# Electronic Supplementary Material (ESI) for Faraday Discussions.
# This journal is © The Royal Society of Chemistry 2016

####################################################################### 
# 
# 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_FePY5Me2Cl_PF6
_database_code_depnum_ccdc_archive 'CCDC 1451777'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;

_audit_creation_date             2015-09-30T17:23:40-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
FePY5Me2Cl_PF6
;
_chemical_formula_moiety         'C29 H25 Cl Fe N5, F6 P'
_chemical_formula_sum            'C29 H25 Cl1 F6 Fe1 N5 P1'
_chemical_formula_weight         679.81
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_Int_Tables_number      57
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.9422(3)
_cell_length_b                   17.1851(6)
_cell_length_c                   20.8463(8)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3203.5(2)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    15905
_cell_measurement_theta_min      3
_cell_measurement_theta_max      27.4
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.41
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1384
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.666
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1955)'
_exptl_absorpt_correction_T_min  0.405
_exptl_absorpt_correction_T_max  1.000
_shelx_estimated_absorpt_T_min   0.936
_shelx_estimated_absorpt_T_max   0.936

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'rotating anode'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'curved image-plate'
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_ub_11      0.028306
_diffrn_orient_matrix_ub_12      0.029269
_diffrn_orient_matrix_ub_13      -0.039642
_diffrn_orient_matrix_ub_21      -0.092986
_diffrn_orient_matrix_ub_22      -0.018826
_diffrn_orient_matrix_ub_23      -0.021664
_diffrn_orient_matrix_ub_31      -0.055301
_diffrn_orient_matrix_ub_32      0.046636
_diffrn_orient_matrix_ub_33      0.016135
_diffrn_measurement_device       'quarter Χ-circle diffractometer'
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0888
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_number            29640
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.001
_diffrn_reflns_theta_max         27.418
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_reflns_Friedel_coverage         0
_reflns_number_total             3741
_reflns_number_gt                2261
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'RAPID AUTO (Rigaku)'
_computing_cell_refinement       'RAPID AUTO (Rigaku)'
_computing_data_reduction        'RAPID AUTO (Rigaku)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   direct
_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0989P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3741
_refine_ls_number_parameters     215
_refine_ls_number_restraints     2
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0584
_refine_ls_wR_factor_ref         0.1904
_refine_ls_wR_factor_gt          0.1566
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.11
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.716
_refine_diff_density_min         -0.617
_refine_diff_density_rms         0.084

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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
C1 C 0.8776(5) 0.1794(2) 0.86098(19) 0.0474(9) Uani 1 1 d . . . . .
H1 H 0.7736 0.1903 0.8631 0.057 Uiso 1 1 calc R U . . .
C2 C 0.9705(5) 0.2132(2) 0.9062(2) 0.0567(10) Uani 1 1 d . . . . .
H2 H 0.9307 0.2455 0.9391 0.068 Uiso 1 1 calc R U . . .
C3 C 1.1226(5) 0.1990(2) 0.9024(2) 0.0601(11) Uani 1 1 d . . . . .
H3 H 1.1896 0.2205 0.933 0.072 Uiso 1 1 calc R U . . .
C4 C 1.1745(5) 0.1532(2) 0.8533(2) 0.0576(11) Uani 1 1 d . . . . .
H4 H 1.2788 0.1435 0.8497 0.069 Uiso 1 1 calc R U . . .
C5 C 1.0779(4) 0.1209(2) 0.8090(2) 0.0468(9) Uani 1 1 d . . . . .
C6 C 1.1334(6) 0.0764(3) 0.75 0.0502(14) Uani 1 2 d S T P . .
C7 C 1.3027(6) 0.0714(3) 0.75 0.0591(16) Uani 1 2 d S T P . .
H7A H 1.3362 0.0435 0.7884 0.089 Uiso 0.5 1 calc R U P . .
H7B H 1.3449 0.1241 0.75 0.089 Uiso 1 2 calc R U P . .
H7C H 1.3362 0.0435 0.7116 0.089 Uiso 0.5 1 calc R U P . .
C8 C 1.0674(6) -0.0067(3) 0.75 0.0490(14) Uani 1 2 d S T P . .
C9 C 1.1581(7) -0.0714(3) 0.75 0.0608(17) Uani 1 2 d S T P . .
H9 H 1.2637 -0.0653 0.75 0.073 Uiso 1 2 calc R U P . .
C10 C 1.0966(7) -0.1454(3) 0.75 0.0634(17) Uani 1 2 d S T P . .
H10 H 1.1588 -0.1903 0.75 0.076 Uiso 1 2 calc R U P . .
C11 C 0.9446(7) -0.1523(3) 0.75 0.0639(17) Uani 1 2 d S T P . .
H11 H 0.8993 -0.2023 0.75 0.077 Uiso 1 2 calc R U P . .
C12 C 0.8559(6) -0.0852(3) 0.75 0.0529(14) Uani 1 2 d S T P . .
C13 C 0.6843(6) -0.0898(3) 0.75 0.0510(14) Uani 1 2 d S T P . .
C14 C 0.6338(7) -0.1761(3) 0.75 0.0668(18) Uani 1 2 d S T P . .
H14A H 0.6725 -0.2021 0.7116 0.1 Uiso 0.5 1 calc R U P . .
H14B H 0.5243 -0.1786 0.75 0.1 Uiso 1 2 calc R U P . .
H14C H 0.6725 -0.2021 0.7884 0.1 Uiso 0.5 1 calc R U P . .
C15 C 0.6233(4) -0.0487(2) 0.6909(2) 0.0489(9) Uani 1 1 d . . . . .
C16 C 0.5320(5) -0.0855(2) 0.6460(2) 0.0590(12) Uani 1 1 d . . . . .
H16 H 0.5121 -0.1396 0.6503 0.071 Uiso 1 1 calc R U . . .
C17 C 0.4707(5) -0.0452(3) 0.5959(2) 0.0640(12) Uani 1 1 d . . . . .
H17 H 0.4091 -0.0708 0.5653 0.077 Uiso 1 1 calc R U . . .
C18 C 0.5003(5) 0.0333(2) 0.5907(2) 0.0563(10) Uani 1 1 d . . . . .
H18 H 0.4582 0.0633 0.5569 0.068 Uiso 1 1 calc R U . . .
C19 C 0.5923(4) 0.0673(2) 0.63568(19) 0.0469(9) Uani 1 1 d . . . . .
H19 H 0.6128 0.1213 0.6318 0.056 Uiso 1 1 calc R U . . .
N1 N 0.9270(3) 0.13161(16) 0.81399(16) 0.0440(7) Uani 1 1 d . . . . .
N2 N 0.6552(3) 0.02800(16) 0.68497(16) 0.0439(7) Uani 1 1 d . . . . .
N3 N 0.9161(5) -0.0131(2) 0.75 0.0500(11) Uani 1 2 d S T P . .
F1 F 0.4115(3) 0.31537(13) 0.50516(12) 0.0585(6) Uani 1 1 d . . . . .
F2 F 0.5376(3) 0.24249(14) 0.57617(13) 0.0752(8) Uani 1 1 d . . . . .
F3 F 0.6644(3) 0.18387(14) 0.49648(15) 0.0757(8) Uani 1 1 d . . . . .
P1 P 0.53818(17) 0.25 0.5 0.0499(4) Uani 1 2 d S T P . .
Cl1 Cl 0.63717(14) 0.18953(6) 0.75 0.0455(3) Uani 1 2 d S T P . .
Fe1 Fe 0.78957(8) 0.08049(4) 0.75 0.0402(3) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.352(5) . ?
C1 C2 1.385(6) . ?
C1 H1 0.95 . ?
C2 C3 1.385(6) . ?
C2 H2 0.95 . ?
C3 C4 1.371(6) . ?
C3 H3 0.95 . ?
C4 C5 1.381(6) . ?
C4 H4 0.95 . ?
C5 N1 1.366(4) . ?
C5 C6 1.531(5) . ?
C6 C7 1.516(8) . ?
C6 C5 1.531(5) 6_557 ?
C6 C8 1.544(7) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N3 1.358(7) . ?
C8 C9 1.377(7) . ?
C9 C10 1.385(8) . ?
C9 H9 0.95 . ?
C10 C11 1.365(9) . ?
C10 H10 0.95 . ?
C11 C12 1.400(8) . ?
C11 H11 0.95 . ?
C12 N3 1.350(6) . ?
C12 C13 1.537(8) . ?
C13 C15 1.521(5) 6_557 ?
C13 C15 1.521(5) . ?
C13 C14 1.549(7) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N2 1.355(4) . ?
C15 C16 1.394(6) . ?
C16 C17 1.369(7) . ?
C16 H16 0.95 . ?
C17 C18 1.379(6) . ?
C17 H17 0.95 . ?
C18 C19 1.377(6) . ?
C18 H18 0.95 . ?
C19 N2 1.352(5) . ?
C19 H19 0.95 . ?
N1 Fe1 2.015(3) . ?
N2 Fe1 2.024(3) . ?
N3 Fe1 1.966(4) . ?
F1 P1 1.599(2) . ?
F2 P1 1.593(3) . ?
F3 P1 1.604(3) . ?
P1 F2 1.593(3) 3_556 ?
P1 F1 1.599(2) 3_556 ?
P1 F3 1.604(3) 3_556 ?
Cl1 Fe1 2.3170(14) . ?
Fe1 N1 2.015(3) 6_557 ?
Fe1 N2 2.024(3) 6_557 ?

