# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2021

####################################################################### 
# 
# 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_JGD-1021-1-19
_database_code_depnum_ccdc_archive 'CCDC 2069077'
loop_
_audit_author_name
_audit_author_address
'Peter Stephens'
;Stony Brook University
United States of America
;
_audit_update_record             
;
2021-03-09 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
Decamethylferrocenium 7,7,8,8-Tetracyano-p-quinodimethanide
;
_chemical_name_common            ?
_chemical_formula_moiety         'C20 H30 Fe, C12 H4 N4'
_chemical_formula_structural     'Fe (C5 (CH3)5)2 C12 H4 N4'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C32 H34 Fe N4'
_chemical_formula_weight         530.48

_exptl_crystal_description       powder

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 21/n'
_symmetry_Int_Tables_number      14

loop_
_space_group_symop_id
_space_group_symop_operation_xyz
1 x,y,z
2 1/2-x,1/2+y,1/2-z
3 -x,-y,-z
4 1/2+x,1/2-y,1/2+z

_cell_length_a                   10.7383(20)
_cell_length_b                   30.81546(60)
_cell_length_c                   8.53463(20)
_cell_angle_alpha                90
_cell_angle_beta                 103.2516(200)
_cell_angle_gamma                90
_cell_volume                     2749.0(10)
_cell_formula_units_Z            4
_cell_measurement_temperature    19 #Kelvin

_cell_special_details            
; ?
;

_pd_spec_mount_mode              transmission
_pd_spec_size_axial              10 #millimeters
_pd_spec_size_equat              1 #mm
_pd_spec_size_thick              1 #mm
_pd_spec_shape                   capillary
_exptl_absorpt_correction_type   none

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
;
capillary
;
_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions



#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; Ferromagnetic polymorph, 19 K
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
;
X16C, National Synchrotron Light Source, Brookhaven National Laboratory
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
NIST standard reference material 1976(sintered plate of Al2O3)
Seven well-isolated reflections were used to calibrate wavelength and detector zero.
;

_diffrn_ambient_temperature      19 #Kelvin
_diffrn_source                   synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Huber diffractometer'
_diffrn_detector                 'NaI scintillation counter'
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  Cryostat rocked 5 or 10 degrees at each point.
;

_diffrn_radiation_wavelength     0.700085
_diffrn_radiation_monochromator  'Si(111) channel cut'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        5601
_pd_meas_2theta_range_min        2.002
_pd_meas_2theta_range_max        30.002
_pd_meas_2theta_range_inc        0.005


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
;
_refine_ls_hydrogen_treatment    noref

# The next three items are given as text.

_pd_proc_ls_profile_function     
;
Simple_Axial_model function with Rp=9999,Rs=330 in TOPAS-Academic
Anisotropic strain broadening per Stephens J.Appl.Cryst.(1999).
;
_pd_proc_ls_background_function  
;
4 Pearson-Voight peaks and Chebyshev polynomial with 11 coefficients
;
_pd_proc_ls_pref_orient_corr     
;
none
;

_pd_proc_ls_prof_R_factor        0.0546
_pd_proc_ls_prof_wR_factor       0.0703
_pd_proc_ls_prof_wR_expected     0.0257
_refine_ls_R_I_factor            0.0301
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?

_refine_special_details          
; 
Molecules are defined as rigid bodies using the z-matrix function 
implemented in TOPAS-Academic. 
The same isotropic displacement parameters are assigned atoms by groups 
in each molecule.  
TCNQ is restrained to have mmm symmetry
Cp* groups are planar, 5 symmetry, parallel and equidistant from Fe.
;

_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     sigma^-2
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     68
_refine_ls_number_restraints     4
_refine_ls_number_constraints    105

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   2.738

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.002
_pd_proc_2theta_range_max        30.002
_pd_proc_2theta_range_inc        0.003
_pd_proc_wavelength              0.700085


_pd_block_diffractogram_id       JGD-1021-1-19
# The id used for the block containing
# the powder pattern profile (section 11).

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       SPEC
_computing_cell_refinement       TOPAS-Academic
_computing_data_reduction        TOPAS-Academic
_computing_structure_solution    TOPAS-Academic
_computing_structure_refinement  TOPAS-Academic
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material  Platon


