or Uij restraint (rigid bond)  P partial occupancy constraint


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
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
C1 C 0.5099(4) -0.1041(4) 0.8646(3) 0.0341 1.0000 Uani . . . . . .
C2 C 0.3737(4) 0.0990(4) 0.7668(3) 0.0351 1.0000 Uani . . . . . .
C3 C 0.3408(4) 0.2278(4) 0.8456(3) 0.0342 1.0000 Uani . . . . . .
C4 C 0.4475(4) 0.1037(4) 0.9941(3) 0.0321 1.0000 Uani . . . . . .
C5 C 0.5718(5) -0.2839(5) 0.8273(4) 0.0466 1.0000 Uani . . . . . .
C6 C 0.2688(5) 0.1643(6) 0.6131(4) 0.0450 1.0000 Uani . . . . . .
C7 C 0.1981(5) 0.4476(4) 0.7870(4) 0.0455 1.0000 Uani . . . . . .
C8 C 0.8872(5) -0.0121(5) 0.6714(4) 0.0406 1.0000 Uani . . . . . .
C9 C 0.7473(4) 0.1855(5) 0.5801(3) 0.0358 1.0000 Uani . . . . . .
C10 C 0.7275(5) 0.3099(5) 0.6560(4) 0.0434 1.0000 Uani . . . . . .
C11 C 0.8529(6) 0.1864(7) 0.7963(4) 0.0552 1.0000 Uani . . . . . .
C12 C 0.9500(5) -0.0113(6) 0.8056(4) 0.0528 1.0000 Uani . . . . . .
Ni1 Ni 0.63604(5) 0.09256(5) 0.79090(4) 0.0319 1.0000 Uani . . . . . .
H51 H 0.6994 -0.3934 0.8879 0.0733 1.0000 Uiso R . . . . .
H53 H 0.5841 -0.2514 0.7221 0.0731 1.0000 Uiso R . . . . .
H52 H 0.4697 -0.3233 0.8480 0.0732 1.0000 Uiso R . . . . .
H61 H 0.2373 0.3012 0.5557 0.0658 1.0000 Uiso R . . . . .
H63 H 0.3544 0.0770 0.5646 0.0660 1.0000 Uiso R . . . . .
H62 H 0.1459 0.1579 0.6234 0.0662 1.0000 Uiso R . . . . .
H71 H 0.2555 0.5129 0.8192 0.0701 1.0000 Uiso R . . . . .
H72 H 0.1738 0.5015 0.6777 0.0701 1.0000 Uiso R . . . . .
H73 H 0.0735 0.4741 0.8242 0.0703 1.0000 Uiso R . . . . .
H81 H 0.9304 -0.1286 0.6455 0.0475 1.0000 Uiso R . . . . .
H91 H 0.6801 0.2309 0.4772 0.0425 1.0000 Uiso R . . . . .
H101 H 0.6436 0.4560 0.6184 0.0516 1.0000 Uiso R . . . . .
H111 H 0.8667 0.2315 0.8751 0.0652 1.0000 Uiso R . . . . .