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
N1 C1 C2 123.6(4) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C1 C2 C3 118.4(4) . . ?
C1 C2 H2 120.8 . . ?
C3 C2 H2 120.8 . . ?
C4 C3 C2 118.5(4) . . ?
C4 C3 H3 120.8 . . ?
C2 C3 H3 120.8 . . ?
C3 C4 C5 121.2(4) . . ?
C3 C4 H4 119.4 . . ?
C5 C4 H4 119.4 . . ?
N1 C5 C4 120.9(4) . . ?
N1 C5 C6 116.6(4) . . ?
C4 C5 C6 122.4(4) . . ?
C7 C6 C5 110.6(3) . 6_557 ?
C7 C6 C5 110.6(3) . . ?
C5 C6 C5 106.9(4) 6_557 . ?
C7 C6 C8 109.2(4) . . ?
C5 C6 C8 109.8(3) 6_557 . ?
C5 C6 C8 109.8(3) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 121.4(5) . . ?
N3 C8 C6 117.1(4) . . ?
C9 C8 C6 121.5(5) . . ?
C8 C9 C10 120.5(5) . . ?
C8 C9 H9 119.7 . . ?
C10 C9 H9 119.7 . . ?
C11 C10 C9 118.4(5) . . ?
C11 C10 H10 120.8 . . ?
C9 C10 H10 120.8 . . ?
C10 C11 C12 119.5(5) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N3 C12 C11 122.0(5) . . ?
N3 C12 C13 116.4(5) . . ?
C11 C12 C13 121.5(5) . . ?
C15 C13 C15 108.2(4) 6_557 . ?
C15 C13 C12 109.5(3) 6_557 . ?
C15 C13 C12 109.5(3) . . ?
C15 C13 C14 109.9(3) 6_557 . ?
C15 C13 C14 109.9(3) . . ?
C12 C13 C14 109.9(4) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 120.3(4) . . ?
N2 C15 C13 116.8(3) . . ?
C16 C15 C13 122.9(3) . . ?
C17 C16 C15 121.2(4) . . ?
C17 C16 H16 119.4 . . ?
C15 C16 H16 119.4 . . ?
C16 C17 C18 118.6(4) . . ?
C16 C17 H17 120.7 . . ?
C18 C17 H17 120.7 . . ?
C19 C18 C17 118.4(4) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
N2 C19 C18 123.7(3) . . ?
N2 C19 H19 118.2 . . ?
C18 C19 H19 118.2 . . ?
C1 N1 C5 117.3(3) . . ?
C1 N1 Fe1 123.0(3) . . ?
C5 N1 Fe1 119.6(3) . . ?
C19 N2 C15 117.9(3) . . ?
C19 N2 Fe1 122.3(2) . . ?
C15 N2 Fe1 119.9(3) . . ?
C12 N3 C8 118.1(4) . . ?
C12 N3 Fe1 121.4(4) . . ?
C8 N3 Fe1 120.5(3) . . ?
F2 P1 F2 179.6(2) 3_556 . ?
F2 P1 F1 90.44(15) 3_556 . ?
F2 P1 F1 89.29(13) . . ?
F2 P1 F1 89.28(13) 3_556 3_556 ?
F2 P1 F1 90.44(15) . 3_556 ?
F1 P1 F1 89.81(18) . 3_556 ?
F2 P1 F3 89.46(15) 3_556 3_556 ?
F2 P1 F3 90.82(16) . 3_556 ?
F1 P1 F3 89.86(13) . 3_556 ?
F1 P1 F3 178.70(16) 3_556 3_556 ?
F2 P1 F3 90.82(16) 3_556 . ?
F2 P1 F3 89.46(15) . . ?
F1 P1 F3 178.70(16) . . ?
F1 P1 F3 89.86(12) 3_556 . ?
F3 P1 F3 90.5(2) 3_556 . ?
N3 Fe1 N1 90.33(13) . 6_557 ?
N3 Fe1 N1 90.33(13) . . ?
N1 Fe1 N1 82.90(18) 6_557 . ?
N3 Fe1 N2 88.68(13) . . ?
N1 Fe1 N2 96.48(13) 6_557 . ?
N1 Fe1 N2 178.83(13) . . ?
N3 Fe1 N2 88.68(13) . 6_557 ?
N1 Fe1 N2 178.83(13) 6_557 6_557 ?
N1 Fe1 N2 96.48(13) . 6_557 ?
N2 Fe1 N2 84.12(18) . 6_557 ?
N3 Fe1 Cl1 179.10(13) . . ?
N1 Fe1 Cl1 90.35(9) 6_557 . ?
N1 Fe1 Cl1 90.35(9) . . ?
N2 Fe1 Cl1 90.65(9) . . ?
N2 Fe1 Cl1 90.65(9) 6_557 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.6(6) . . . . ?
C1 C2 C3 C4 1.1(6) . . . . ?
C2 C3 C4 C5 -0.8(6) . . . . ?
C3 C4 C5 N1 -2.2(6) . . . . ?
C3 C4 C5 C6 173.7(4) . . . . ?
N1 C5 C6 C7 178.1(4) . . . . ?
C4 C5 C6 C7 2.1(5) . . . . ?
N1 C5 C6 C5 57.7(5) . . . 6_557 ?
C4 C5 C6 C5 -118.3(4) . . . 6_557 ?
N1 C5 C6 C8 -61.3(4) . . . . ?
C4 C5 C6 C8 122.7(4) . . . . ?
C7 C6 C8 N3 180 . . . . ?
C5 C6 C8 N3 -58.6(3) 6_557 . . . ?
C5 C6 C8 N3 58.6(3) . . . . ?
C7 C6 C8 C9 0 . . . . ?
C5 C6 C8 C9 121.4(3) 6_557 . . . ?
C5 C6 C8 C9 -121.4(3) . . . . ?
N3 C8 C9 C10 0 . . . . ?
C6 C8 C9 C10 180 . . . . ?
C8 C9 C10 C11 0 . . . . ?
C9 C10 C11 C12 0 . . . . ?
C10 C11 C12 N3 0 . . . . ?
C10 C11 C12 C13 180 . . . . ?
N3 C12 C13 C15 -59.2(3) . . . 6_557 ?
C11 C12 C13 C15 120.8(3) . . . 6_557 ?
N3 C12 C13 C15 59.2(3) . . . . ?
C11 C12 C13 C15 -120.8(3) . . . . ?
N3 C12 C13 C14 180 . . . . ?
C11 C12 C13 C14 0 . . . . ?
C15 C13 C15 N2 58.6(6) 6_557 . . . ?
C12 C13 C15 N2 -60.7(4) . . . . ?
C14 C13 C15 N2 178.4(4) . . . . ?
C15 C13 C15 C16 -118.1(4) 6_557 . . . ?
C12 C13 C15 C16 122.6(4) . . . . ?
C14 C13 C15 C16 1.8(6) . . . . ?
N2 C15 C16 C17 -1.2(6) . . . . ?
C13 C15 C16 C17 175.3(4) . . . . ?
C15 C16 C17 C18 -0.4(7) . . . . ?
C16 C17 C18 C19 1.1(6) . . . . ?
C17 C18 C19 N2 -0.3(6) . . . . ?
C2 C1 N1 C5 -4.5(5) . . . . ?
C2 C1 N1 Fe1 178.3(3) . . . . ?
C4 C5 N1 C1 4.7(5) . . . . ?
C6 C5 N1 C1 -171.4(3) . . . . ?
C4 C5 N1 Fe1 -178.0(3) . . . . ?
C6 C5 N1 Fe1 5.9(4) . . . . ?
C18 C19 N2 C15 -1.3(6) . . . . ?
C18 C19 N2 Fe1 -179.9(3) . . . . ?
C16 C15 N2 C19 2.0(5) . . . . ?
C13 C15 N2 C19 -174.8(3) . . . . ?
C16 C15 N2 Fe1 -179.4(3) . . . . ?
C13 C15 N2 Fe1 3.9(5) . . . . ?
C11 C12 N3 C8 0 . . . . ?
C13 C12 N3 C8 180 . . . . ?
C11 C12 N3 Fe1 180 . . . . ?
C13 C12 N3 Fe1 0 . . . . ?
C9 C8 N3 C12 0 . . . . ?
C6 C8 N3 C12 180 . . . . ?
C9 C8 N3 Fe1 180 . . . . ?
C6 C8 N3 Fe1 0 . . . . ?

# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 171 43 ' '
2 0.000 0.000 0.500 171 43 ' '
3 0.000 0.500 0.500 171 43 ' '
4 0.000 0.500 1.000 171 43 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 2.278
2 0 0 4.559
1 1 0 2.568
0 2 0 2.370
1 1 1 2.747
0 2 1 2.564
0 0 2 1.954
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL SIR97 run in space group P b c m
CELL    8.9422   17.1851   20.8463     90.00     90.00     90.00
SPGR Pbcm
# Solvent Accessible Volume =     701.3
# Electrons Found in S.A.V. =     172.6
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 1.000 1.000 0.000 !       4.52 eA-3
C102 0.920 0.582 0.421 !       2.87 eA-3
C103 0.030 0.545 0.049 !       2.17 eA-3
C104 0.100 0.038 0.033 !       1.84 eA-3
Q105 0.935 0.406 0.252 !       1.05 eA-3
Q106 0.780 0.313 0.249 !       0.98 eA-3
Q107 0.218 0.874 0.316 !       0.84 eA-3
Q108 0.646 0.422 0.248 !       0.79 eA-3
Q109 0.278 0.855 0.281 !       0.77 eA-3
Q110 0.276 0.422 0.249 !       0.75 eA-3
Q111 0.664 0.470 0.263 !       0.64 eA-3
Q112 0.209 0.578 0.249 !       0.61 eA-3
Q113 0.646 0.516 0.254 !       0.61 eA-3
Q114 0.212 0.951 0.191 !       0.61 eA-3
Q115 0.946 0.906 0.253 !       0.60 eA-3
C116 0.096 1.001 0.396 !       0.59 eA-3
Q117 0.250 0.937 0.245 !       0.57 eA-3
Q118 0.664 0.297 0.500 !       0.55 eA-3
Q119 0.441 0.874 0.233 !       0.55 eA-3
Q120 0.472 0.906 0.249 !       0.53 eA-3
Q121 0.491 0.766 0.251 !       0.53 eA-3
Q122 0.143 0.858 0.258 !       0.52 eA-3
Q123 0.154 0.981 0.213 !       0.52 eA-3
Q124 0.383 0.250 0.500 !       0.51 eA-3
;

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_RuPY5Me2Cl_PF6
_database_code_depnum_ccdc_archive 'CCDC 1451778'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;

_audit_creation_date             2015-10-01T11:27:27-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
RuPY5Me2Cl_PF6
;
_chemical_formula_moiety         'C29 H25 N5 Cl1 Ru1, P1 F6'
_chemical_formula_sum            'C29 H25 Cl1 F6 N5 P1 Ru1'
_chemical_formula_weight         725.03
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_Int_Tables_number      57
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.9368(13)
_cell_length_b                   17.315(3)
_cell_length_c                   20.910(3)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3235.6(9)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    8835
_cell_measurement_theta_min      3.22
_cell_measurement_theta_max      27.47
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Block
_exptl_crystal_colour            orange
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.06
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1456
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.939
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.923
_shelx_estimated_absorpt_T_max   0.96

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'Rotating Anode'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_detector_area_resol_mean 28.57
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_ub_11      -0.0338
_diffrn_orient_matrix_ub_12      0.077
_diffrn_orient_matrix_ub_13      0.0738
_diffrn_orient_matrix_ub_21      0.055
_diffrn_orient_matrix_ub_22      0.0142
_diffrn_orient_matrix_ub_23      0.0104
_diffrn_orient_matrix_ub_31      -0.0018
_diffrn_orient_matrix_ub_32      0.0327
_diffrn_orient_matrix_ub_33      -0.0349
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0311
_diffrn_reflns_av_unetI/netI     0.0207
_diffrn_reflns_number            23789
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.221
_diffrn_reflns_theta_max         27.471
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.993
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.993
_reflns_Friedel_coverage         0
_reflns_number_total             3796
_reflns_number_gt                3426
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al, 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0366P)²+2.0785P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3796
_refine_ls_number_parameters     215
_refine_ls_number_restraints     2
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0353
_refine_ls_R_factor_gt           0.0315
_refine_ls_wR_factor_ref         0.0735
_refine_ls_wR_factor_gt          0.0712
_refine_ls_goodness_of_fit_ref   1.085
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.056
_refine_diff_density_min         -0.473
_refine_diff_density_rms         0.069

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.0898(2) 0.06630(12) 0.86541(10) 0.0254(4) Uani 1 1 d . . . . .
H1 H 0.1084 0.1201 0.8695 0.03 Uiso 1 1 calc R U . . .
C2 C -0.0012(3) 0.03115(14) 0.91015(11) 0.0335(5) Uani 1 1 d . . . . .
H2 H -0.0428 0.06 0.9445 0.04 Uiso 1 1 calc R U . . .
C3 C -0.0304(3) -0.04698(14) 0.90391(12) 0.0397(6) Uani 1 1 d . . . . .
H3 H -0.0923 -0.073 0.9339 0.048 Uiso 1 1 calc R U . . .
C4 C 0.0323(3) -0.08627(12) 0.85327(12) 0.0353(5) Uani 1 1 d . . . . .
H4 H 0.0131 -0.1399 0.8483 0.042 Uiso 1 1 calc R U . . .
C5 C 0.1236(2) -0.04825(11) 0.80923(11) 0.0271(4) Uani 1 1 d . . . . .
C6 C 0.1881(3) -0.08813(15) 0.75 0.0291(7) Uani 1 2 d S T P . .
C7 C 0.1401(4) -0.17343(17) 0.75 0.0442(9) Uani 1 2 d S T P . .
H7A H 0.1812 -0.1992 0.7121 0.066 Uiso 0.5 1 calc R U P . .
H7B H 0.0307 -0.1767 0.7492 0.066 Uiso 1 2 calc R U P . .
H7C H 0.178 -0.1987 0.7887 0.066 Uiso 0.5 1 calc R U P . .
C8 C 0.3600(3) -0.08329(15) 0.75 0.0282(6) Uani 1 2 d S T P . .
C9 C 0.4486(4) -0.14979(18) 0.75 0.0403(8) Uani 1 2 d S T P . .
H9 H 0.4036 -0.1995 0.75 0.048 Uiso 1 2 calc R U P . .
C10 C 0.6008(4) -0.14246(19) 0.75 0.0435(9) Uani 1 2 d S T P . .
H10 H 0.6627 -0.1871 0.75 0.052 Uiso 1 2 calc R U P . .
C11 C 0.6640(4) -0.06943(19) 0.75 0.0381(8) Uani 1 2 d S T P . .
H11 H 0.7698 -0.0638 0.75 0.046 Uiso 1 2 calc R U P . .
C12 C 0.5732(3) -0.00452(16) 0.75 0.0273(6) Uani 1 2 d S T P . .
C13 C 0.6365(3) 0.07817(15) 0.75 0.0247(6) Uani 1 2 d S T P . .
C14 C 0.8079(3) 0.07277(19) 0.75 0.0341(7) Uani 1 2 d S T P . .
H14A H 0.8413 0.045 0.7883 0.051 Uiso 0.5 1 calc R U P . .
H14B H 0.8507 0.1249 0.75 0.051 Uiso 1 2 calc R U P . .
H14C H 0.8413 0.045 0.7117 0.051 Uiso 0.5 1 calc R U P . .
C15 C 0.5841(2) 0.12335(11) 0.80893(10) 0.0248(4) Uani 1 1 d . . . . .
C16 C 0.6838(2) 0.15607(13) 0.85237(11) 0.0327(5) Uani 1 1 d . . . . .
H16 H 0.7881 0.1468 0.8481 0.039 Uiso 1 1 calc R U . . .
C17 C 0.6319(3) 0.20190(14) 0.90165(11) 0.0382(5) Uani 1 1 d . . . . .
H17 H 0.6996 0.2236 0.9317 0.046 Uiso 1 1 calc R U . . .
C18 C 0.4805(3) 0.21578(14) 0.90655(10) 0.0333(5) Uani 1 1 d . . . . .
H18 H 0.442 0.248 0.9394 0.04 Uiso 1 1 calc R U . . .
C19 C 0.3863(2) 0.18174(11) 0.86265(10) 0.0257(4) Uani 1 1 d . . . . .
H19 H 0.282 0.1918 0.8658 0.031 Uiso 1 1 calc R U . . .
N1 N 0.15345(17) 0.02823(9) 0.81628(8) 0.0213(3) Uani 1 1 d . . . . .
N2 N 0.43475(17) 0.13476(9) 0.81535(8) 0.0215(3) Uani 1 1 d . . . . .
N3 N 0.4217(3) -0.01176(13) 0.75 0.0243(5) Uani 1 2 d S T P . .
F1 F 0.17196(15) 0.18437(8) 1.00248(9) 0.0520(4) Uani 1 1 d . . . . .
F2 F 0.04501(19) 0.24504(9) 0.92380(7) 0.0530(4) Uani 1 1 d . . . . .
F3 F -0.08064(15) 0.31505(7) 0.99631(7) 0.0384(3) Uani 1 1 d . . . . .
P1 P 0.04600(8) 0.25 1 0.02691(17) Uani 1 2 d S T P . .
Cl1 Cl 0.13233(7) 0.19513(3) 0.75 0.02070(14) Uani 1 2 d S T P . .
Ru1 Ru 0.29102(2) 0.08286(2) 0.75 0.01749(7) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.347(3) . ?
C1 C2 1.381(3) . ?
C1 H1 0.95 . ?
C2 C3 1.384(3) . ?
C2 H2 0.95 . ?
C3 C4 1.378(4) . ?
C3 H3 0.95 . ?
C4 C5 1.396(3) . ?
C4 H4 0.95 . ?
C5 N1 1.359(2) . ?
C5 C6 1.531(3) . ?
C6 C5 1.531(3) 6_557 ?
C6 C7 1.538(4) . ?
C6 C8 1.538(4) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N3 1.356(3) . ?
C8 C9 1.398(4) . ?
C9 C10 1.366(5) . ?
C9 H9 0.95 . ?
C10 C11 1.385(5) . ?
C10 H10 0.95 . ?
C11 C12 1.387(4) . ?
C11 H11 0.95 . ?
C12 N3 1.359(3) . ?
C12 C13 1.540(4) . ?
C13 C15 1.533(3) . ?
C13 C15 1.533(3) 6_557 ?
C13 C14 1.535(4) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N2 1.356(2) . ?
C15 C16 1.393(3) . ?
C16 C17 1.381(3) . ?
C16 H16 0.95 . ?
C17 C18 1.378(3) . ?
C17 H17 0.95 . ?
C18 C19 1.378(3) . ?
C18 H18 0.95 . ?
C19 N2 1.352(3) . ?
C19 H19 0.95 . ?
N1 Ru1 2.0802(16) . ?
N2 Ru1 2.0796(16) . ?
N3 Ru1 2.012(2) . ?
F1 P1 1.6004(14) . ?
F2 P1 1.5957(15) . ?
F3 P1 1.5986(13) . ?
P1 F2 1.5957(15) 3_557 ?
P1 F3 1.5986(13) 3_557 ?
P1 F1 1.6003(14) 3_557 ?
Cl1 Ru1 2.4064(7) . ?
Ru1 N2 2.0796(16) 6_557 ?
Ru1 N1 2.0802(16) 6_557 ?