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_thermal_displace_type
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv
Fe1 Fe Uiso 0.73295(240) 0.63415(70) 0.86815(400) 1.000 1.45(15)
C1 C Uiso 0.5758(24) 0.5911(7) 0.868(4) 1.000 1.84(35)
C2 C Uiso 0.5695(24) 0.6292(7) 0.972(4) 1.000 1.84(35)
C3 C Uiso 0.5599(24) 0.6687(7) 0.871(4) 1.000 1.84(35)
C4 C Uiso 0.5603(24) 0.6550(7) 0.704(4) 1.000 1.84(35)
C5 C Uiso 0.5701(24) 0.6070(7) 0.703(4) 1.000 1.84(35)
C6 C Uiso 0.5851(24) 0.5504(7) 0.932(4) 1.000 1.55(18)
C7 C Uiso 0.5711(24) 0.6327(7) 1.131(4) 1.000 1.55(18)
C8 C Uiso 0.5516(24) 0.7115(7) 0.905(4) 1.000 1.55(18)
C9 C Uiso 0.5535(24) 0.6779(7) 0.567(4) 1.000 1.55(18)
C10 C Uiso 0.5742(24) 0.5784(7) 0.583(4) 1.000 1.55(18)
C11 C Uiso 0.9010(24) 0.6373(7) 1.060(4) 1.000 1.55(18)
C12 C Uiso 0.9074(24) 0.5990(7) 0.957(4) 1.000 1.55(18)
C13 C Uiso 0.9017(24) 0.6146(7) 0.792(4) 1.000 1.55(18)
C14 C Uiso 0.8919(24) 0.6626(7) 0.792(4) 1.000 1.55(18)
C15 C Uiso 0.8915(24) 0.6766(7) 0.958(4) 1.000 1.55(18)
C16 C Uiso 0.9045(24) 0.6320(7) 1.219(4) 1.000 1.55(18)
C17 C Uiso 0.9167(24) 0.5558(7) 0.990(4) 1.000 1.55(18)
C18 C Uiso 0.9041(24) 0.5933(7) 0.653(4) 1.000 1.55(18)
C19 C Uiso 0.8840(24) 0.6926(7) 0.673(4) 1.000 1.55(18)
C20 C Uiso 0.8843(24) 0.7165(7) 1.023(4) 1.000 1.55(18)
N1 N Uiso 0.28895(240) 0.26249(70) 0.6914(40) 1.000 1.55(18)
N2 N Uiso 0.27713(240) 0.18055(70) 0.2659(40) 1.000 1.55(18)
N3 N Uiso 0.25299(240) -0.03554(70) 0.8069(40) 1.000 1.55(18)
N4 N Uiso 0.26480(240) 0.04640(70) 1.2324(40) 1.000 1.55(18)
C21 C Uiso 0.2751(24) 0.1503(7) 0.656(4) 1.000 1.55(18)
C22 C Uiso 0.2763(24) 0.1543(7) 0.819(4) 1.000 1.55(18)
C23 C Uiso 0.2721(24) 0.1174(7) 0.911(4) 1.000 1.55(18)
C24 C Uiso 0.2668(24) 0.0765(7) 0.841(4) 1.000 1.55(18)
C25 C Uiso 0.2657(24) 0.0726(7) 0.678(4) 1.000 1.55(18)
C26 C Uiso 0.2698(24) 0.1095(7) 0.586(4) 1.000 1.55(18)
C27 C Uiso 0.2793(24) 0.1878(7) 0.563(4) 1.000 1.55(18)
C28 C Uiso 0.2845(24) 0.2277(7) 0.631(4) 1.000 1.55(18)
C29 C Uiso 0.2781(24) 0.1839(7) 0.404(4) 1.000 1.55(18)
C30 C Uiso 0.2627(24) 0.0391(7) 0.935(4) 1.000 1.55(18)
C31 C Uiso 0.2575(24) -0.0008(7) 0.8666(4) 1.000 1.55(18)
C32 C Uiso 0.2638(24) 0.0430(7) 1.0943(4) 1.000 1.55(18)
H6A H Uiso 0.5874 0.5467 1.0374 1.000 1.55(18)
H6B H Uiso 0.5241 0.5306 0.8940 1.000 1.55(18)
H6C H Uiso 0.6529 0.5337 0.9283 1.000 1.55(18)
H7A H Uiso 0.5664 0.6590 1.1755 1.000 1.55(18)
H7B H Uiso 0.5099 0.6198 1.1715 1.000 1.55(18)
H7C H Uiso 0.6388 0.6228 1.2058 1.000 1.55(18)
H8A H Uiso 0.5464 0.7315 0.8278 1.000 1.55(18)
H8B H Uiso 0.4857 0.7212 0.9450 1.000 1.55(18)
H8C H Uiso 0.6146 0.7243 0.9793 1.000 1.55(18)
H9A H Uiso 0.5550 0.6640 0.4748 1.000 1.55(18)
H9B H Uiso 0.4850 0.6947 0.5276 1.000 1.55(18)
H9C H Uiso 0.6138 0.6978 0.5618 1.000 1.55(18)
H10A H Uiso 0.5804 0.5497 0.6043 1.000 1.55(18)
H10B H Uiso 0.5087 0.5769 0.4961 1.000 1.55(18)
H10C H Uiso 0.6375 0.5800 0.5304 1.000 1.55(18)
H16A H Uiso 0.9106 0.6051 1.2625 1.000 1.55(18)
H16B H Uiso 0.9675 0.6442 1.2943 1.000 1.55(18)
H16C H Uiso 0.8387 0.6412 1.2600 1.000 1.55(18)
H17A H Uiso 0.9195 0.5367 0.9118 1.000 1.55(18)
H17B H Uiso 0.9844 0.5454 1.0636 1.000 1.55(18)
H17C H Uiso 0.8556 0.5424 1.0293 1.000 1.55(18)
H18A H Uiso 0.8996 0.6083 0.5617 1.000 1.55(18)
H18B H Uiso 0.9718 0.5767 0.6474 1.000 1.55(18)
H18C H Uiso 0.8430 0.5737 0.6131 1.000 1.55(18)
H19A H Uiso 0.8785 0.7210 0.6961 1.000 1.55(18)
H19B H Uiso 0.9472 0.6948 0.6209 1.000 1.55(18)
H19C H Uiso 0.8184 0.6918 0.5866 1.000 1.55(18)
H20A H Uiso 0.8853 0.7191 1.1292 1.000 1.55(18)
H20B H Uiso 0.9446 0.7366 1.0208 1.000 1.55(18)
H20C H Uiso 0.8157 0.7335 0.9865 1.000 1.55(18)
H22 H Uiso 0.2797 0.1808 0.8648 1.000 1.55(18)
H23 H Uiso 0.2729 0.1200 1.0170 1.000 1.55(18)
H25 H Uiso 0.2622 0.0461 0.6335 1.000 1.55(18)
H26 H Uiso 0.2690 0.1069 0.4813 1.000 1.55(18)