H121 H 1.0492 -0.1291 0.8904 0.0624 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          1.711(14)

loop_
_oxford_twin_element_scale_factors
0.9370(18)
0.0630(18)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
C1 . C4 2_657 1.417(4) yes
C1 . C2 . 1.442(4) yes
C1 . C5 . 1.504(4) yes
C1 . Ni1 . 2.142(3) yes
C2 . C3 . 1.445(4) yes
C2 . C6 . 1.499(4) yes
C2 . Ni1 . 1.997(3) yes
C3 . C4 . 1.420(4) yes
C3 . C7 . 1.500(4) yes
C3 . Ni1 . 2.145(3) yes
C4 . Ni1 2_657 2.391(3) yes
C4 . C4 2_657 1.470(5) yes
C4 . Ni1 . 2.390(3) yes
C5 . H51 . 0.975 no
C5 . H53 . 0.964 no
C5 . H52 . 0.961 no
C6 . H61 . 0.967 no
C6 . H63 . 0.974 no
C6 . H62 . 0.962 no
C7 . H71 . 0.962 no
C7 . H72 . 0.971 no
C7 . H73 . 0.958 no
C8 . C9 . 1.407(4) yes
C8 . C12 . 1.402(5) yes
C8 . Ni1 . 2.183(3) yes
C8 . H81 . 0.982 no
C9 . C10 . 1.413(4) yes
C9 . Ni1 . 2.185(3) yes
C9 . H91 . 0.992 no
C10 . C11 . 1.408(5) yes
C10 . Ni1 . 2.180(3) yes
C10 . H101 . 0.986 no
C11 . C12 . 1.407(6) yes
C11 . Ni1 . 2.133(3) yes
C11 . H111 . 0.987 no
C12 . Ni1 . 2.128(3) yes
C12 . H121 . 0.987 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C4 2_657 C1 . C2 . 107.3(2) yes
C4 2_657 C1 . C5 . 126.9(3) yes
C2 . C1 . C5 . 125.3(3) yes
C4 2_657 C1 . Ni1 . 81.67(16) yes
C2 . C1 . Ni1 . 64.31(14) yes
C5 . C1 . Ni1 . 124.8(2) yes
C1 . C2 . C3 . 109.2(2) yes
C1 . C2 . C6 . 125.5(3) yes
C3 . C2 . C6 . 125.2(3) yes
C1 . C2 . Ni1 . 75.11(17) yes
C3 . C2 . Ni1 . 75.18(16) yes
C6 . C2 . Ni1 . 120.27(19) yes
C2 . C3 . C4 . 107.1(2) yes
C2 . C3 . C7 . 125.8(3) yes
C4 . C3 . C7 . 126.6(3) yes
C2 . C3 . Ni1 . 64.19(15) yes
C4 . C3 . Ni1 . 81.44(17) yes
C7 . C3 . Ni1 . 125.4(2) yes
Ni1 2_657 C4 . C4 2_657 72.1(2) yes
Ni1 2_657 C4 . C3 . 130.7(2) yes
C4 2_657 C4 . C3 . 108.1(3) yes
Ni1 2_657 C4 . C1 2_657 62.43(14) yes
C4 2_657 C4 . C1 2_657 108.2(3) yes
C3 . C4 . C1 2_657 143.7(2) yes
Ni1 2_657 C4 . Ni1 . 144.20(11) yes
C4 2_657 C4 . Ni1 . 72.14(19) yes
C3 . C4 . Ni1 . 62.56(14) yes
C1 2_657 C4 . Ni1 . 130.9(2) yes
C1 . C5 . H51 . 110.6 no
C1 . C5 . H53 . 110.2 no
H51 . C5 . H53 . 109.2 no
C1 . C5 . H52 . 108.2 no
H51 . C5 . H52 . 109.7 no
H53 . C5 . H52 . 108.9 no
C2 . C6 . H61 . 108.4 no
C2 . C6 . H63 . 109.6 no
H61 . C6 . H63 . 111.3 no
C2 . C6 . H62 . 108.6 no
H61 . C6 . H62 . 108.8 no
H63 . C6 . H62 . 110.1 no
C3 . C7 . H71 . 109.5 no
C3 . C7 . H72 . 109.4 no
H71 . C7 . H72 . 109.1 no
C3 . C7 . H73 . 111.1 no
H71 . C7 . H73 . 108.3 no
H72 . C7 . H73 . 109.4 no
C9 . C8 . C12 . 107.5(3) yes
C9 . C8 . Ni1 . 71.28(16) yes
C12 . C8 . Ni1 . 68.92(18) yes
C9 . C8 . H81 . 125.7 no
C12 . C8 . H81 . 126.8 no
Ni1 . C8 . H81 . 124.4 no
C8 . C9 . C10 . 108.6(3) yes
C8 . C9 . Ni1 . 71.14(16) yes