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
N1 C1 C2 123.4(2) . . ?
N1 C1 H1 118.3 . . ?
C2 C1 H1 118.3 . . ?
C1 C2 C3 118.5(2) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 118.6(2) . . ?
C4 C3 H3 120.7 . . ?
C2 C3 H3 120.7 . . ?
C3 C4 C5 120.8(2) . . ?
C3 C4 H4 119.6 . . ?
C5 C4 H4 119.6 . . ?
N1 C5 C4 120.2(2) . . ?
N1 C5 C6 116.97(19) . . ?
C4 C5 C6 122.8(2) . . ?
C5 C6 C5 108.0(2) 6_557 . ?
C5 C6 C7 109.17(16) 6_557 . ?
C5 C6 C7 109.16(16) . . ?
C5 C6 C8 110.57(16) 6_557 . ?
C5 C6 C8 110.57(16) . . ?
C7 C6 C8 109.3(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 121.4(3) . . ?
N3 C8 C6 117.2(2) . . ?
C9 C8 C6 121.4(3) . . ?
C10 C9 C8 119.2(3) . . ?
C10 C9 H9 120.4 . . ?
C8 C9 H9 120.4 . . ?
C9 C10 C11 119.4(3) . . ?
C9 C10 H10 120.3 . . ?
C11 C10 H10 120.3 . . ?
C10 C11 C12 120.1(3) . . ?
C10 C11 H11 120 . . ?
C12 C11 H11 120 . . ?
N3 C12 C11 120.6(3) . . ?
N3 C12 C13 116.9(2) . . ?
C11 C12 C13 122.6(3) . . ?
C15 C13 C15 107.0(2) . 6_557 ?
C15 C13 C14 109.63(15) . . ?
C15 C13 C14 109.63(15) 6_557 . ?
C15 C13 C12 111.25(15) . . ?
C15 C13 C12 111.25(15) 6_557 . ?
C14 C13 C12 108.1(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 120.38(19) . . ?
N2 C15 C13 117.04(18) . . ?
C16 C15 C13 122.46(19) . . ?
C17 C16 C15 120.4(2) . . ?
C17 C16 H16 119.8 . . ?
C15 C16 H16 119.8 . . ?
C18 C17 C16 119.0(2) . . ?
C18 C17 H17 120.5 . . ?
C16 C17 H17 120.5 . . ?
C19 C18 C17 118.4(2) . . ?
C19 C18 H18 120.8 . . ?
C17 C18 H18 120.8 . . ?
N2 C19 C18 123.29(19) . . ?
N2 C19 H19 118.4 . . ?
C18 C19 H19 118.4 . . ?
C1 N1 C5 118.49(17) . . ?
C1 N1 Ru1 122.36(13) . . ?
C5 N1 Ru1 119.13(14) . . ?
C19 N2 C15 118.40(17) . . ?
C19 N2 Ru1 122.87(13) . . ?
C15 N2 Ru1 118.69(13) . . ?
C8 N3 C12 119.3(2) . . ?
C8 N3 Ru1 120.49(19) . . ?
C12 N3 Ru1 120.19(18) . . ?
F2 P1 F2 179.36(14) . 3_557 ?
F2 P1 F3 90.36(8) . 3_557 ?
F2 P1 F3 89.18(8) 3_557 3_557 ?
F2 P1 F3 89.19(8) . . ?
F2 P1 F3 90.36(8) 3_557 . ?
F3 P1 F3 89.86(10) 3_557 . ?
F2 P1 F1 90.55(9) . 3_557 ?
F2 P1 F1 89.89(9) 3_557 3_557 ?
F3 P1 F1 179.01(9) 3_557 3_557 ?
F3 P1 F1 89.78(7) . 3_557 ?
F2 P1 F1 89.89(9) . . ?
F2 P1 F1 90.56(9) 3_557 . ?
F3 P1 F1 89.78(7) 3_557 . ?
F3 P1 F1 179.01(9) . . ?
F1 P1 F1 90.60(11) 3_557 . ?
N3 Ru1 N2 89.62(7) . . ?
N3 Ru1 N2 89.62(7) . 6_557 ?
N2 Ru1 N2 82.15(9) . 6_557 ?
N3 Ru1 N1 88.45(7) . . ?
N2 Ru1 N1 97.11(6) . . ?
N2 Ru1 N1 177.93(6) 6_557 . ?
N3 Ru1 N1 88.45(7) . 6_557 ?
N2 Ru1 N1 177.93(6) . 6_557 ?
N2 Ru1 N1 97.11(6) 6_557 6_557 ?
N1 Ru1 N1 83.56(9) . 6_557 ?
N3 Ru1 Cl1 179.38(7) . . ?
N2 Ru1 Cl1 90.85(5) . . ?
N2 Ru1 Cl1 90.85(5) 6_557 . ?
N1 Ru1 Cl1 91.09(4) . . ?
N1 Ru1 Cl1 91.09(4) 6_557 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 -0.9(3) . . . . ?
C1 C2 C3 C4 -0.1(3) . . . . ?
C2 C3 C4 C5 0.1(3) . . . . ?
C3 C4 C5 N1 0.8(3) . . . . ?
C3 C4 C5 C6 -176.2(2) . . . . ?
N1 C5 C6 C5 -60.4(3) . . . 6_557 ?
C4 C5 C6 C5 116.7(2) . . . 6_557 ?
N1 C5 C6 C7 -179.0(2) . . . . ?
C4 C5 C6 C7 -1.9(3) . . . . ?
N1 C5 C6 C8 60.7(2) . . . . ?
C4 C5 C6 C8 -122.2(2) . . . . ?
C5 C6 C8 N3 59.79(15) 6_557 . . . ?
C5 C6 C8 N3 -59.80(15) . . . . ?
C7 C6 C8 N3 180 . . . . ?
C5 C6 C8 C9 -120.21(15) 6_557 . . . ?
C5 C6 C8 C9 120.20(15) . . . . ?
C7 C6 C8 C9 0 . . . . ?
N3 C8 C9 C10 0 . . . . ?
C6 C8 C9 C10 180 . . . . ?
C8 C9 C10 C11 0 . . . . ?
C9 C10 C11 C12 0 . . . . ?
C10 C11 C12 N3 0 . . . . ?
C10 C11 C12 C13 180 . . . . ?
N3 C12 C13 C15 59.60(15) . . . . ?
C11 C12 C13 C15 -120.40(15) . . . . ?
N3 C12 C13 C15 -59.60(15) . . . 6_557 ?
C11 C12 C13 C15 120.40(15) . . . 6_557 ?
N3 C12 C13 C14 180 . . . . ?
C11 C12 C13 C14 0 . . . . ?
C15 C13 C15 N2 59.8(3) 6_557 . . . ?
C14 C13 C15 N2 178.62(18) . . . . ?
C12 C13 C15 N2 -61.9(2) . . . . ?
C15 C13 C15 C16 -116.1(2) 6_557 . . . ?
C14 C13 C15 C16 2.7(3) . . . . ?
C12 C13 C15 C16 122.2(2) . . . . ?
N2 C15 C16 C17 -1.4(3) . . . . ?
C13 C15 C16 C17 174.3(2) . . . . ?
C15 C16 C17 C18 -1.1(4) . . . . ?
C16 C17 C18 C19 1.4(4) . . . . ?
C17 C18 C19 N2 0.7(3) . . . . ?
C2 C1 N1 C5 1.8(3) . . . . ?
C2 C1 N1 Ru1 -179.63(16) . . . . ?
C4 C5 N1 C1 -1.8(3) . . . . ?
C6 C5 N1 C1 175.42(18) . . . . ?
C4 C5 N1 Ru1 179.64(15) . . . . ?
C6 C5 N1 Ru1 -3.2(2) . . . . ?
C18 C19 N2 C15 -3.1(3) . . . . ?
C18 C19 N2 Ru1 179.34(16) . . . . ?
C16 C15 N2 C19 3.4(3) . . . . ?
C13 C15 N2 C19 -172.55(17) . . . . ?
C16 C15 N2 Ru1 -178.91(15) . . . . ?
C13 C15 N2 Ru1 5.1(2) . . . . ?
C9 C8 N3 C12 0 . . . . ?
C6 C8 N3 C12 180 . . . . ?
C9 C8 N3 Ru1 180 . . . . ?
C6 C8 N3 Ru1 0 . . . . ?
C11 C12 N3 C8 0 . . . . ?
C13 C12 N3 C8 180 . . . . ?
C11 C12 N3 Ru1 180 . . . . ?
C13 C12 N3 Ru1 0 . . . . ?

# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.000 174 45 ' '
2 0.500 0.500 0.500 174 45 ' '
3 0.500 1.000 0.500 174 45 ' '
4 0.500 1.000 1.000 174 45 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 2.279
1 1 0 2.565
0 2 0 2.352
1 1 1 2.744
0 2 1 2.546
0 0 2 1.948
1 0 2 2.999
2 0 2 4.962
0 2 2 3.055
0 0 4 3.898
1 2 4 5.095
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL SIR97 run in space group P b c m
CELL    8.9368   17.3150   20.9100     90.00     90.00     90.00
SPGR Pbcm
# Solvent Accessible Volume =     715.2
# Electrons Found in S.A.V. =     178.6
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.500 1.000 0.500 !       4.35 eA-3
C102 0.582 0.084 0.421 !       3.22 eA-3
Q103 0.131 0.312 0.244 !       2.56 eA-3
C104 0.530 0.547 0.458 !       2.37 eA-3
C105 0.596 0.039 0.034 !       1.91 eA-3
Q106 0.042 0.250 0.000 !       1.72 eA-3
Q107 0.714 0.250 0.249 !       1.09 eA-3
Q108 0.869 0.031 0.249 !       0.89 eA-3
Q109 0.945 0.745 0.084 !       0.71 eA-3
Q110 0.154 0.472 0.312 !       0.67 eA-3
Q111 0.866 0.359 0.251 !       0.67 eA-3
Q112 0.873 0.922 0.249 !       0.65 eA-3
Q113 0.345 0.922 0.250 !       0.64 eA-3
Q114 0.381 0.796 0.406 !       0.62 eA-3
Q115 0.552 0.797 0.255 !       0.61 eA-3
Q116 0.114 0.548 0.189 !       0.61 eA-3
Q117 0.434 0.353 0.193 !       0.60 eA-3
Q118 0.726 0.797 0.254 !       0.59 eA-3
Q119 0.168 0.188 0.500 !       0.59 eA-3
Q120 0.191 0.594 0.245 !       0.59 eA-3
Q121 0.419 0.869 0.314 !       0.58 eA-3
Q122 0.558 0.016 0.244 !       0.57 eA-3
Q123 0.590 0.656 0.244 !       0.55 eA-3
Q124 0.444 0.656 0.246 !       0.54 eA-3
Q125 0.507 0.781 0.098 !       0.54 eA-3
Q126 0.318 0.847 0.139 !       0.53 eA-3
Q127 0.915 0.316 0.504 !       0.50 eA-3
;

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_OsPY5Me2Cl_PF6
_database_code_depnum_ccdc_archive 'CCDC 1451779'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;

_audit_creation_date             2015-10-01T13:44:10-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
OsPY5Me2Cl_PF6
;
_chemical_formula_moiety         'C29 H25 N5 Cl Os, P1 F6'
_chemical_formula_sum            'C29 H25 Cl1 F6 N5 Os1 P1'
_chemical_formula_weight         814.16
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_H-M   'P b c m'
_symmetry_space_group_name_Hall  '-P 2c 2b'
_symmetry_Int_Tables_number      57
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z+1/2'
'x, -y+1/2, -z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z-1/2'
'-x, y-1/2, z'
'x, -y-1/2, z-1/2'