#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 This is somewhat meaningless, since the geometries were modeled as rigid bodies.
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.14(3) . . yes
Fe1 C15 2.15(3) . . yes
C1 C2 1.48(4) . . no
C1 C6 1.36(3) . . no
C2 C3 1.48(4) . . no
C2 C7 1.36(5) . . no
N1 C28 1.18(3) . . yes
C21 C22 1.39(5) . . no
C21 C27 1.41(4) . . no
C27 C28 1.36(3) . . no
C22 H22 0.9000 . . no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 40.5(11) . . . yes
C1 Fe1 C3 68.0(11) . . . yes
C1 Fe1 C4 67.9(12) . . . yes
C1 Fe1 C5 40.3(13) . . . yes
C1 Fe1 C11 123.5(18) . . . yes
C1 Fe1 C12 108.1(13) . . . yes
C1 Fe1 C13 123.1(14) . . . yes
C1 Fe1 C14 158.7(19) . . . yes
C1 Fe1 C15 160(2) . . . yes
C2 C1 C5 108 . . . no
C22 C21 C26 120 . . . no
C22 C21 C27 120 . . . no
N2 C29 C27 180 . . . yes
_exptl_crystal_colour            purple
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_jsm197
_database_code_depnum_ccdc_archive 'CCDC 2069829'
loop_
_audit_author_name
_audit_author_address
'Arnold L. Rheingold'
;Department of Chemistry and Biochemistry, University of California, San Diego
United States of America
;
_audit_update_record             
;
2021-03-11 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;
_audit_creation_date             2015-06-24
_audit_creation_method           
;
Olex2 1.2
(compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998)
;
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C20 H30 Fe, C12 H4 N4'
_chemical_formula_sum            'C32 H34 Fe N4'
_chemical_formula_weight         530.48
_chemical_melting_point          ?
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_H-M_alt        'P -1'
_space_group_name_Hall           '-P 1'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   9.8228(12)
_cell_length_b                   10.2621(14)
_cell_length_c                   16.5194(19)
_cell_angle_alpha                103.762(3)
_cell_angle_beta                 92.367(4)
_cell_angle_gamma                116.138(3)
_cell_volume                     1431.5(3)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3500
_cell_measurement_temperature    300.15
_cell_measurement_theta_max      24.45
_cell_measurement_theta_min      2.30
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.553
_exptl_absorpt_correction_T_max  0.312
_exptl_absorpt_correction_T_min  0.226
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   ?
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.231
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             560
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.13
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0201
_diffrn_reflns_av_unetI/netI     0.0333
_diffrn_reflns_Laue_measured_fraction_full 0.960
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            10835
_diffrn_reflns_point_group_measured_fraction_full 0.960
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.388
_diffrn_reflns_theta_min         2.601
_diffrn_ambient_temperature      300.15
_diffrn_detector                 'Bruker APEX-II CCD'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD Area Detector'
_diffrn_measured_fraction_theta_full 0.960
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device       'Kappa Four-Circle Diffractometer'
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       'φ and ω scans'
_diffrn_radiation_monochromator  'Double Bounce Multilayer Mirrors'
_diffrn_radiation_probe          X-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'Micro Focus Rotating Anode'
_diffrn_source_type              'Bruker TXS'
_diffrn_standards_number         0
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4532
_reflns_number_total             5558
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       ?
_computing_data_collection       ?
_computing_data_reduction        ?
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.370
_refine_diff_density_min         -0.221
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.022
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     344
_refine_ls_number_reflns         5558
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0645
_refine_ls_R_factor_gt           0.0500
_refine_ls_restrained_S_all      1.022
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0733P)²+0.5640P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1365
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C22(H22), C23(H23), C25(H25), C26(H26)
2.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C10(H10A,
 H10B,H10C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C),
 C19(H19A,H19B,H19C), C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.02588(4) 0.24137(4) 0.26211(2) 0.03927(14) Uani 1 1 d . . . . .
N1 N 0.6349(5) 0.4189(5) 1.0668(2) 0.1088(13) Uani 1 1 d . . . . .
N2 N 0.8042(5) 0.1171(5) 0.9348(2) 0.1161(14) Uani 1 1 d . . . . .
N3 N 0.2174(5) 0.3839(5) 0.6112(2) 0.1022(11) Uani 1 1 d . . . . .
N4 N 0.3922(4) 0.0938(4) 0.4688(2) 0.0962(10) Uani 1 1 d . . . . .
C1 C 0.1610(4) 0.4737(3) 0.3169(2) 0.0638(8) Uani 1 1 d . . . . .
C2 C 0.1104(3) 0.4464(3) 0.2314(2) 0.0636(8) Uani 1 1 d . . . . .
C3 C 0.1701(4) 0.3532(4) 0.18542(18) 0.0726(10) Uani 1 1 d . . . . .
C4 C 0.2553(4) 0.3283(4) 0.2440(3) 0.0752(10) Uani 1 1 d . . . . .
C5 C 0.2490(3) 0.4016(4) 0.3242(2) 0.0693(9) Uani 1 1 d . . . . .
C6 C 0.1335(7) 0.5728(5) 0.3909(4) 0.180(4) Uani 1 1 d . . . . .
H6A H 0.2273 0.6647 0.4150 0.270 Uiso 1 1 calc GR . . . .
H6B H 0.0998 0.5201 0.4328 0.270 Uiso 1 1 calc GR . . . .
H6C H 0.0559 0.5968 0.3719 0.270 Uiso 1 1 calc GR . . . .
C7 C 0.0158(5) 0.5091(6) 0.1965(5) 0.187(4) Uani 1 1 d . . . . .
H7A H 0.0801 0.6137 0.2004 0.281 Uiso 1 1 calc GR . . . .
H7B H -0.0655 0.5008 0.2286 0.281 Uiso 1 1 calc GR . . . .
H7C H -0.0275 0.4529 0.1385 0.281 Uiso 1 1 calc GR . . . .
C8 C 0.1504(8) 0.2994(6) 0.0906(3) 0.203(4) Uani 1 1 d . . . . .
H8A H 0.2344 0.3710 0.0713 0.305 Uiso 1 1 calc GR . . . .
H8B H 0.0553 0.2903 0.0660 0.305 Uiso 1 1 calc GR . . . .
H8C H 0.1491 0.2026 0.0741 0.305 Uiso 1 1 calc GR . . . .
C9 C 0.3456(6) 0.2414(6) 0.2217(6) 0.214(5) Uani 1 1 d . . . . .
H9A H 0.4474 0.3091 0.2157 0.321 Uiso 1 1 calc GR . . . .
H9B H 0.2949 0.1628 0.1695 0.321 Uiso 1 1 calc GR . . . .
H9C H 0.3519 0.1970 0.2659 0.321 Uiso 1 1 calc GR . . . .
C10 C 0.3297(6) 0.4054(7) 0.4051(4) 0.196(4) Uani 1 1 d . . . . .
H10A H 0.4379 0.4718 0.4120 0.294 Uiso 1 1 calc GR . . . .
H10B H 0.3138 0.3052 0.4028 0.294 Uiso 1 1 calc GR . . . .
H10C H 0.2889 0.4415 0.4521 0.294 Uiso 1 1 calc GR . . . .
C11 C -0.1393(3) 0.0228(3) 0.19283(17) 0.0536(7) Uani 1 1 d . . . . .
C12 C -0.0632(3) 0.0160(3) 0.2648(2) 0.0581(7) Uani 1 1 d . . . . .
C13 C -0.0882(3) 0.1029(3) 0.33766(18) 0.0609(8) Uani 1 1 d . . . . .