C10 . C9 . Ni1 . 70.95(16) yes
C8 . C9 . H91 . 125.6 no
C10 . C9 . H91 . 125.7 no
Ni1 . C9 . H91 . 126.6 no
C9 . C10 . C11 . 107.2(3) yes
C9 . C10 . Ni1 . 71.27(16) yes
C11 . C10 . Ni1 . 69.13(18) yes
C9 . C10 . H101 . 127.1 no
C11 . C10 . H101 . 125.7 no
Ni1 . C10 . H101 . 125.4 no
C10 . C11 . C12 . 108.2(3) yes
C10 . C11 . Ni1 . 72.79(18) yes
C12 . C11 . Ni1 . 70.5(2) yes
C10 . C11 . H111 . 125.4 no
C12 . C11 . H111 . 126.4 no
Ni1 . C11 . H111 . 121.3 no
C11 . C12 . C8 . 108.5(3) yes
C11 . C12 . Ni1 . 70.9(2) yes
C8 . C12 . Ni1 . 73.15(18) yes
C11 . C12 . H121 . 125.9 no
C8 . C12 . H121 . 125.6 no
Ni1 . C12 . H121 . 123.5 no
C4 . Ni1 . C4 2_657 35.80(11) yes
C4 . Ni1 . C9 . 161.61(10) yes
C4 2_657 Ni1 . C9 . 161.62(10) yes
C4 . Ni1 . C8 . 159.40(11) yes
C4 2_657 Ni1 . C8 . 127.68(10) yes
C9 . Ni1 . C8 . 37.58(11) yes
C4 . Ni1 . C10 . 127.76(10) yes
C4 2_657 Ni1 . C10 . 158.91(12) yes
C9 . Ni1 . C10 . 37.79(12) yes
C8 . Ni1 . C10 . 63.34(11) yes
C4 . Ni1 . C3 . 35.99(11) yes
C4 2_657 Ni1 . C3 . 61.82(10) yes
C9 . Ni1 . C3 . 129.37(11) yes
C8 . Ni1 . C3 . 163.40(12) yes
C10 . Ni1 . C3 . 113.01(11) yes
C4 . Ni1 . C1 . 61.82(9) yes
C4 2_657 Ni1 . C1 . 35.90(10) yes
C9 . Ni1 . C1 . 129.43(11) yes
C8 . Ni1 . C1 . 112.23(11) yes
C10 . Ni1 . C1 . 164.39(13) yes
C4 . Ni1 . C11 . 112.72(12) yes
C4 2_657 Ni1 . C11 . 125.48(13) yes
C9 . Ni1 . C11 . 63.45(12) yes
C8 . Ni1 . C11 . 63.76(14) yes
C10 . Ni1 . C11 . 38.08(15) yes
C4 . Ni1 . C12 . 126.17(12) yes
C4 2_657 Ni1 . C12 . 112.24(12) yes
C9 . Ni1 . C12 . 63.34(12) yes
C8 . Ni1 . C12 . 37.93(14) yes
C10 . Ni1 . C12 . 63.88(14) yes
C4 . Ni1 . C2 . 62.65(11) yes
C4 2_657 Ni1 . C2 . 62.56(11) yes
C9 . Ni1 . C2 . 114.65(11) yes
C8 . Ni1 . C2 . 127.31(12) yes
C10 . Ni1 . C2 . 128.54(13) yes
C3 . Ni1 . C1 . 66.56(10) yes
C3 . Ni1 . C11 . 124.52(14) yes
C1 . Ni1 . C11 . 155.75(15) yes
C3 . Ni1 . C12 . 157.37(15) yes
C1 . Ni1 . C12 . 122.91(14) yes
C11 . Ni1 . C12 . 38.57(16) yes
C3 . Ni1 . C2 . 40.63(11) yes
C1 . Ni1 . C2 . 40.59(11) yes
C11 . Ni1 . C2 . 161.39(16) yes
C12 . Ni1 . C2 . 159.37(15) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 02/06/14 at 18:23:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
SUMFIX ELEMENT SCALES 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  53,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  61,X'S) H   (  63,X'S) H   (  62,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) H   (  73,X'S) 
RIDE C   (   8,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) 
RIDE C   (  12,X'S) H   ( 121,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 02/06/14 at 18:23:57
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;


#===END