_cell_length_a                   8.978(2)
_cell_length_b                   17.366(5)
_cell_length_c                   20.947(6)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3265.9(15)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    9853
_cell_measurement_theta_min      3.14
_cell_measurement_theta_max      27.48
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Block
_exptl_crystal_colour            Red
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.09
_exptl_crystal_density_diffrn    1.656
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1584
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    4.096
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.76
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.404
_shelx_estimated_absorpt_T_max   0.709

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'Rotating Anode'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_detector_area_resol_mean 28.57
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_ub_11      0.1114
_diffrn_orient_matrix_ub_12      -0.0024
_diffrn_orient_matrix_ub_13      0.001
_diffrn_orient_matrix_ub_21      0.0013
_diffrn_orient_matrix_ub_22      0.0468
_diffrn_orient_matrix_ub_23      -0.0335
_diffrn_orient_matrix_ub_31      0.0002
_diffrn_orient_matrix_ub_32      0.0278
_diffrn_orient_matrix_ub_33      0.0388
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0362
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_number            22873
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_theta_min         3.211
_diffrn_reflns_theta_max         27.488
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.983
_diffrn_measured_fraction_theta_max 0.983
_diffrn_reflns_Laue_measured_fraction_full 0.983
_diffrn_reflns_Laue_measured_fraction_max 0.983
_diffrn_reflns_point_group_measured_fraction_full 0.983
_diffrn_reflns_point_group_measured_fraction_max 0.983
_reflns_Friedel_coverage         0
_reflns_number_total             3801
_reflns_number_gt                3371
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   geom

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0276P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3801
_refine_ls_number_parameters     215
_refine_ls_number_restraints     2
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0214
_refine_ls_R_factor_gt           0.019
_refine_ls_wR_factor_ref         0.0493
_refine_ls_wR_factor_gt          0.0485
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0
_refine_diff_density_max         1.48
_refine_diff_density_min         -0.791
_refine_diff_density_rms         0.086

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Os Os -1.2165 7.603 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C 0.3855(3) 0.18141(13) 0.86256(11) 0.0256(5) Uani 1 1 d . . . . .
H1 H 0.2818 0.1915 0.8658 0.031 Uiso 1 1 calc R U . . .
C2 C 0.4791(3) 0.21517(16) 0.90637(12) 0.0351(6) Uani 1 1 d . . . . .
H2 H 0.4405 0.2471 0.9393 0.042 Uiso 1 1 calc R U . . .
C3 C 0.6293(3) 0.20169(15) 0.90152(13) 0.0386(6) Uani 1 1 d . . . . .
H3 H 0.6966 0.2236 0.9314 0.046 Uiso 1 1 calc R U . . .
C4 C 0.6808(3) 0.15575(15) 0.85240(13) 0.0324(6) Uani 1 1 d . . . . .
H4 H 0.7846 0.1464 0.8483 0.039 Uiso 1 1 calc R U . . .
C5 C 0.5823(2) 0.12306(12) 0.80888(11) 0.0216(4) Uani 1 1 d . . . . .
C6 C 0.6342(4) 0.07821(16) 0.75 0.0238(7) Uani 1 2 d S T P . .
C7 C 0.8057(4) 0.0733(2) 0.75 0.0321(9) Uani 1 2 d S T P . .
H7A H 0.8392 0.0457 0.7882 0.048 Uiso 0.5 1 calc R U P . .
H7B H 0.8477 0.1254 0.75 0.048 Uiso 1 2 calc R U P . .
H7C H 0.8392 0.0457 0.7118 0.048 Uiso 0.5 1 calc R U P . .
C8 C 0.5716(3) -0.00452(18) 0.75 0.0251(7) Uani 1 2 d S T P . .
C9 C 0.6607(4) -0.0692(2) 0.75 0.0356(9) Uani 1 2 d S T P . .
H9 H 0.766 -0.0635 0.75 0.043 Uiso 1 2 calc R U P . .
C10 C 0.5998(4) -0.1418(2) 0.75 0.0405(9) Uani 1 2 d S T P . .
H10 H 0.6619 -0.1861 0.75 0.049 Uiso 1 2 calc R U P . .
C11 C 0.4473(4) -0.14901(19) 0.75 0.0366(9) Uani 1 2 d S T P . .
H11 H 0.4027 -0.1986 0.75 0.044 Uiso 1 2 calc R U P . .
C12 C 0.3585(4) -0.08314(16) 0.75 0.0252(7) Uani 1 2 d S T P . .
C13 C 0.1878(4) -0.08782(17) 0.75 0.0258(8) Uani 1 2 d S T P . .
C14 C 0.1386(4) -0.17239(18) 0.75 0.0391(9) Uani 1 2 d S T P . .
H14A H 0.1774 -0.1981 0.7882 0.059 Uiso 0.5 1 calc R U P . .
H14B H 0.1774 -0.1981 0.7118 0.059 Uiso 0.5 1 calc R U P . .
H14C H 0.0296 -0.1751 0.75 0.059 Uiso 1 2 calc R U P . .
C15 C 0.1228(2) -0.04773(12) 0.69071(11) 0.0236(5) Uani 1 1 d . . . . .
C16 C 0.0321(3) -0.08542(13) 0.64659(13) 0.0329(6) Uani 1 1 d . . . . .
H16 H 0.0128 -0.1389 0.6514 0.039 Uiso 1 1 calc R U . . .
C17 C -0.0297(3) -0.04583(15) 0.59605(13) 0.0384(6) Uani 1 1 d . . . . .
H17 H -0.0912 -0.0716 0.566 0.046 Uiso 1 1 calc R U . . .
C18 C -0.0006(3) 0.03145(15) 0.59000(11) 0.0317(5) Uani 1 1 d . . . . .
H18 H -0.042 0.0602 0.5557 0.038 Uiso 1 1 calc R U . . .
C19 C 0.0896(2) 0.06666(13) 0.63461(11) 0.0233(5) Uani 1 1 d . . . . .
H19 H 0.1084 0.1202 0.6303 0.028 Uiso 1 1 calc R U . . .
N1 N 0.43294(18) 0.13450(10) 0.81498(8) 0.0189(4) Uani 1 1 d . . . . .
N2 N 0.15271(18) 0.02905(10) 0.68409(8) 0.0188(4) Uani 1 1 d . . . . .
N3 N 0.4195(3) -0.01111(14) 0.75 0.0218(6) Uani 1 2 d S T P . .
F1 F -0.08143(17) 0.31483(8) 0.99596(8) 0.0437(4) Uani 1 1 d . . . . .
F2 F 0.0434(2) 0.24488(10) 0.92418(8) 0.0603(5) Uani 1 1 d . . . . .
F3 F 0.16937(18) 0.18468(10) 1.00260(10) 0.0594(5) Uani 1 1 d . . . . .
P1 P 0.04441(9) 0.25 1 0.02781(18) Uani 1 2 d S T P . .
Cl1 Cl 0.13264(8) 0.19488(4) 0.75 0.02053(15) Uani 1 2 d S T P . .
Os1 Os 0.29007(2) 0.08301(2) 0.75 0.01484(5) Uani 1 2 d S T P . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.356(3) . ?
C1 C2 1.375(3) . ?
C1 H1 0.95 . ?
C2 C3 1.372(4) . ?
C2 H2 0.95 . ?
C3 C4 1.382(4) . ?
C3 H3 0.95 . ?
C4 C5 1.391(3) . ?
C4 H4 0.95 . ?
C5 N1 1.362(2) . ?
C5 C6 1.531(3) . ?
C6 C5 1.531(3) 6_557 ?
C6 C7 1.542(5) . ?
C6 C8 1.543(4) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N3 1.370(4) . ?
C8 C9 1.379(4) . ?
C9 C10 1.374(5) . ?
C9 H9 0.95 . ?
C10 C11 1.375(5) . ?
C10 H10 0.95 . ?
C11 C12 1.394(4) . ?
C11 H11 0.95 . ?
C12 N3 1.366(4) . ?
C12 C13 1.535(5) . ?
C13 C14 1.534(4) . ?
C13 C15 1.539(3) 6_557 ?
C13 C15 1.539(3) . ?
C14 H14A 0.98 . ?
C14 H14B 0.98 . ?
C14 H14C 0.98 . ?
C15 N2 1.367(3) . ?
C15 C16 1.395(3) . ?
C16 C17 1.379(4) . ?
C16 H16 0.95 . ?
C17 C18 1.373(4) . ?
C17 H17 0.95 . ?
C18 C19 1.380(3) . ?
C18 H18 0.95 . ?
C19 N2 1.350(3) . ?
C19 H19 0.95 . ?
N1 Os1 2.0731(17) . ?
N2 Os1 2.0747(17) . ?
N3 Os1 2.005(2) . ?
F1 P1 1.5973(15) . ?
F2 P1 1.5907(17) . ?
F3 P1 1.5964(17) . ?
P1 F2 1.5907(17) 3_557 ?
P1 F3 1.5964(17) 3_557 ?
P1 F1 1.5973(16) 3_557 ?
Cl1 Os1 2.4026(8) . ?
Os1 N1 2.0730(17) 6_557 ?
Os1 N2 2.0747(17) 6_557 ?

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
N1 C1 C2 123.7(2) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 118.6(2) . . ?
C3 C2 H2 120.7 . . ?
C1 C2 H2 120.7 . . ?
C2 C3 C4 118.9(2) . . ?
C2 C3 H3 120.6 . . ?
C4 C3 H3 120.6 . . ?
C3 C4 C5 120.7(2) . . ?
C3 C4 H4 119.7 . . ?
C5 C4 H4 119.7 . . ?
N1 C5 C4 120.3(2) . . ?
N1 C5 C6 116.7(2) . . ?
C4 C5 C6 122.8(2) . . ?
C5 C6 C5 107.3(2) 6_557 . ?
C5 C6 C7 109.37(17) 6_557 . ?
C5 C6 C7 109.37(17) . . ?
C5 C6 C8 111.28(16) 6_557 . ?
C5 C6 C8 111.28(16) . . ?
C7 C6 C8 108.2(2) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N3 C8 C9 120.7(3) . . ?
N3 C8 C6 116.2(3) . . ?
C9 C8 C6 123.2(3) . . ?
C10 C9 C8 121.1(3) . . ?
C10 C9 H9 119.5 . . ?
C8 C9 H9 119.5 . . ?
C9 C10 C11 118.6(3) . . ?
C9 C10 H10 120.7 . . ?
C11 C10 H10 120.7 . . ?
C10 C11 C12 119.7(3) . . ?
C10 C11 H11 120.2 . . ?
C12 C11 H11 120.2 . . ?
N3 C12 C11 121.5(3) . . ?
N3 C12 C13 116.7(2) . . ?
C11 C12 C13 121.9(3) . . ?
C14 C13 C12 109.8(3) . . ?
C14 C13 C15 108.91(18) . 6_557 ?
C12 C13 C15 110.78(17) . 6_557 ?
C14 C13 C15 108.91(18) . . ?
C12 C13 C15 110.78(17) . . ?
C15 C13 C15 107.6(2) 6_557 . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
H14A C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
N2 C15 C16 120.3(2) . . ?
N2 C15 C13 116.6(2) . . ?
C16 C15 C13 123.0(2) . . ?
C17 C16 C15 120.6(2) . . ?
C17 C16 H16 119.7 . . ?
C15 C16 H16 119.7 . . ?
C18 C17 C16 118.8(2) . . ?
C18 C17 H17 120.6 . . ?
C16 C17 H17 120.6 . . ?
C17 C18 C19 118.8(2) . . ?
C17 C18 H18 120.6 . . ?
C19 C18 H18 120.6 . . ?
N2 C19 C18 123.5(2) . . ?
N2 C19 H19 118.2 . . ?
C18 C19 H19 118.2 . . ?
C1 N1 C5 117.78(18) . . ?
C1 N1 Os1 123.18(14) . . ?
C5 N1 Os1 119.00(14) . . ?
C19 N2 C15 117.86(18) . . ?
C19 N2 Os1 122.81(14) . . ?
C15 N2 Os1 119.32(14) . . ?
C12 N3 C8 118.4(3) . . ?
C12 N3 Os1 120.9(2) . . ?
C8 N3 Os1 120.6(2) . . ?
F2 P1 F2 179.36(16) . 3_557 ?
F2 P1 F3 89.90(10) . . ?
F2 P1 F3 90.55(11) 3_557 . ?
F2 P1 F3 90.55(11) . 3_557 ?
F2 P1 F3 89.90(10) 3_557 3_557 ?
F3 P1 F3 90.70(13) . 3_557 ?
F2 P1 F1 88.99(9) . . ?
F2 P1 F1 90.55(10) 3_557 . ?
F3 P1 F1 178.84(10) . . ?
F3 P1 F1 89.68(9) 3_557 . ?
F2 P1 F1 90.55(10) . 3_557 ?
F2 P1 F1 89.00(9) 3_557 3_557 ?
F3 P1 F1 89.68(9) . 3_557 ?
F3 P1 F1 178.84(10) 3_557 3_557 ?
F1 P1 F1 89.96(12) . 3_557 ?
N3 Os1 N1 89.60(7) . 6_557 ?
N3 Os1 N1 89.60(7) . . ?
N1 Os1 N1 82.08(10) 6_557 . ?
N3 Os1 N2 88.65(7) . 6_557 ?
N1 Os1 N2 178.12(6) 6_557 6_557 ?
N1 Os1 N2 97.22(7) . 6_557 ?
N3 Os1 N2 88.65(7) . . ?
N1 Os1 N2 97.22(7) 6_557 . ?
N1 Os1 N2 178.12(6) . . ?
N2 Os1 N2 83.42(10) 6_557 . ?
N3 Os1 Cl1 179.38(7) . . ?
N1 Os1 Cl1 90.87(5) 6_557 . ?
N1 Os1 Cl1 90.87(5) . . ?
N2 Os1 Cl1 90.89(5) 6_557 . ?
N2 Os1 Cl1 90.89(5) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.8(4) . . . . ?
C1 C2 C3 C4 0.9(4) . . . . ?
C2 C3 C4 C5 -0.6(4) . . . . ?
C3 C4 C5 N1 -1.5(4) . . . . ?
C3 C4 C5 C6 174.0(2) . . . . ?
N1 C5 C6 C5 59.6(3) . . . 6_557 ?
C4 C5 C6 C5 -116.0(2) . . . 6_557 ?
N1 C5 C6 C7 178.13(19) . . . . ?
C4 C5 C6 C7 2.5(3) . . . . ?
N1 C5 C6 C8 -62.4(3) . . . . ?
C4 C5 C6 C8 122.0(3) . . . . ?
C5 C6 C8 N3 -59.81(17) 6_557 . . . ?
C5 C6 C8 N3 59.81(17) . . . . ?
C7 C6 C8 N3 180 . . . . ?
C5 C6 C8 C9 120.19(17) 6_557 . . . ?
C5 C6 C8 C9 -120.19(17) . . . . ?
C7 C6 C8 C9 0 . . . . ?
N3 C8 C9 C10 0 . . . . ?
C6 C8 C9 C10 180 . . . . ?
C8 C9 C10 C11 0 . . . . ?
C9 C10 C11 C12 0 . . . . ?
C10 C11 C12 N3 0 . . . . ?
C10 C11 C12 C13 180 . . . . ?
N3 C12 C13 C14 180 . . . . ?
C11 C12 C13 C14 0 . . . . ?
N3 C12 C13 C15 -59.69(16) . . . 6_557 ?
C11 C12 C13 C15 120.31(16) . . . 6_557 ?
N3 C12 C13 C15 59.69(16) . . . . ?
C11 C12 C13 C15 -120.31(16) . . . . ?
C14 C13 C15 N2 178.3(2) . . . . ?
C12 C13 C15 N2 -60.9(2) . . . . ?
C15 C13 C15 N2 60.4(3) 6_557 . . . ?
C14 C13 C15 C16 1.1(3) . . . . ?
C12 C13 C15 C16 121.9(2) . . . . ?
C15 C13 C15 C16 -116.8(2) 6_557 . . . ?
N2 C15 C16 C17 -0.6(4) . . . . ?
C13 C15 C16 C17 176.6(2) . . . . ?
C15 C16 C17 C18 -0.2(4) . . . . ?
C16 C17 C18 C19 0.2(4) . . . . ?
C17 C18 C19 N2 0.5(4) . . . . ?
C2 C1 N1 C5 -2.9(3) . . . . ?
C2 C1 N1 Os1 179.23(18) . . . . ?
C4 C5 N1 C1 3.1(3) . . . . ?
C6 C5 N1 C1 -172.6(2) . . . . ?
C4 C5 N1 Os1 -178.88(17) . . . . ?
C6 C5 N1 Os1 5.4(2) . . . . ?
C18 C19 N2 C15 -1.2(3) . . . . ?
C18 C19 N2 Os1 179.28(17) . . . . ?
C16 C15 N2 C19 1.2(3) . . . . ?
C13 C15 N2 C19 -176.1(2) . . . . ?
C16 C15 N2 Os1 -179.27(17) . . . . ?
C13 C15 N2 Os1 3.4(3) . . . . ?
C11 C12 N3 C8 0 . . . . ?
C13 C12 N3 C8 180 . . . . ?
C11 C12 N3 Os1 180 . . . . ?
C13 C12 N3 Os1 0 . . . . ?
C9 C8 N3 C12 0 . . . . ?
C6 C8 N3 C12 180 . . . . ?
C9 C8 N3 Os1 180 . . . . ?
C6 C8 N3 Os1 0 . . . . ?