C14 C -0.1811(3) 0.1615(3) 0.3096(2) 0.0594(8) Uani 1 1 d . . . . .
C15 C -0.2122(3) 0.1126(3) 0.22061(19) 0.0536(7) Uani 1 1 d . . . . .
C16 C -0.1479(5) -0.0602(4) 0.1027(2) 0.0864(12) Uani 1 1 d . . . . .
H16A H -0.2292 -0.1622 0.0895 0.130 Uiso 1 1 calc GR . . . .
H16B H -0.0519 -0.0616 0.0960 0.130 Uiso 1 1 calc GR . . . .
H16C H -0.1680 -0.0097 0.0654 0.130 Uiso 1 1 calc GR . . . .
C17 C 0.0236(5) -0.0740(4) 0.2668(3) 0.0988(13) Uani 1 1 d . . . . .
H17A H -0.0433 -0.1694 0.2757 0.148 Uiso 1 1 calc GR . . . .
H17B H 0.1101 -0.0183 0.3120 0.148 Uiso 1 1 calc GR . . . .
H17C H 0.0593 -0.0914 0.2140 0.148 Uiso 1 1 calc GR . . . .
C18 C -0.0325(5) 0.1250(5) 0.4291(2) 0.1131(18) Uani 1 1 d . . . . .
H18A H -0.1153 0.0600 0.4522 0.170 Uiso 1 1 calc GR . . . .
H18B H 0.0022 0.2286 0.4608 0.170 Uiso 1 1 calc GR . . . .
H18C H 0.0509 0.1005 0.4323 0.170 Uiso 1 1 calc GR . . . .
C19 C -0.2454(5) 0.2544(5) 0.3649(3) 0.1112(17) Uani 1 1 d . . . . .
H19A H -0.3464 0.1882 0.3729 0.167 Uiso 1 1 calc GR . . . .
H19B H -0.2513 0.3254 0.3380 0.167 Uiso 1 1 calc GR . . . .
H19C H -0.1792 0.3081 0.4188 0.167 Uiso 1 1 calc GR . . . .
C20 C -0.3105(4) 0.1447(5) 0.1642(3) 0.0887(12) Uani 1 1 d . . . . .
H20A H -0.4142 0.0644 0.1521 0.133 Uiso 1 1 calc GR . . . .
H20B H -0.2708 0.1513 0.1123 0.133 Uiso 1 1 calc GR . . . .
H20C H -0.3091 0.2388 0.1921 0.133 Uiso 1 1 calc GR . . . .
C21 C 0.5835(3) 0.2558(3) 0.84750(17) 0.0508(6) Uani 1 1 d . . . . .
C22 C 0.5962(3) 0.1704(3) 0.76968(18) 0.0548(7) Uani 1 1 d . . . . .
H22 H 0.6516 0.1168 0.7702 0.066 Uiso 1 1 calc R . . . .
C23 C 0.5296(3) 0.1647(3) 0.69428(18) 0.0524(6) Uani 1 1 d . . . . .
H23 H 0.5404 0.1077 0.6444 0.063 Uiso 1 1 calc R . . . .
C24 C 0.4435(3) 0.2446(3) 0.69047(17) 0.0492(6) Uani 1 1 d . . . . .
C25 C 0.4306(3) 0.3301(3) 0.76868(18) 0.0531(6) Uani 1 1 d . . . . .
H25 H 0.3750 0.3836 0.7683 0.064 Uiso 1 1 calc R . . . .
C26 C 0.4977(3) 0.3355(3) 0.84385(18) 0.0521(6) Uani 1 1 d . . . . .
H26 H 0.4871 0.3925 0.8938 0.063 Uiso 1 1 calc R . . . .
C27 C 0.6422(4) 0.3487(4) 1.0038(2) 0.0733(9) Uani 1 1 d . . . . .
C28 C 0.6535(4) 0.2625(4) 0.92649(19) 0.0609(7) Uani 1 1 d . . . . .
C29 C 0.7373(5) 0.1828(5) 0.9311(2) 0.0754(10) Uani 1 1 d . . . . .
C30 C 0.2856(4) 0.3186(4) 0.6111(2) 0.0692(8) Uani 1 1 d . . . . .
C31 C 0.3728(3) 0.2401(3) 0.61255(19) 0.0576(7) Uani 1 1 d . . . . .
C32 C 0.3840(4) 0.1585(4) 0.5330(2) 0.0668(8) Uani 1 1 d . . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.086(3) . ?
Fe1 C2 2.092(3) . ?
Fe1 C3 2.082(3) . ?
Fe1 C4 2.092(3) . ?
Fe1 C5 2.097(3) . ?
Fe1 C11 2.096(3) . ?
Fe1 C12 2.095(3) . ?
Fe1 C13 2.095(3) . ?
Fe1 C14 2.095(3) . ?
Fe1 C15 2.098(3) . ?
N1 C27 1.141(4) . ?
N2 C29 1.139(4) . ?
N3 C30 1.138(4) . ?
N4 C32 1.137(4) . ?
C1 C2 1.397(5) . ?
C1 C5 1.381(5) . ?
C1 C6 1.510(5) . ?
C2 C3 1.421(5) . ?
C2 C7 1.506(5) . ?
C3 C4 1.394(5) . ?
C3 C8 1.505(5) . ?
C4 C5 1.378(5) . ?
C4 C9 1.512(5) . ?
C5 C10 1.509(5) . ?
C11 C12 1.410(4) . ?
C11 C15 1.407(4) . ?
C11 C16 1.507(4) . ?
C12 C13 1.418(4) . ?
C12 C17 1.513(4) . ?
C13 C14 1.411(4) . ?
C13 C18 1.514(4) . ?
C14 C15 1.408(4) . ?
C14 C19 1.518(4) . ?
C15 C20 1.504(4) . ?
C21 C22 1.417(4) . ?
C21 C26 1.418(4) . ?
C21 C28 1.421(4) . ?
C22 C23 1.359(4) . ?
C23 C24 1.421(4) . ?
C24 C25 1.424(4) . ?
C24 C31 1.418(4) . ?
C25 C26 1.359(4) . ?
C27 C28 1.409(4) . ?
C28 C29 1.404(4) . ?
C30 C31 1.413(4) . ?
C31 C32 1.418(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 39.06(13) . . ?
C1 Fe1 C4 64.66(12) . . ?
C1 Fe1 C5 38.55(13) . . ?
C1 Fe1 C11 167.39(14) . . ?
C1 Fe1 C12 152.10(14) . . ?
C1 Fe1 C13 119.70(12) . . ?
C1 Fe1 C14 110.95(11) . . ?
C1 Fe1 C15 130.62(13) . . ?
C2 Fe1 C5 65.45(12) . . ?
C2 Fe1 C11 130.63(12) . . ?
C2 Fe1 C12 167.63(13) . . ?
C2 Fe1 C13 151.63(14) . . ?
C2 Fe1 C14 119.92(13) . . ?
C2 Fe1 C15 110.90(11) . . ?
C3 Fe1 C1 65.54(11) . . ?
C3 Fe1 C2 39.82(14) . . ?
C3 Fe1 C4 39.02(15) . . ?
C3 Fe1 C5 65.25(13) . . ?
C3 Fe1 C11 111.28(11) . . ?
C3 Fe1 C12 130.34(13) . . ?
C3 Fe1 C13 166.78(16) . . ?
C3 Fe1 C14 153.01(15) . . ?
C3 Fe1 C15 120.96(13) . . ?
C4 Fe1 C2 65.73(12) . . ?
C4 Fe1 C5 38.41(14) . . ?
C4 Fe1 C11 121.35(13) . . ?
C4 Fe1 C12 111.39(12) . . ?
C4 Fe1 C13 129.91(15) . . ?
C4 Fe1 C14 166.29(16) . . ?
C4 Fe1 C15 153.51(15) . . ?
C5 Fe1 C15 166.73(14) . . ?
C11 Fe1 C5 152.85(14) . . ?
C11 Fe1 C15 39.21(11) . . ?
C12 Fe1 C5 120.50(13) . . ?
C12 Fe1 C11 39.34(12) . . ?
C12 Fe1 C13 39.58(12) . . ?
C12 Fe1 C14 65.86(11) . . ?
C12 Fe1 C15 65.85(11) . . ?
C13 Fe1 C5 110.47(12) . . ?
C13 Fe1 C11 66.32(11) . . ?
C13 Fe1 C14 39.35(12) . . ?
C13 Fe1 C15 66.16(11) . . ?
C14 Fe1 C5 130.05(13) . . ?
C14 Fe1 C11 65.85(11) . . ?
C14 Fe1 C15 39.25(12) . . ?
C2 C1 Fe1 70.71(16) . . ?
C2 C1 C6 126.5(4) . . ?
C5 C1 Fe1 71.16(18) . . ?
C5 C1 C2 109.2(3) . . ?
C5 C1 C6 124.2(4) . . ?
C6 C1 Fe1 127.0(2) . . ?
C1 C2 Fe1 70.22(17) . . ?
C1 C2 C3 106.4(3) . . ?
C1 C2 C7 125.9(4) . . ?
C3 C2 Fe1 69.73(16) . . ?
C3 C2 C7 127.7(5) . . ?
C7 C2 Fe1 126.3(2) . . ?
C2 C3 Fe1 70.45(16) . . ?
C2 C3 C8 125.5(5) . . ?
C4 C3 Fe1 70.85(18) . . ?
C4 C3 C2 107.5(3) . . ?
C4 C3 C8 126.9(5) . . ?
C8 C3 Fe1 126.5(2) . . ?
C3 C4 Fe1 70.14(17) . . ?
C3 C4 C9 124.9(5) . . ?
C5 C4 Fe1 70.99(18) . . ?
C5 C4 C3 108.8(3) . . ?
C5 C4 C9 126.3(5) . . ?
C9 C4 Fe1 127.2(3) . . ?
C1 C5 Fe1 70.29(17) . . ?
C1 C5 C10 126.6(5) . . ?
C4 C5 Fe1 70.59(18) . . ?
C4 C5 C1 108.2(3) . . ?
C4 C5 C10 125.2(5) . . ?
C10 C5 Fe1 126.3(2) . . ?
C12 C11 Fe1 70.28(16) . . ?
C12 C11 C16 125.3(3) . . ?
C15 C11 Fe1 70.46(15) . . ?
C15 C11 C12 107.9(2) . . ?
C15 C11 C16 126.6(3) . . ?
C16 C11 Fe1 127.6(2) . . ?
C11 C12 Fe1 70.38(15) . . ?
C11 C12 C13 108.2(3) . . ?
C11 C12 C17 127.2(3) . . ?
C13 C12 Fe1 70.22(16) . . ?
C13 C12 C17 124.4(3) . . ?
C17 C12 Fe1 127.6(2) . . ?
C12 C13 Fe1 70.21(15) . . ?
C12 C13 C18 127.2(4) . . ?
C14 C13 Fe1 70.35(15) . . ?
C14 C13 C12 107.2(2) . . ?
C14 C13 C18 125.5(3) . . ?
C18 C13 Fe1 126.6(2) . . ?
C13 C14 Fe1 70.30(16) . . ?
C13 C14 C19 126.5(3) . . ?
C15 C14 Fe1 70.46(15) . . ?
C15 C14 C13 108.5(2) . . ?
C15 C14 C19 124.9(4) . . ?
C19 C14 Fe1 127.6(2) . . ?
C11 C15 Fe1 70.33(15) . . ?
C11 C15 C14 108.0(3) . . ?
C11 C15 C20 125.3(3) . . ?
C14 C15 Fe1 70.29(16) . . ?
C14 C15 C20 126.7(3) . . ?
C20 C15 Fe1 126.6(2) . . ?
C22 C21 C26 117.3(2) . . ?
C22 C21 C28 122.0(3) . . ?
C26 C21 C28 120.7(3) . . ?
C23 C22 C21 121.8(3) . . ?
C22 C23 C24 121.0(3) . . ?
C23 C24 C25 117.1(2) . . ?
C31 C24 C23 122.0(3) . . ?
C31 C24 C25 120.9(2) . . ?
C26 C25 C24 121.5(3) . . ?
C25 C26 C21 121.2(3) . . ?
N1 C27 C28 179.1(4) . . ?
C27 C28 C21 122.0(3) . . ?
C29 C28 C21 121.3(3) . . ?
C29 C28 C27 116.7(3) . . ?
N2 C29 C28 179.5(5) . . ?
N3 C30 C31 178.7(4) . . ?
C30 C31 C24 120.5(3) . . ?
C30 C31 C32 116.4(3) . . ?
C32 C31 C24 123.0(3) . . ?
N4 C32 C31 179.2(4) . . ?