# SQUEEZE RESULTS (Version =  30715)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.500 0.500 0.000 182 46 ' '
2 0.500 0.500 0.500 182 46 ' '
3 0.500 1.000 0.500 182 46 ' '
4 0.500 1.000 1.000 182 46 ' '
# Missing Reflections Below sin(th)/lambda = 0.25
loop_
_platon_missing_refln_index_h
_platon_missing_refln_index_k
_platon_missing_refln_index_l
_platon_missing_refln_theta
1 0 0 2.268
3 0 0 6.820
1 1 0 2.554
0 2 0 2.346
1 3 0 4.189
3 3 0 7.682
1 4 0 5.217
2 4 0 6.539
0 6 0 7.053
3 6 0 9.835
0 8 0 9.422
1 1 1 2.733
0 2 1 2.539
2 2 1 5.205
2 4 1 6.611
0 0 2 1.944
1 0 2 2.988
2 0 2 4.941
0 2 2 3.047
1 3 2 4.620
0 4 2 5.083
0 6 2 7.318
2 6 2 8.626
1 1 3 3.879
0 2 3 3.745
0 4 3 5.531
0 0 4 3.891
2 0 4 5.985
1 2 4 5.082
2 6 4 9.270
1 1 5 5.498
0 4 5 6.770
0 0 6 5.842
0 6 6 9.177
0 0 8 7.800
_platon_squeeze_void_probe_radius 1.20
_platon_squeeze_details          
;
TITL SIR97 run in space group P b c m
CELL    8.9780   17.3660   20.9470     90.00     90.00     90.00
SPGR Pbcm
# Solvent Accessible Volume =     750.4
# Electrons Found in S.A.V. =     181.8
# Note: Atoms in Void as Cxxx and Qxxx all others
C101 0.500 0.500 0.500 !       3.60 eA-3
C102 0.418 0.570 0.076 !       2.83 eA-3
C103 0.534 0.543 0.458 !       2.06 eA-3
C104 0.432 0.517 0.461 !       1.73 eA-3
C105 0.592 0.040 0.028 !       1.69 eA-3
Q106 0.713 0.250 0.249 !       1.40 eA-3
Q107 0.132 0.422 0.247 !       1.12 eA-3
Q108 0.137 0.312 0.246 !       0.98 eA-3
Q109 0.879 0.031 0.251 !       0.61 eA-3
Q110 0.496 0.876 0.189 !       0.54 eA-3
Q111 0.313 0.922 0.249 !       0.53 eA-3
Q112 0.029 0.250 0.000 !       0.53 eA-3
Q113 0.313 0.375 0.248 !       0.53 eA-3
Q114 0.383 0.374 0.207 !       0.51 eA-3
;
# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_FePY5Me2OH2_PF6
_database_code_depnum_ccdc_archive 'CCDC 1451780'
_audit_update_record             
;
2016-10-07 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;

_audit_creation_date             2015-10-01T14:38:01-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
FePY5Me2OH2_PF6
;
_chemical_formula_moiety         'C29 H27 N5 O1 Fe, 2(P1 F6)'
_chemical_formula_sum            'C29 H33 F12 Fe N5 O4 P2'
_chemical_formula_weight         861.39
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_Int_Tables_number      2
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.6708(3)
_cell_length_b                   12.9661(3)
_cell_length_c                   13.4037(4)
_cell_angle_alpha                72.8880(10)
_cell_angle_beta                 65.5780(10)
_cell_angle_gamma                66.9360(10)
_cell_volume                     1677.90(8)
_cell_formula_units_Z            2
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    15259
_cell_measurement_theta_min      3.03
_cell_measurement_theta_max      27.46
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       platelet
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_exptl_crystal_density_diffrn    1.705
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             876
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.657
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'ABSCOR (Rigaku, 1955)'
_exptl_absorpt_correction_T_min  0.71
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.937
_shelx_estimated_absorpt_T_max   0.937

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_source                   'rotating anode'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_detector                 'curved image-plate'
_diffrn_detector_area_resol_mean 10
_diffrn_orient_matrix_type       fs_process
_diffrn_orient_matrix_ub_11      0.08406
_diffrn_orient_matrix_ub_12      -0.041805
_diffrn_orient_matrix_ub_13      -0.053434
_diffrn_orient_matrix_ub_21      0.051678
_diffrn_orient_matrix_ub_22      0.028037
_diffrn_orient_matrix_ub_23      0.023975
_diffrn_orient_matrix_ub_31      0.007946
_diffrn_orient_matrix_ub_32      -0.068355
_diffrn_orient_matrix_ub_33      0.058783
_diffrn_measurement_device_type  'Rigaku R-Axis Rapid'
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_av_unetI/netI     0.0263
_diffrn_reflns_number            16616
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.037
_diffrn_reflns_theta_max         27.465
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_reflns_Friedel_coverage         0
_reflns_number_total             7611
_reflns_number_gt                6804
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_cell_refinement       'CrystalClear (Rigaku/MSC Inc., 2006)'
_computing_data_reduction        
'CrystalClear (Rigaku/MSC Inc., 2006), SORTAV (Blessing, 1995)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0695P)²+0.3549P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         7611
_refine_ls_number_parameters     640
_refine_ls_number_restraints     54
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0381
_refine_ls_R_factor_gt           0.0342
_refine_ls_wR_factor_ref         0.1083
_refine_ls_wR_factor_gt          0.1053
_refine_ls_goodness_of_fit_ref   1.111
_refine_ls_restrained_S_all      1.126
_refine_ls_shift/su_max          0.01
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.565
_refine_diff_density_min         -0.339
_refine_diff_density_rms         0.075