_shelx_SHELXL_version_number     2014/7
_olex2_submission_special_instructions 'No special instructions were received'
####################################################################### 
# 
# 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_JGD-1026-1-17
_database_code_depnum_ccdc_archive 'CCDC 2069078'
loop_
_audit_author_name
_audit_author_address
'Peter Stephens'
;Stony Brook University
United States of America
;
_audit_update_record             
;
2021-03-09 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
Decamethylferrocenium 7,7,8,8-Tetracyano-p-quinodimethanide
;
_chemical_name_common            ?
_chemical_formula_moiety         'C20 H30 Fe, C12 H4 N4'
_chemical_formula_structural     'Fe (C5 (CH3)5)2 C12 H4 N4'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C32 H34 Fe N4'
_chemical_formula_weight         530.48

_exptl_crystal_description       powder

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz #<--must include 'x,y,z'
1 '-x, -y, -z'
2 'x, y, z'

_cell_length_a                   9.65612(27)
_cell_length_b                   10.43874(26)
_cell_length_c                   8.63142(30)
_cell_angle_alpha                92.9050(71)
_cell_angle_beta                 109.2794(29)
_cell_angle_gamma                119.6756(35)
_cell_volume                     688.771(57)
_cell_formula_units_Z            1
_cell_measurement_temperature    17 #Kelvin

_cell_special_details            
; ?
;

_pd_spec_mount_mode              transmission
_pd_spec_size_axial              10 #millimeters
_pd_spec_size_equat              1 #mm
_pd_spec_size_thick              1 #mm
_pd_spec_shape                   capillary
_exptl_absorpt_correction_type   none

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
# This field should be
# used to give details of the 
# container.
;
capillary
;
_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions



#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; Metamagnetic polymorph, 17 K
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
;
X16C, National Synchrotron Light Source, Brookhaven National Laboratory
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
NIST standard reference material 1976(sintered plate of Al2O3)
Seven well-isolated reflections were used to calibrate wavelength and detector zero.
;

_diffrn_ambient_temperature      17 #Kelvin
_diffrn_source                   synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Huber diffractometer'
_diffrn_detector                 'NaI scintillation counter'
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  Cryostat rocked 5 or 10 degrees at each point.
;

_diffrn_radiation_wavelength     0.699350
_diffrn_radiation_monochromator  'Si(111) channel cut'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        4667
_pd_meas_2theta_range_min        4.001
_pd_meas_2theta_range_max        17.999
_pd_meas_2theta_range_inc        0.003


#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
Molecules are defined as rigid bodies using the z-matrix function 
implemented in TOPAS-Academic.  The same isotropic displacement parameters are 
assigned to all of the molecules.
;
_refine_ls_hydrogen_treatment    noref

# The next three items are given as text.

_pd_proc_ls_profile_function     
;
Simple_Axial_model function with Rp=9999,Rs=330 in TOPAS-Academic
Anisotropic strain broadening per Stephens J.Appl.Cryst.(1999).
;
_pd_proc_ls_background_function  
;
24 Pearson-Voight peaks and Chebyshev polynomial with 12 coefficients
;
_pd_proc_ls_pref_orient_corr     
;
none
;

_pd_proc_ls_prof_R_factor        0.05583
_pd_proc_ls_prof_wR_factor       0.07062
_pd_proc_ls_prof_wR_expected     0.02164
_refine_ls_R_I_factor            ?
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;

_refine_ls_matrix_type           ?
_refine_ls_weighting_scheme      
sigma # options are 'sigma'(based on measured su's)
# or 'calc' (calculated weights)
_refine_ls_weighting_details     1/(sigma*sigma)
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     149
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    ?