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_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
C1 C 0.09555(17) -0.01992(13) 0.16107(13) 0.0237(3) Uani 1 1 d . . . . .
H1 H 0.1831 -0.0444 0.1624 0.028 Uiso 1 1 calc R U . . .
C2 C 0.04921(18) -0.09882(14) 0.15258(14) 0.0275(3) Uani 1 1 d . . . . .
H2 H 0.1035 -0.1756 0.1493 0.033 Uiso 1 1 calc R U . . .
C3 C -0.07678(19) -0.06477(15) 0.14885(15) 0.0292(4) Uani 1 1 d . . . . .
H3 H -0.1128 -0.1179 0.1464 0.035 Uiso 1 1 calc R U . . .
C4 C -0.14977(17) 0.04974(14) 0.14875(14) 0.0266(3) Uani 1 1 d . . . . .
H4 H -0.2358 0.0762 0.1438 0.032 Uiso 1 1 calc R U . . .
C5 C -0.09658(15) 0.12542(13) 0.15582(12) 0.0202(3) Uani 1 1 d . . . . .
C6 C -0.16720(15) 0.25405(13) 0.14526(13) 0.0214(3) Uani 1 1 d . . . . .
C7 C -0.29415(17) 0.28203(15) 0.12020(16) 0.0292(4) Uani 1 1 d . . . . .
H7A H -0.3559 0.2471 0.1828 0.044 Uiso 1 1 calc R U . . .
H7B H -0.2722 0.2524 0.053 0.044 Uiso 1 1 calc R U . . .
H7C H -0.3354 0.3645 0.1088 0.044 Uiso 1 1 calc R U . . .
C8 C 0.13112(17) 0.34393(14) -0.02126(14) 0.0254(3) Uani 1 1 d . . . . .
H8 H 0.2108 0.336 -0.0121 0.031 Uiso 1 1 calc R U . . .
C9 C 0.11264(18) 0.40188(14) -0.12072(14) 0.0285(4) Uani 1 1 d . . . . .
H9 H 0.1779 0.4326 -0.1781 0.034 Uiso 1 1 calc R U . . .
C10 C -0.00256(19) 0.41397(14) -0.13464(14) 0.0301(4) Uani 1 1 d . . . . .
H10 H -0.0181 0.4524 -0.2023 0.036 Uiso 1 1 calc R U . . .
C11 C -0.09541(18) 0.36906(14) -0.04822(15) 0.0280(3) Uani 1 1 d . . . . .
H11 H -0.1763 0.3778 -0.0558 0.034 Uiso 1 1 calc R U . . .
C12 C -0.07066(16) 0.31099(13) 0.04993(13) 0.0215(3) Uani 1 1 d . . . . .
C13 C -0.19937(15) 0.29369(13) 0.25350(13) 0.0213(3) Uani 1 1 d . . . . .
C14 C -0.32815(17) 0.35025(15) 0.31317(16) 0.0299(4) Uani 1 1 d . . . . .
H14 H -0.3981 0.3673 0.2862 0.036 Uiso 1 1 calc R U . . .
C15 C -0.35367(18) 0.38150(17) 0.41180(18) 0.0358(4) Uani 1 1 d . . . . .
H15 H -0.4413 0.4207 0.4533 0.043 Uiso 1 1 calc R U . . .
C16 C -0.25100(18) 0.35545(15) 0.44962(16) 0.0303(4) Uani 1 1 d . . . . .
H16 H -0.2673 0.3759 0.5179 0.036 Uiso 1 1 calc R U . . .
C17 C -0.12317(16) 0.29902(13) 0.38728(13) 0.0216(3) Uani 1 1 d . . . . .
C18 C -0.00571(16) 0.26890(13) 0.42515(13) 0.0220(3) Uani 1 1 d . . . . .
C19 C -0.05364(18) 0.30397(16) 0.53953(14) 0.0291(4) Uani 1 1 d . . . . .
H19A H -0.0993 0.3859 0.5348 0.044 Uiso 1 1 calc R U . . .
H19B H 0.0226 0.2854 0.5626 0.044 Uiso 1 1 calc R U . . .
H19C H -0.1146 0.263 0.594 0.044 Uiso 1 1 calc R U . . .
C20 C 0.09404(16) 0.32887(13) 0.33893(13) 0.0213(3) Uani 1 1 d . . . . .
C21 C 0.13631(18) 0.39864(14) 0.36831(14) 0.0268(3) Uani 1 1 d . . . . .
H21 H 0.0944 0.4189 0.4405 0.032 Uiso 1 1 calc R U . . .
C22 C 0.23968(19) 0.43870(15) 0.29215(15) 0.0290(4) Uani 1 1 d . . . . .
H22 H 0.2691 0.4865 0.3114 0.035 Uiso 1 1 calc R U . . .
C23 C 0.29865(17) 0.40771(14) 0.18826(15) 0.0266(3) Uani 1 1 d . . . . .
H23 H 0.3711 0.432 0.1349 0.032 Uiso 1 1 calc R U . . .
C24 C 0.24993(16) 0.34038(13) 0.16335(13) 0.0222(3) Uani 1 1 d . . . . .
H24 H 0.2911 0.3193 0.0915 0.027 Uiso 1 1 calc R U . . .
C25 C 0.07248(15) 0.14139(13) 0.42992(13) 0.0210(3) Uani 1 1 d . . . . .
C26 C 0.09978(18) 0.07497(15) 0.52490(14) 0.0276(3) Uani 1 1 d . . . . .
H26 H 0.0565 0.1039 0.5931 0.033 Uiso 1 1 calc R U . . .
C27 C 0.18984(19) -0.03315(16) 0.52017(15) 0.0308(4) Uani 1 1 d . . . . .
H27 H 0.2089 -0.0789 0.5847 0.037 Uiso 1 1 calc R U . . .
C28 C 0.25140(17) -0.07327(14) 0.42036(15) 0.0275(3) Uani 1 1 d . . . . .
H28 H 0.3161 -0.146 0.4139 0.033 Uiso 1 1 calc R U . . .
C29 C 0.21661(16) -0.00492(13) 0.32979(14) 0.0227(3) Uani 1 1 d . . . . .
H29 H 0.2583 -0.0332 0.2613 0.027 Uiso 1 1 calc R U . . .
N1 N 0.02333(13) 0.09014(11) 0.16755(10) 0.0188(3) Uani 1 1 d . . . . .
N2 N 0.04345(13) 0.29797(11) 0.06344(11) 0.0199(3) Uani 1 1 d . . . . .
N3 N -0.09726(13) 0.26962(10) 0.28918(11) 0.0189(3) Uani 1 1 d . . . . .
N4 N 0.14730(13) 0.30278(11) 0.23508(11) 0.0191(3) Uani 1 1 d . . . . .
N5 N 0.12656(13) 0.09995(11) 0.33326(11) 0.0187(2) Uani 1 1 d . . . . .
O1 O 0.26736(11) 0.12518(10) 0.10441(10) 0.0227(2) Uani 1 1 d . . . . .
O2 O 0.32402(16) 0.11075(15) -0.10243(13) 0.0404(3) Uani 1 1 d . . . . .
O3 O 0.49013(13) 0.10009(12) 0.14063(13) 0.0341(3) Uani 1 1 d . . . . .
O4 O 0.5127(4) 0.1010(4) 0.3281(2) 0.0904(9) Uani 1 1 d . . . . .
Fe1 Fe 0.08362(2) 0.19907(2) 0.19909(2) 0.01632(8) Uani 1 1 d . . . . .
P1 P 0.56814(17) 0.32434(15) 0.84233(15) 0.0206(5) Uani 0.767(6) 1 d . . P A 1
F1 F 0.5848(4) 0.2278(3) 0.9452(3) 0.0946(14) Uani 0.767(6) 1 d . U P A 1
F2 F 0.5618(2) 0.4187(2) 0.7358(2) 0.0599(8) Uani 0.767(6) 1 d . U P A 1
F3 F 0.6466(3) 0.2316(2) 0.7654(3) 0.0692(9) Uani 0.767(6) 1 d . U P A 1
F4 F 0.4970(3) 0.4202(4) 0.9171(4) 0.1090(16) Uani 0.767(6) 1 d . U P A 1
F5 F 0.7129(3) 0.3298(3) 0.8224(3) 0.0496(8) Uani 0.767(6) 1 d . . P A 1
F6 F 0.4285(7) 0.3164(7) 0.8651(7) 0.0619(15) Uani 0.767(6) 1 d . . P A 1
P1A P 0.5663(9) 0.3250(8) 0.8404(7) 0.052(3) Uani 0.233(6) 1 d . . P A 2
F1A F 0.5241(7) 0.3132(12) 0.9744(5) 0.071(3) Uani 0.233(6) 1 d . U P A 2
F2A F 0.6080(7) 0.1887(6) 0.8649(13) 0.093(5) Uani 0.233(6) 1 d . U P A 2
F3A F 0.6084(11) 0.3207(15) 0.7203(6) 0.109(5) Uani 0.233(6) 1 d . U P A 2
F4A F 0.5219(6) 0.4505(5) 0.8244(11) 0.075(4) Uani 0.233(6) 1 d . U P A 2
F5A F 0.6828(10) 0.3450(9) 0.8490(8) 0.036(2) Uani 0.233(6) 1 d . U P A 2
F6A F 0.439(2) 0.310(3) 0.839(2) 0.096(8) Uani 0.233(6) 1 d . . P A 2
P2 P 0.3324(3) 0.2441(2) 0.5850(3) 0.0356(4) Uani 0.675(4) 1 d . . P B 3
F7 F 0.3383(3) 0.1195(2) 0.6539(2) 0.0758(10) Uani 0.675(4) 1 d . . P B 3
F8 F 0.3278(4) 0.3662(2) 0.5144(3) 0.0703(11) Uani 0.675(4) 1 d . . P B 3
F9 F 0.3666(3) 0.2740(3) 0.6742(2) 0.0652(8) Uani 0.675(4) 1 d . . P B 3
F10 F 0.2956(6) 0.2120(5) 0.4961(3) 0.0432(8) Uani 0.675(4) 1 d . . P B 3
F11 F 0.4851(4) 0.1975(5) 0.5159(3) 0.0628(10) Uani 0.675(4) 1 d . . P B 3
F12 F 0.1793(2) 0.2884(3) 0.6519(3) 0.0785(12) Uani 0.675(4) 1 d . . P B 3
P2A P 0.3206(7) 0.2808(4) 0.5827(6) 0.0349(9) Uani 0.325(4) 1 d . . P B 4
F7A F 0.2617(7) 0.2223(7) 0.7050(5) 0.095(3) Uani 0.325(4) 1 d . . P B 4
F8A F 0.3765(8) 0.3429(9) 0.4638(5) 0.079(3) Uani 0.325(4) 1 d . . P B 4
F9A F 0.3746(6) 0.3447(7) 0.6302(5) 0.0701(18) Uani 0.325(4) 1 d . . P B 4
F10A F 0.2725(14) 0.2142(12) 0.5360(9) 0.066(3) Uani 0.325(4) 1 d . . P B 4
F11A F 0.1850(5) 0.3795(5) 0.5995(5) 0.0596(16) Uani 0.325(4) 1 d . . P B 4
F12A F 0.4572(10) 0.1784(10) 0.5658(9) 0.090(3) Uani 0.325(4) 1 d . . P B 4
H30 H 0.331(2) 0.1190(18) 0.1196(19) 0.029(5) Uiso 1 1 d . . . . .
H31 H 0.287(2) 0.1217(18) 0.034(2) 0.031(5) Uiso 1 1 d . . . . .
H34 H 0.521(3) 0.149(2) 0.088(3) 0.055(8) Uiso 1 1 d . . . . .
H37 H 0.452(4) 0.131(3) 0.376(4) 0.092(14) Uiso 1 1 d . . . . .
H32 H 0.373(4) 0.054(3) -0.113(3) 0.077(11) Uiso 1 1 d . . . . .
H36 H 0.535(2) 0.038(2) 0.345(2) 0.022(7) Uiso 1 1 d . . . . .
H35 H 0.488(3) 0.105(3) 0.203(3) 0.070(10) Uiso 1 1 d . . . . .
H33 H 0.341(4) 0.157(3) -0.165(3) 0.093(12) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.351(2) . ?
C1 C2 1.380(2) . ?
C1 H1 0.95 . ?
C2 C3 1.378(3) . ?
C2 H2 0.95 . ?
C3 C4 1.393(2) . ?
C3 H3 0.95 . ?
C4 C5 1.392(2) . ?
C4 H4 0.95 . ?
C5 N1 1.353(2) . ?
C5 C6 1.537(2) . ?
C6 C13 1.532(2) . ?
C6 C12 1.534(2) . ?
C6 C7 1.536(2) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N2 1.345(2) . ?
C8 C9 1.382(2) . ?
C8 H8 0.95 . ?
C9 C10 1.375(3) . ?
C9 H9 0.95 . ?
C10 C11 1.384(3) . ?
C10 H10 0.95 . ?
C11 C12 1.394(2) . ?
C11 H11 0.95 . ?
C12 N2 1.356(2) . ?
C13 N3 1.356(2) . ?
C13 C14 1.387(2) . ?
C14 C15 1.377(3) . ?
C14 H14 0.95 . ?
C15 C16 1.375(3) . ?
C15 H15 0.95 . ?
C16 C17 1.390(2) . ?
C16 H16 0.95 . ?
C17 N3 1.357(2) . ?
C17 C18 1.526(2) . ?
C18 C20 1.537(2) . ?
C18 C19 1.540(2) . ?
C18 C25 1.541(2) . ?
C19 H19A 0.98 . ?
C19 H19B 0.98 . ?
C19 H19C 0.98 . ?
C20 N4 1.355(2) . ?
C20 C21 1.392(2) . ?
C21 C22 1.388(3) . ?
C21 H21 0.95 . ?
C22 C23 1.376(3) . ?
C22 H22 0.95 . ?
C23 C24 1.384(2) . ?
C23 H23 0.95 . ?
C24 N4 1.351(2) . ?
C24 H24 0.95 . ?
C25 N5 1.354(2) . ?
C25 C26 1.393(2) . ?
C26 C27 1.384(3) . ?
C26 H26 0.95 . ?
C27 C28 1.378(3) . ?
C27 H27 0.95 . ?
C28 C29 1.384(2) . ?
C28 H28 0.95 . ?
C29 N5 1.354(2) . ?
C29 H29 0.95 . ?
N1 Fe1 2.0112(13) . ?
N2 Fe1 2.0080(13) . ?
N3 Fe1 1.9443(13) . ?
N4 Fe1 2.0137(13) . ?
N5 Fe1 2.0043(13) . ?
O1 Fe1 1.9956(11) . ?
O1 H30 0.82(2) . ?
O1 H31 0.89(2) . ?
O2 H32 0.75(4) . ?
O2 H33 0.87(4) . ?
O3 H34 0.86(3) . ?
O3 H35 0.84(3) . ?
O4 H37 0.79(4) . ?
O4 H36 0.75(2) . ?
P1 F3 1.560(3) . ?
P1 F6 1.570(8) . ?
P1 F4 1.573(3) . ?
P1 F1 1.587(3) . ?
P1 F2 1.590(2) . ?
P1 F5 1.625(3) . ?
P1A F4A 1.479(11) . ?
P1A F3A 1.488(11) . ?
P1A F5A 1.534(14) . ?
P1A F6A 1.57(3) . ?
P1A F2A 1.608(12) . ?
P1A F1A 1.630(11) . ?
P2 F12 1.581(4) . ?
P2 F8 1.581(4) . ?
P2 F11 1.588(5) . ?
P2 F9 1.590(4) . ?
P2 F7 1.598(3) . ?
P2 F10 1.622(5) . ?
P2A F8A 1.553(10) . ?
P2A F10A 1.561(13) . ?
P2A F7A 1.574(8) . ?
P2A F11A 1.575(7) . ?
P2A F9A 1.594(8) . ?
P2A F12A 1.605(11) . ?