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   3.263

_refine_ls_restrained_S_all      ?
_refine_ls_shift/su_max          ?
_refine_ls_shift/su_mean         ?

# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        4.001
_pd_proc_2theta_range_max        17.999
_pd_proc_2theta_range_inc        0.003
_pd_proc_wavelength              0.699350


_pd_block_diffractogram_id       JGD-1026-1-17
# The id used for the block containing
# the powder pattern profile (section 11).

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       SPEC
_computing_cell_refinement       TOPAS-Academic
_computing_data_reduction        TOPAS-Academic
_computing_structure_solution    TOPAS-Academic
_computing_structure_refinement  TOPAS-Academic
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material  Platon


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv

C1 C 0 -0.1027(12) 0.12115(97) 0.07042(87) 1 16.6(6)
C2 C 0 0.0861(13) 0.21114(41) 0.15635(45) 1 16.6(6)
C3 C 0 0.1559(10) 0.23859(13) 0.02808(69) 1 16.6(6)
C4 C 0 0.0103(11) 0.16557(48) -0.13712(48) 1 16.6(6)
C5 C 0 -0.1495(10) 0.09298(95) -0.11096(76) 1 16.6(6)
C6 C 0 -0.2118(17) 0.0747(16) 0.1724(15) 1 16.6(6)
C7 C 0 0.2082(18) 0.27411(59) 0.34213(47) 1 16.6(6)
C8 C 0 0.3405(11) 0.32400(79) 0.0409(14) 1 16.6(6)
C9 C 0 0.0022(17) 0.15539(79) -0.31500(65) 1 16.6(6)
C10 C 0 -0.3391(11) 0.0013(16) -0.2337(13) 1 16.6(6)
Fe1 Fe 0 0 0 0 1 16.6(6)
C1a C 0 0.02708(31) 0.51188(31) -0.14862(17) 1 10.7(6)
C2a C 0 -0.14282(20) 0.42817(23) -0.15837(14) 1 10.7(6)
C3a C 0 -0.16923(11) 0.41663(28) -0.00902(32) 1 10.7(6)
C4a C 0 -0.28912(41) 0.35458(47) -0.32169(29) 1 10.7(6)
C5a C 0 -0.25995(73) 0.36744(68) -0.47493(11) 1 10.7(6)
C6a C 0 -0.46459(29) 0.26813(62) -0.33176(62) 1 10.7(6)
N1a N 0 -0.24305(94) 0.3730(11) -0.60140(12) 1 10.7(6)
N2a N 0 -0.60280(20) 0.19936(67) -0.33317(90) 1 10.7(6)
H6a H 0 -0.1661(46) 0.0623(73) 0.2850(42) 1 16.6(6)
H6b H 0 -0.2505(61) 0.1383(35) 0.2024(58) 1 16.6(6)
H6c H 0 -0.3242(44) -0.0216(34) 0.1285(46) 1 16.6(6)
H7a H 0 0.3334(18) 0.3391(40) 0.37590(78) 1 16.6(6)
H7b H 0 0.1989(45) 0.3389(39) 0.4173(11) 1 16.6(6)
H7c H 0 0.2104(41) 0.20507(83) 0.4126(13) 1 16.6(6)
H8a H 0 0.3689(78) 0.381(37) -0.041(19) 1 16.6(6)
H8b H 0 0.435(19) 0.4043(99) 0.142(53) 1 16.6(6)
H8c H 0 0.396(14) 0.269(38) 0.034(38) 1 16.6(6)
H9a H 0 -0.0972(43) 0.1439(56) -0.4070(14) 1 16.6(6)
H9b H 0 0.0926(46) 0.2388(16) -0.3382(20) 1 16.6(6)
H9c H 0 0.0036(45) 0.0735(22) -0.3715(16) 1 16.6(6)
H10a H 0 -0.4244(15) 0.0090(43) -0.2055(24) 1 16.6(6)
H10b H 0 -0.3733(15) 0.0157(38) -0.3471(17) 1 16.6(6)
H10c H 0 -0.4026(18) -0.1093(15) -0.2670(48) 1 16.6(6)
H3a H 0 -0.28696(19) 0.35863(48) -0.01456(54) 1 10.7(6)
H1a H 0 0.04673(53) 0.52054(52) -0.25185(29) 1 10.7(6)

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.125(12) . . yes
Fe1 C2 2.124(5) . . yes
Fe1 C3 2.124(2) . . yes
Fe1 C4 2.125(5) . . yes
Fe1 C5 2.124(10) . . yes
C1 C2 1.448(15) . . no
C1 C5 1.448(10) . . no
C1 C6 1.51(2) . . no
C2 C3 1.448(11) . . no
C2 C7 1.506(7) . . no
C3 C4 1.448(8) . . no
C3 C8 1.507(14) . . no
C4 C5 1.447(14) . . no
C4 C9 1.507(9) . . no
C5 C10 1.507(16) . . no
N1A C5A 1.156(7) . . yes
N2A C6A 1.156(7) . . yes
C1A C2A 1.394(4) . . no
C2A C3A 1.395(3) . . no
C2A C4A 1.440(3) . . no
C4A C5A 1.440(5) . . no
C4A C6A 1.440(7) . . no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 39.9(4) . . . yes
C1A C2A C4A 120.0(2) . . . no
_exptl_crystal_colour            purple
_exptl_crystal_preparation       'Magnetic properties'
####################################################################### 
# 
# 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_JGD-1026-roomT
_database_code_depnum_ccdc_archive 'CCDC 2069080'
loop_
_audit_author_name
_audit_author_address
'Peter Stephens'
;Stony Brook University
United States of America
;
_audit_update_record             
;
2021-03-09 deposited with the CCDC.	2021-07-23 downloaded from the CCDC.
;

# 5. CHEMICAL DATA

_chemical_name_systematic        
;
Decamethylferrocenium 7,7,8,8-Tetracyano-p-quinodimethanide
;
_chemical_name_common            ?
_chemical_formula_moiety         'C20 H30 Fe, C12 H4 N4'
_chemical_formula_structural     'Fe (C5 (CH3)5)2 C12 H4 N4'
_chemical_formula_analytical     ?
_chemical_formula_sum            'C32 H34 Fe N4'
_chemical_formula_weight         530.48

_exptl_crystal_description       powder

loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
_atom_type_scat_length_neutron # include if applicable
? ? ? ? ? ?

#==============================================================================

# 6. POWDER SPECIMEN AND CRYSTAL DATA

_symmetry_cell_setting           Triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_symmetry_Int_Tables_number      2

loop_
_symmetry_equiv_pos_site_id
_symmetry_equiv_pos_as_xyz
1 x,y,z
2 -x,-y,-z

_cell_length_a                   9.78875(13)
_cell_length_b                   10.6249(8)
_cell_length_c                   17.2551(2)
_cell_angle_alpha                94.7462(15)
_cell_angle_beta                 107.4293(8)
_cell_angle_gamma                119.725(1)
_cell_volume                     1427.81(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    295
_cell_special_details            
; Cell setting chosen to emphasize relationship to mid-temperature subcell.
;
_exptl_crystal_density_diffrn    1.234

# The next three fields give the specimen dimensions in mm.  The equatorial 
# plane contains the incident and diffracted beam.

_pd_spec_size_axial              1 # mm perpendicular to 
# equatorial plane

_pd_spec_size_equat              1 # parallel to 
# scattering vector 
# in transmission

_pd_spec_size_thick              8 # parallel to 
# scattering vector 
# in reflection

# The next five fields are character fields that describe the specimen.

_pd_spec_mounting                
;
capillary
;
_pd_spec_mount_mode              transmission

_pd_spec_shape                   cylinder

_pd_char_particle_morphology     ?
_pd_char_colour                  ? # use ICDD colour descriptions


#==============================================================================

# 7. EXPERIMENTAL DATA

_exptl_special_details           
; Metamagnetic polymorph, room temperature
;

# The following item is used to identify the equipment used to record 
# the powder pattern when the diffractogram was measured at a laboratory 
# other than the authors' home institution, e.g. when neutron or synchrotron
# radiation is used.

_pd_instr_location               
;
X16C, National Synchrotron Light Source, Brookhaven National Laboratory
;
_pd_calibration_special_details  
# description of the method used
# to calibrate the instrument
;
NIST standard reference material 1976(sintered plate of Al2O3)
Well-isolated 7 reflections were used to calibrate wavelength and detector zero.
;

_diffrn_ambient_temperature      295
_diffrn_source                   synchrotron
_diffrn_source_target            ?
_diffrn_source_type              ?
_diffrn_radiation_type           synchrotron
_diffrn_measurement_device_type  'Huber diffractometer'
_diffrn_detector                 'NaI scintillation counter'
_diffrn_detector_type            ? # make or model of detector

_pd_meas_scan_method             step # options are 'step', 'cont',
# 'tof', 'fixed' or
# 'disp' (= dispersive)
_pd_meas_special_details         
;  ?
;

# The following six items are used for angular dispersive measurements only.

_diffrn_radiation_wavelength     0.700065
_diffrn_radiation_monochromator  'Si(111) channel cut'

#  The following four items give details of the measured (not processed)
#  powder pattern.  Angles are in degrees.

_pd_meas_number_of_points        5601
_pd_meas_2theta_range_min        2.0
_pd_meas_2theta_range_max        30.0
_pd_meas_2theta_range_inc        0.005

#==============================================================================

# 8. REFINEMENT DATA

# Use the next field to give any special details about the fitting of the
# powder pattern.

_pd_proc_ls_special_details      
;
Molecules are defined as rigid bodies using the z-matrix function 
implemented in TOPAS-Academic.  The same isotropic displacement parameters are 
assigned to all of the molecules.
;

# The next three items are given as text.

_pd_proc_ls_profile_function     
;
Simple_Axial_model function with Rp=9999,Rs=330 in TOPAS-Academic
Anisotropic strain broadening per Stephens J.Appl.Cryst.(1999).
;
_pd_proc_ls_background_function  
;
10 Pseudo-Voight peaks and Chebyshev polynomial with 10 coefficients
;
_pd_proc_ls_pref_orient_corr     
;
none
;

_pd_proc_ls_prof_R_factor        0.05899 # 5.959(%)
_pd_proc_ls_prof_wR_factor       0.07257 # 7.465(%)    
_pd_proc_ls_prof_wR_expected     0.04111 # 4.114(%)        
_refine_ls_R_I_factor            0.0233
_refine_ls_R_Fsqd_factor         ?
_refine_ls_R_factor_all          ?

_refine_special_details          
; ?
;
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      sigma
_refine_ls_weighting_details     1/(sigma*sigma)
_refine_ls_extinction_coef       ?
_refine_ls_number_parameters     110
_refine_ls_number_restraints     ?
_refine_ls_number_constraints    99

# The following item is the same as CHI, the square root of 'CHI squared'
_refine_ls_goodness_of_fit_all   1.765


# The following four items apply to angular dispersive measurements.
# 2theta minimum, maximum and increment (in degrees) are for the 
# intensities used in the refinement.

_pd_proc_2theta_range_min        2.0
_pd_proc_2theta_range_max        30.0
_pd_proc_2theta_range_inc        0.005
_pd_proc_wavelength              0.700065


_pd_block_diffractogram_id       JGD-1026-roomT
# The id used for the block containing
# the powder pattern profile (section 11).

# Give appropriate details in the next two text fields.

_pd_proc_info_excluded_regions   ?
_pd_proc_info_data_reduction     ?

# The following items are used to identify the programs used.

_computing_data_collection       SPEC
_computing_cell_refinement       TOPAS-Academic
_computing_data_reduction        TOPAS-Academic
_computing_structure_solution    TOPAS-Academic
_computing_structure_refinement  TOPAS-Academic
_computing_molecular_graphics    'Crystal Maker'
_computing_publication_material  Platon


#==============================================================================


# 9. ATOMIC COORDINATES AND DISPLACEMENT PARAMETERS

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_symmetry_multiplicity
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_occupancy
_atom_site_B_iso_or_equiv