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
N1 C1 C2 123.62(16) . . ?
N1 C1 H1 118.2 . . ?
C2 C1 H1 118.2 . . ?
C3 C2 C1 119.13(15) . . ?
C3 C2 H2 120.4 . . ?
C1 C2 H2 120.4 . . ?
C2 C3 C4 118.03(16) . . ?
C2 C3 H3 121 . . ?
C4 C3 H3 121 . . ?
C5 C4 C3 119.99(16) . . ?
C5 C4 H4 120 . . ?
C3 C4 H4 120 . . ?
N1 C5 C4 121.69(14) . . ?
N1 C5 C6 116.13(13) . . ?
C4 C5 C6 122.12(14) . . ?
C13 C6 C12 109.47(13) . . ?
C13 C6 C7 110.62(13) . . ?
C12 C6 C7 110.46(13) . . ?
C13 C6 C5 109.05(12) . . ?
C12 C6 C5 107.10(12) . . ?
C7 C6 C5 110.06(13) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 124.15(16) . . ?
N2 C8 H8 117.9 . . ?
C9 C8 H8 117.9 . . ?
C10 C9 C8 118.34(17) . . ?
C10 C9 H9 120.8 . . ?
C8 C9 H9 120.8 . . ?
C9 C10 C11 118.73(16) . . ?
C9 C10 H10 120.6 . . ?
C11 C10 H10 120.6 . . ?
C10 C11 C12 120.20(16) . . ?
C10 C11 H11 119.9 . . ?
C12 C11 H11 119.9 . . ?
N2 C12 C11 121.18(15) . . ?
N2 C12 C6 116.81(13) . . ?
C11 C12 C6 121.95(15) . . ?
N3 C13 C14 121.57(15) . . ?
N3 C13 C6 117.26(13) . . ?
C14 C13 C6 121.16(15) . . ?
C15 C14 C13 119.44(16) . . ?
C15 C14 H14 120.3 . . ?
C13 C14 H14 120.3 . . ?
C16 C15 C14 119.34(16) . . ?
C16 C15 H15 120.3 . . ?
C14 C15 H15 120.3 . . ?
C15 C16 C17 119.55(16) . . ?
C15 C16 H16 120.2 . . ?
C17 C16 H16 120.2 . . ?
N3 C17 C16 121.32(15) . . ?
N3 C17 C18 117.08(13) . . ?
C16 C17 C18 121.60(15) . . ?
C17 C18 C20 109.51(13) . . ?
C17 C18 C19 110.08(13) . . ?
C20 C18 C19 110.55(13) . . ?
C17 C18 C25 111.85(12) . . ?
C20 C18 C25 104.71(12) . . ?
C19 C18 C25 110.03(14) . . ?
C18 C19 H19A 109.5 . . ?
C18 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C18 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
N4 C20 C21 121.50(15) . . ?
N4 C20 C18 116.64(13) . . ?
C21 C20 C18 121.62(14) . . ?
C22 C21 C20 120.05(16) . . ?
C22 C21 H21 120 . . ?
C20 C21 H21 120 . . ?
C23 C22 C21 118.64(15) . . ?
C23 C22 H22 120.7 . . ?
C21 C22 H22 120.7 . . ?
C22 C23 C24 118.48(15) . . ?
C22 C23 H23 120.8 . . ?
C24 C23 H23 120.8 . . ?
N4 C24 C23 123.94(15) . . ?
N4 C24 H24 118 . . ?
C23 C24 H24 118 . . ?
N5 C25 C26 121.21(15) . . ?
N5 C25 C18 116.43(13) . . ?
C26 C25 C18 121.94(14) . . ?
C27 C26 C25 120.13(16) . . ?
C27 C26 H26 119.9 . . ?
C25 C26 H26 119.9 . . ?
C28 C27 C26 118.90(16) . . ?
C28 C27 H27 120.6 . . ?
C26 C27 H27 120.6 . . ?
C27 C28 C29 118.31(16) . . ?
C27 C28 H28 120.8 . . ?
C29 C28 H28 120.8 . . ?
N5 C29 C28 123.71(15) . . ?
N5 C29 H29 118.1 . . ?
C28 C29 H29 118.1 . . ?
C1 N1 C5 117.21(14) . . ?
C1 N1 Fe1 122.95(11) . . ?
C5 N1 Fe1 119.80(10) . . ?
C8 N2 C12 117.39(14) . . ?
C8 N2 Fe1 122.63(11) . . ?
C12 N2 Fe1 119.66(11) . . ?
C13 N3 C17 118.77(13) . . ?
C13 N3 Fe1 120.63(10) . . ?
C17 N3 Fe1 120.57(11) . . ?
C24 N4 C20 117.23(13) . . ?
C24 N4 Fe1 123.13(11) . . ?
C20 N4 Fe1 119.37(10) . . ?
C29 N5 C25 117.54(14) . . ?
C29 N5 Fe1 122.66(11) . . ?
C25 N5 Fe1 119.58(10) . . ?
Fe1 O1 H30 120.5(15) . . ?
Fe1 O1 H31 122.0(14) . . ?
H30 O1 H31 114(2) . . ?
H32 O2 H33 106(4) . . ?
H34 O3 H35 113(3) . . ?
H37 O4 H36 112(4) . . ?
N3 Fe1 O1 178.44(5) . . ?
N3 Fe1 N5 91.64(5) . . ?
O1 Fe1 N5 89.14(5) . . ?
N3 Fe1 N2 89.15(5) . . ?
O1 Fe1 N2 90.08(5) . . ?
N5 Fe1 N2 179.16(5) . . ?
N3 Fe1 N1 89.99(5) . . ?
O1 Fe1 N1 88.58(5) . . ?
N5 Fe1 N1 95.96(5) . . ?
N2 Fe1 N1 84.31(5) . . ?
N3 Fe1 N4 90.65(5) . . ?
O1 Fe1 N4 90.80(5) . . ?
N5 Fe1 N4 81.69(5) . . ?
N2 Fe1 N4 98.02(5) . . ?
N1 Fe1 N4 177.59(5) . . ?
F3 P1 F6 95.1(3) . . ?
F3 P1 F4 176.4(2) . . ?
F6 P1 F4 88.3(3) . . ?
F3 P1 F1 88.8(2) . . ?
F6 P1 F1 90.8(4) . . ?
F4 P1 F1 92.1(3) . . ?
F3 P1 F2 89.25(19) . . ?
F6 P1 F2 92.6(4) . . ?
F4 P1 F2 89.6(2) . . ?
F1 P1 F2 176.2(2) . . ?
F3 P1 F5 85.0(2) . . ?
F6 P1 F5 178.2(4) . . ?
F4 P1 F5 91.5(2) . . ?
F1 P1 F5 87.37(18) . . ?
F2 P1 F5 89.19(16) . . ?
F4A P1A F3A 93.7(10) . . ?
F4A P1A F5A 79.8(7) . . ?
F3A P1A F5A 103.1(7) . . ?
F4A P1A F6A 97.5(13) . . ?
F3A P1A F6A 80.8(12) . . ?
F5A P1A F6A 175.3(12) . . ?
F4A P1A F2A 176.6(9) . . ?
F3A P1A F2A 89.2(9) . . ?
F5A P1A F2A 101.2(8) . . ?
F6A P1A F2A 81.2(13) . . ?
F4A P1A F1A 93.1(8) . . ?
F3A P1A F1A 173.1(11) . . ?
F5A P1A F1A 78.8(7) . . ?
F6A P1A F1A 97.6(12) . . ?
F2A P1A F1A 83.9(8) . . ?
F12 P2 F8 90.6(3) . . ?
F12 P2 F11 178.2(3) . . ?
F8 P2 F11 89.9(3) . . ?
F12 P2 F9 90.7(2) . . ?
F8 P2 F9 90.7(2) . . ?
F11 P2 F9 91.0(3) . . ?
F12 P2 F7 90.1(3) . . ?
F8 P2 F7 178.7(3) . . ?
F11 P2 F7 89.3(2) . . ?
F9 P2 F7 90.3(2) . . ?
F12 P2 F10 88.6(3) . . ?
F8 P2 F10 90.2(3) . . ?
F11 P2 F10 89.7(3) . . ?
F9 P2 F10 178.8(3) . . ?
F7 P2 F10 88.7(3) . . ?
F8A P2A F10A 90.1(6) . . ?
F8A P2A F7A 177.8(6) . . ?
F10A P2A F7A 91.5(6) . . ?
F8A P2A F11A 89.5(5) . . ?
F10A P2A F11A 91.0(7) . . ?
F7A P2A F11A 89.0(5) . . ?
F8A P2A F9A 90.1(5) . . ?
F10A P2A F9A 177.8(7) . . ?
F7A P2A F9A 88.3(5) . . ?
F11A P2A F9A 91.2(4) . . ?
F8A P2A F12A 91.1(6) . . ?
F10A P2A F12A 88.0(7) . . ?
F7A P2A F12A 90.5(6) . . ?
F11A P2A F12A 178.8(7) . . ?
F9A P2A F12A 89.9(6) . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 0.9(3) . . . . ?
C1 C2 C3 C4 2.9(3) . . . . ?
C2 C3 C4 C5 -2.0(3) . . . . ?
C3 C4 C5 N1 -2.8(2) . . . . ?
C3 C4 C5 C6 174.24(15) . . . . ?
N1 C5 C6 C13 -64.48(17) . . . . ?
C4 C5 C6 C13 118.33(16) . . . . ?
N1 C5 C6 C12 53.89(17) . . . . ?
C4 C5 C6 C12 -123.31(16) . . . . ?
N1 C5 C6 C7 174.00(14) . . . . ?
C4 C5 C6 C7 -3.2(2) . . . . ?
N2 C8 C9 C10 0.2(3) . . . . ?
C8 C9 C10 C11 0.8(3) . . . . ?
C9 C10 C11 C12 -1.2(3) . . . . ?
C10 C11 C12 N2 0.5(2) . . . . ?
C10 C11 C12 C6 -176.47(15) . . . . ?
C13 C6 C12 N2 54.83(17) . . . . ?
C7 C6 C12 N2 176.88(13) . . . . ?
C5 C6 C12 N2 -63.25(17) . . . . ?
C13 C6 C12 C11 -128.03(15) . . . . ?
C7 C6 C12 C11 -6.0(2) . . . . ?
C5 C6 C12 C11 113.88(16) . . . . ?
C12 C6 C13 N3 -61.19(17) . . . . ?
C7 C6 C13 N3 176.85(14) . . . . ?
C5 C6 C13 N3 55.67(18) . . . . ?
C12 C6 C13 C14 119.81(16) . . . . ?
C7 C6 C13 C14 -2.1(2) . . . . ?
C5 C6 C13 C14 -123.33(16) . . . . ?
N3 C13 C14 C15 -0.9(3) . . . . ?
C6 C13 C14 C15 178.05(16) . . . . ?
C13 C14 C15 C16 -0.4(3) . . . . ?
C14 C15 C16 C17 0.6(3) . . . . ?
C15 C16 C17 N3 0.4(3) . . . . ?
C15 C16 C17 C18 179.56(16) . . . . ?
N3 C17 C18 C20 60.50(17) . . . . ?
C16 C17 C18 C20 -118.66(17) . . . . ?
N3 C17 C18 C19 -177.76(13) . . . . ?
C16 C17 C18 C19 3.1(2) . . . . ?
N3 C17 C18 C25 -55.11(18) . . . . ?
C16 C17 C18 C25 125.73(16) . . . . ?
C17 C18 C20 N4 -60.50(18) . . . . ?
C19 C18 C20 N4 178.05(14) . . . . ?
C25 C18 C20 N4 59.58(17) . . . . ?
C17 C18 C20 C21 125.01(16) . . . . ?
C19 C18 C20 C21 3.6(2) . . . . ?
C25 C18 C20 C21 -114.91(16) . . . . ?
N4 C20 C21 C22 -3.2(3) . . . . ?
C18 C20 C21 C22 171.03(15) . . . . ?
C20 C21 C22 C23 -0.2(3) . . . . ?
C21 C22 C23 C24 1.7(3) . . . . ?
C22 C23 C24 N4 0.0(3) . . . . ?
C17 C18 C25 N5 60.59(18) . . . . ?
C20 C18 C25 N5 -57.92(17) . . . . ?
C19 C18 C25 N5 -176.73(13) . . . . ?
C17 C18 C25 C26 -126.82(16) . . . . ?
C20 C18 C25 C26 114.67(16) . . . . ?
C19 C18 C25 C26 -4.1(2) . . . . ?
N5 C25 C26 C27 4.0(3) . . . . ?
C18 C25 C26 C27 -168.23(16) . . . . ?
C25 C26 C27 C28 0.0(3) . . . . ?
C26 C27 C28 C29 -2.4(3) . . . . ?
C27 C28 C29 N5 0.9(3) . . . . ?
C2 C1 N1 C5 -5.6(2) . . . . ?
C2 C1 N1 Fe1 172.06(13) . . . . ?
C4 C5 N1 C1 6.4(2) . . . . ?
C6 C5 N1 C1 -170.78(14) . . . . ?
C4 C5 N1 Fe1 -171.29(12) . . . . ?
C6 C5 N1 Fe1 11.50(18) . . . . ?
C9 C8 N2 C12 -0.8(2) . . . . ?
C9 C8 N2 Fe1 172.62(13) . . . . ?
C11 C12 N2 C8 0.4(2) . . . . ?
C6 C12 N2 C8 177.60(13) . . . . ?
C11 C12 N2 Fe1 -173.19(12) . . . . ?
C6 C12 N2 Fe1 3.98(18) . . . . ?
C14 C13 N3 C17 1.9(2) . . . . ?
C6 C13 N3 C17 -177.08(13) . . . . ?
C14 C13 N3 Fe1 -175.99(12) . . . . ?
C6 C13 N3 Fe1 5.02(18) . . . . ?
C16 C17 N3 C13 -1.7(2) . . . . ?
C18 C17 N3 C13 179.16(13) . . . . ?
C16 C17 N3 Fe1 176.23(12) . . . . ?
C18 C17 N3 Fe1 -2.93(18) . . . . ?
C23 C24 N4 C20 -3.2(2) . . . . ?
C23 C24 N4 Fe1 -177.14(12) . . . . ?
C21 C20 N4 C24 4.8(2) . . . . ?
C18 C20 N4 C24 -169.74(14) . . . . ?
C21 C20 N4 Fe1 178.92(12) . . . . ?
C18 C20 N4 Fe1 4.43(18) . . . . ?
C28 C29 N5 C25 3.0(2) . . . . ?
C28 C29 N5 Fe1 177.58(12) . . . . ?
C26 C25 N5 C29 -5.4(2) . . . . ?
C18 C25 N5 C29 167.24(14) . . . . ?
C26 C25 N5 Fe1 179.86(12) . . . . ?
C18 C25 N5 Fe1 -7.50(18) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
####################################################################### 
# 
# 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_RuPY5Me2OH2_NO3
_database_code_depnum_ccdc_archive 'CCDC 1451781'
_audit_update_record             
;
2016-02-04 deposited with the CCDC.
2016-12-02 downloaded from the CCDC.
;