C1 C 2 0.0132(12) 0.3424(7) 0.8166(4) 1 6.87(18)
C2 C 2 -0.1010(12) 0.2823(6) 0.7362(4) 1 6.87(18)
C3 C 2 -0.0146(12) 0.3200(7) 0.6857(4) 1 6.87(18)
C4 C 2 0.1531(12) 0.4034(11) 0.7349(4) 1 6.87(18)
C5 C 2 0.1703(12) 0.4173(11) 0.8158(4) 1 6.87(18)
C6 C 2 -0.0465(15) 0.3189(9) 0.8872(6) 1 6.87(18)
C7 C 2 -0.2918(14) 0.1887(9) 0.6987(6) 1 6.87(18)
C8 C 2 -0.0728(15) 0.2857(9) 0.5919(5) 1 6.87(18)
C9 C 2 0.3079(14) 0.4758(16) 0.7144(6) 1 6.87(18)
C10 C 2 0.3241(14) 0.4963(16) 0.8970(5) 1 6.87(18)
C11 C 2 -0.1007(12) 0.6126(11) 0.7194(5) 1 6.87(18)
C12 C 2 -0.0422(13) 0.6464(11) 0.8041(5) 1 6.87(18)
C13 C 2 0.1293(13) 0.7304(7) 0.8349(4) 1 6.87(18)
C14 C 2 0.1768(13) 0.7485(6) 0.7692(5) 1 6.87(18)
C15 C 2 0.0347(13) 0.6757(9) 0.6979(4) 1 6.87(18)
C16 C 2 -0.2885(14) 0.5194(17) 0.6677(8) 1 6.87(18)
C17 C 2 -0.132(2) 0.6077(16) 0.8630(8) 1 6.87(18)
C18 C 2 0.2616(19) 0.7996(10) 0.9230(6) 1 6.87(18)
C19 C 2 0.3484(16) 0.8300(10) 0.7648(10) 1 6.87(18)
C20 C 2 0.008(2) 0.6568(13) 0.6070(6) 1 6.87(18)
Fe1 Fe 2 0.0419(3) 0.5179(5) 0.76147(18) 1 2.49(15)
H6a H 2 -0.172(2) 0.253(13) 0.8640(7) 1 6.87(18)
H6b H 2 0.003(15) 0.272(15) 0.922(5) 1 6.87(18)
H6c H 2 -0.010(16) 0.416(2) 0.922(5) 1 6.87(18)
H7a H 2 -0.3340(12) 0.222(12) 0.651(6) 1 6.87(18)
H7b H 2 -0.3323(18) 0.082(2) 0.679(9) 1 6.87(18)
H7c H 2 -0.3345(14) 0.200(14) 0.742(3) 1 6.87(18)
H8a H 2 -0.040(16) 0.220(13) 0.5718(11) 1 6.87(18)
H8b H 2 -0.197(2) 0.234(14) 0.5660(7) 1 6.87(18)
H8c H 2 -0.019(14) 0.3800(17) 0.5762(7) 1 6.87(18)
H9a H 2 0.355(11) 0.413(8) 0.718(9) 1 6.87(18)
H9b H 2 0.276(4) 0.486(15) 0.657(3) 1 6.87(18)
H9c H 2 0.394(7) 0.576(7) 0.755(5) 1 6.87(18)
H10a H 2 0.289(2) 0.500(14) 0.9442(8) 1 6.87(18)
H10b H 2 0.381(10) 0.442(9) 0.903(4) 1 6.87(18)
H10c H 2 0.403(8) 0.599(5) 0.897(4) 1 6.87(18)
H16a H 2 -0.349(2) 0.531(13) 0.701(3) 1 6.87(18)
H16b H 2 -0.313(3) 0.553(11) 0.617(5) 1 6.87(18)
H16c H 2 -0.327(4) 0.413(3) 0.651(8) 1 6.87(18)
H17a H 2 -0.152(15) 0.686(8) 0.878(7) 1 6.87(18)
H17b H 2 -0.242(8) 0.511(7) 0.835(3) 1 6.87(18)
H17c H 2 -0.061(8) 0.601(15) 0.914(4) 1 6.87(18)
H18a H 2 0.375(2) 0.860(13) 0.9219(10) 1 6.87(18)
H18b H 2 0.242(11) 0.864(13) 0.956(3) 1 6.87(18)
H18c H 2 0.255(13) 0.7198(12) 0.950(3) 1 6.87(18)
H19a H 2 0.335(2) 0.805(13) 0.7060(16) 1 6.87(18)
H19b H 2 0.403(8) 0.9390(11) 0.786(9) 1 6.87(18)
H19c H 2 0.420(6) 0.800(13) 0.800(8) 1 6.87(18)
H20a H 2 -0.107(7) 0.569(10) 0.5720(7) 1 6.87(18)
H20b H 2 0.021(19) 0.748(7) 0.592(2) 1 6.87(18)
H20c H 2 0.094(12) 0.641(17) 0.598(2) 1 6.87(18)
C21 C 2 0.8885(8) -0.0545(9) 0.1899(5) 1 6.0(2)
C22 C 2 1.0572(11) 0.027(5) 0.1914(5) 1 6.0(2)
C23 C 2 1.1972(12) 0.098(7) 0.2678(6) 1 6.0(2)
C24 C 2 1.1728(12) 0.090(5) 0.3450(7) 1 6.0(2)
C25 C 2 1.0041(11) 0.0081(11) 0.3436(7) 1 6.0(2)
C26 C 2 0.8641(9) -0.063(2) 0.2672(6) 1 6.0(2)
C27 C 2 0.7443(10) -0.128(3) 0.1112(6) 1 6.0(2)
C28 C 2 0.7624(10) -0.1224(11) 0.0324(8) 1 6.0(2)
C29 C 2 0.5732(15) -0.211(7) 0.1066(6) 1 6.0(2)
C30 C 2 1.3128(17) 0.161(7) 0.4214(9) 1 6.0(2)
C31 C 2 1.2938(17) 0.155(5) 0.5039(10) 1 6.0(2)
C32 C 2 1.4917(18) 0.248(12) 0.4263(10) 1 6.0(2)
N1 N 2 0.7761(11) -0.1183(18) -0.0273(9) 1 6.0(2)
N2 N 2 0.4436(17) -0.273(10) 0.1031(7) 1 6.0(2)
N3 N 2 1.2801(18) 0.151(3) 0.5636(11) 1 6.0(2)
N4 N 2 1.621 0.310 0.4298 1 6.0(2)
H22 H 2 1.0740 0.033 0.1383 1 6.0(2)
H23 H 2 1.3133 0.154 0.2688 1 6.0(2)
H25 H 2 0.9873 0.0023 0.3967 1 6.0(2)
H26 H 2 0.7481 -0.119 0.2662 1 6.0(2)

#===============================================================================

# 10. MOLECULAR GEOMETRY

_geom_special_details            
;
 Bond distances, angles etc. have been calculated using the
 rounded fractional coordinates. All su's are estimated
 from the variances of the (full) variance-covariance matrix.
 The cell esds are taken into account in the estimation of
 distances, angles and torsion angles
;

loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_1
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 C1 2.096(8) . . yes
C1 C5 1.341(17) . . no
C1 C6 1.490(15) . . no
N1 C28 1.080(19) . . yes
C6 H6B 0.98(14) . . no
C6 H6C 0.98(7) . . no
C6 H6A 0.98(8) . . no
C21 C22 1.43(4) . . no
C21 C26 1.426(14) . . no
C21 C27 1.425(15) . . no
C22 C23 1.38(3) . . no
C23 C24 1.42(3) . . no
C24 C25 1.43(4) . . no
C22 H22 0.98(3) . . no

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_2
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Fe1 C2 37.3(3) . . . yes
C1 Fe1 C12 115.4(4) . . . yes
C1 C5 C4 108.0(9) . . . no
C22 C21 C26 120.0(9) . . . no
C31 C30 C32 116(2) . . . no
_exptl_crystal_colour            purple
_exptl_crystal_preparation       'Magnetic properties'