_audit_creation_date             2015-10-01T15:06:52-00:00
_audit_creation_method           'WinGX routine CIF_UPDATE'

#----------------------------------------------------------------------------#
#                   CHEMICAL INFORMATION                                     #
#----------------------------------------------------------------------------#

_chemical_name_systematic        
;
RuPY5Me2OH2_NO3
;
_chemical_formula_moiety         'C29 H27 N5 O1 Ru1, 2(N O3)'
_chemical_formula_sum            'C29 H27 N7 O7 Ru'
_chemical_formula_weight         686.64
_chemical_compound_source        'synthesis as described'

#----------------------------------------------------------------------------#
#                   UNIT CELL INFORMATION                                    #
#----------------------------------------------------------------------------#

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'C 2/c'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_Int_Tables_number      15
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, y, -z+1/2'
'x+1/2, y+1/2, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y, z-1/2'
'-x+1/2, -y+1/2, -z'
'x+1/2, -y+1/2, z-1/2'

_cell_length_a                   21.360(6)
_cell_length_b                   11.500(3)
_cell_length_c                   13.126(4)
_cell_angle_alpha                90
_cell_angle_beta                 121.481(3)
_cell_angle_gamma                90
_cell_volume                     2749.7(13)
_cell_formula_units_Z            4
_cell_measurement_temperature    123(2)
_cell_measurement_reflns_used    4493
_cell_measurement_theta_min      3.37
_cell_measurement_theta_max      27.48
_cell_measurement_wavelength     0.71073

#----------------------------------------------------------------------------#
#                   CRYSTAL INFORMATION                                      #
#----------------------------------------------------------------------------#

_exptl_crystal_description       Chip
_exptl_crystal_colour            Yellow
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.08
_exptl_crystal_density_diffrn    1.659
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1400
_exptl_special_details           
;
 ?
;

#----------------------------------------------------------------------------#
#                   ABSORPTION CORRECTION                                    #
#----------------------------------------------------------------------------#

_exptl_absorpt_coefficient_mu    0.634
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'REQAB (Rigaku, 1998)'
_exptl_absorpt_correction_T_min  0.922
_exptl_absorpt_correction_T_max  1
_shelx_estimated_absorpt_T_min   0.823
_shelx_estimated_absorpt_T_max   0.951

#----------------------------------------------------------------------------#
#                   DATA COLLECTION                                          #
#----------------------------------------------------------------------------#

_diffrn_radiation_source         'Rotating Anode'
_diffrn_ambient_temperature      123(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_measurement_device_type  'Rigaku Saturn'
_diffrn_detector_area_resol_mean 28.57
_diffrn_orient_matrix_type       d*trek
_diffrn_orient_matrix_ub_11      0.0022
_diffrn_orient_matrix_ub_12      0.0132
_diffrn_orient_matrix_ub_13      -0.0532
_diffrn_orient_matrix_ub_21      0.0137
_diffrn_orient_matrix_ub_22      -0.0835
_diffrn_orient_matrix_ub_23      -0.0202
_diffrn_orient_matrix_ub_31      -0.0733
_diffrn_orient_matrix_ub_32      0.0003
_diffrn_orient_matrix_ub_33      -0.0511
_diffrn_measurement_method       ω
_diffrn_standards_number         0
_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_decay_%        ?
_diffrn_reflns_av_R_equivalents  0.0179
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_number            10049
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         3.366
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_full 0.981
_diffrn_measured_fraction_theta_max 0.981
_diffrn_reflns_Laue_measured_fraction_full 0.981
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_point_group_measured_fraction_full 0.981
_diffrn_reflns_point_group_measured_fraction_max 0.981
_reflns_Friedel_coverage         0
_reflns_number_total             3092
_reflns_number_gt                2831
_reflns_threshold_expression     'I > 2σ(I)'

#----------------------------------------------------------------------------#
#                   COMPUTER PROGRAMS USED                                   #
#----------------------------------------------------------------------------#

_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008), '
_computing_structure_solution    'SIR-97 (Altomare et al., 1999)'
_computing_structure_refinement  'SHELXL-2014 (Sheldrick, 2014)'
_computing_molecular_graphics    'ORTEP-3 for Windows (Farrugia, 2012)'
_computing_publication_material  'WinGX publication routines (Farrugia, 2012)'

#----------------------------------------------------------------------------#
#                   STRUCTURE SOLUTION                                       #
#----------------------------------------------------------------------------#

_atom_sites_solution_hydrogens   mixed

#----------------------------------------------------------------------------#
#                   REFINEMENT INFORMATION                                   #
#----------------------------------------------------------------------------#

_refine_special_details          
;
 ?
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0335P)²+3.4075P] where P=(Fo²+2Fc²)/3'
_refine_ls_hydrogen_treatment    mixed
_refine_ls_extinction_method     none
_refine_ls_number_reflns         3092
_refine_ls_number_parameters     206
_refine_ls_number_restraints     0
_refine_ls_number_constraints    0
_refine_ls_R_factor_all          0.0254
_refine_ls_R_factor_gt           0.0231
_refine_ls_wR_factor_ref         0.0632
_refine_ls_wR_factor_gt          0.0617
_refine_ls_goodness_of_fit_ref   1.08
_refine_ls_restrained_S_all      1.08
_refine_ls_shift/su_max          0
_refine_ls_shift/su_mean         0
_refine_diff_density_max         0.561
_refine_diff_density_min         -0.54
_refine_diff_density_rms         0.06

#----------------------------------------------------------------------------#
#                   CONSTRAINTS AND RESTRAINTS                               #
#----------------------------------------------------------------------------#


#----------------------------------------------------------------------------#
#                   ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS         #
#----------------------------------------------------------------------------#

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 0 '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'
O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ru Ru -1.2594 0.8363 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_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
C1 C -0.12283(9) 0.26555(15) 0.49884(16) 0.0200(3) Uani 1 1 d . . . . .
H1 H -0.0897 0.3237 0.5041 0.024 Uiso 1 1 calc R U . . .
C2 C -0.18901(10) 0.25376(17) 0.39279(15) 0.0228(4) Uani 1 1 d . . . . .
H2 H -0.2006 0.3015 0.3261 0.027 Uiso 1 1 calc R U . . .
C3 C -0.23807(10) 0.17112(17) 0.38552(16) 0.0231(4) Uani 1 1 d . . . . .
H3 H -0.2841 0.161 0.3136 0.028 Uiso 1 1 calc R U . . .
C4 C -0.21916(9) 0.10345(15) 0.48433(15) 0.0202(3) Uani 1 1 d . . . . .
H4 H -0.2525 0.0468 0.4811 0.024 Uiso 1 1 calc R U . . .
C5 C -0.15121(9) 0.11813(14) 0.58878(14) 0.0163(3) Uani 1 1 d . . . . .
C6 C -0.12850(9) 0.04470(15) 0.70148(15) 0.0183(3) Uani 1 1 d . . . . .
C7 C -0.19162(10) -0.03793(16) 0.67669(17) 0.0250(4) Uani 1 1 d . . . . .
H7A H -0.202 -0.09 0.6105 0.038 Uiso 1 1 calc R U . . .
H7B H -0.2356 0.0076 0.6554 0.038 Uiso 1 1 calc R U . . .
H7C H -0.1774 -0.084 0.7484 0.038 Uiso 1 1 calc R U . . .
C8 C -0.11330(9) 0.12942(15) 0.80273(14) 0.0188(3) Uani 1 1 d . . . . .
C9 C -0.15468(10) 0.12949(18) 0.85678(16) 0.0248(4) Uani 1 1 d . . . . .
H9 H -0.1888 0.0686 0.8403 0.03 Uiso 1 1 calc R U . . .
C10 C -0.14627(11) 0.21800(19) 0.93433(17) 0.0301(4) Uani 1 1 d . . . . .
H10 H -0.1742 0.2184 0.9717 0.036 Uiso 1 1 calc R U . . .
C11 C -0.09673(11) 0.30561(18) 0.95660(17) 0.0296(4) Uani 1 1 d . . . . .
H11 H -0.0914 0.3693 1.0067 0.036 Uiso 1 1 calc R U . . .
C12 C -0.05499(10) 0.29865(16) 0.90420(16) 0.0229(4) Uani 1 1 d . . . . .
H12 H -0.0201 0.3582 0.9209 0.028 Uiso 1 1 calc R U . . .
C13 C -0.06023(9) -0.02637(15) 0.73070(14) 0.0187(3) Uani 1 1 d . . . . .
C14 C -0.06040(10) -0.14682(16) 0.73357(17) 0.0269(4) Uani 1 1 d . . . . .
H14 H -0.1018 -0.1875 0.7243 0.032 Uiso 1 1 calc R U . . .
C15 C 0 -0.2073(2) 0.75 0.0298(6) Uani 1 2 d S T P . .
H15 H 0 -0.29 0.75 0.036 Uiso 1 2 calc R U P . .
N1 N -0.10281(8) 0.19862(11) 0.59546(12) 0.0157(3) Uani 1 1 d . . . . .
N2 N -0.06140(8) 0.21136(12) 0.83061(13) 0.0171(3) Uani 1 1 d . . . . .
N3 N 0 0.03315(17) 0.75 0.0173(4) Uani 1 2 d S T P . .
N4 N -0.13541(8) 0.57867(14) 0.70135(15) 0.0258(3) Uani 1 1 d . . . . .
O1 O 0 0.38949(15) 0.75 0.0234(4) Uani 1 2 d S T P . .
O2 O -0.12066(8) 0.51414(13) 0.63829(13) 0.0335(3) Uani 1 1 d . . . . .
O3 O -0.09322(11) 0.57855(17) 0.81144(15) 0.0562(5) Uani 1 1 d . . . . .
O4 O -0.18928(8) 0.64403(13) 0.65095(14) 0.0371(4) Uani 1 1 d . . . . .
Ru1 Ru 0 0.20730(2) 0.75 0.01426(7) Uani 1 2 d S T P . .
H16 H 0.0413(11) 0.4382(19) 0.7834(19) 0.025(5) Uiso 1 1 d . . . . .



#----------------------------------------------------------------------------#
#                   MOLECULAR GEOMETRY                                       #
#----------------------------------------------------------------------------#

_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
C1 N1 1.348(2) . ?
C1 C2 1.378(2) . ?
C1 H1 0.95 . ?
C2 C3 1.381(3) . ?
C2 H2 0.95 . ?
C3 C4 1.380(3) . ?
C3 H3 0.95 . ?
C4 C5 1.392(2) . ?
C4 H4 0.95 . ?
C5 N1 1.356(2) . ?
C5 C6 1.545(2) . ?
C6 C13 1.535(2) . ?
C6 C7 1.539(2) . ?
C6 C8 1.539(2) . ?
C7 H7A 0.98 . ?
C7 H7B 0.98 . ?
C7 H7C 0.98 . ?
C8 N2 1.352(2) . ?
C8 C9 1.393(2) . ?
C9 C10 1.383(3) . ?
C9 H9 0.95 . ?
C10 C11 1.377(3) . ?
C10 H10 0.95 . ?
C11 C12 1.384(3) . ?
C11 H11 0.95 . ?
C12 N2 1.350(2) . ?
C12 H12 0.95 . ?
C13 N3 1.359(2) . ?
C13 C14 1.386(3) . ?
C14 C15 1.380(2) . ?
C14 H14 0.95 . ?
C15 C14 1.380(2) 2_556 ?
C15 H15 0.95 . ?
N1 Ru1 2.0724(15) . ?
N2 Ru1 2.0715(15) . ?
N3 C13 1.3593(19) 2_556 ?
N3 Ru1 2.003(2) . ?
N4 O4 1.238(2) . ?
N4 O3 1.241(2) . ?
N4 O2 1.268(2) . ?
O1 Ru1 2.0952(18) . ?
O1 H16 0.94(2) . ?
Ru1 N2 2.0716(15) 2_556 ?
Ru1 N1 2.0724(15) 2_556 ?

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
N1 C1 C2 123.24(17) . . ?
N1 C1 H1 118.4 . . ?
C2 C1 H1 118.4 . . ?
C1 C2 C3 118.60(17) . . ?
C1 C2 H2 120.7 . . ?
C3 C2 H2 120.7 . . ?
C4 C3 C2 118.96(16) . . ?
C4 C3 H3 120.5 . . ?
C2 C3 H3 120.5 . . ?
C3 C4 C5 120.03(16) . . ?
C3 C4 H4 120 . . ?
C5 C4 H4 120 . . ?
N1 C5 C4 120.95(15) . . ?
N1 C5 C6 117.62(14) . . ?
C4 C5 C6 121.43(15) . . ?
C13 C6 C7 109.69(14) . . ?
C13 C6 C8 112.12(13) . . ?
C7 C6 C8 109.87(14) . . ?
C13 C6 C5 108.21(13) . . ?
C7 C6 C5 109.43(13) . . ?
C8 C6 C5 107.45(14) . . ?
C6 C7 H7A 109.5 . . ?
C6 C7 H7B 109.5 . . ?
H7A C7 H7B 109.5 . . ?
C6 C7 H7C 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
N2 C8 C9 120.70(16) . . ?
N2 C8 C6 116.64(14) . . ?
C9 C8 C6 122.43(15) . . ?
C10 C9 C8 120.14(17) . . ?
C10 C9 H9 119.9 . . ?
C8 C9 H9 119.9 . . ?
C11 C10 C9 118.99(18) . . ?
C11 C10 H10 120.5 . . ?
C9 C10 H10 120.5 . . ?
C10 C11 C12 118.37(18) . . ?
C10 C11 H11 120.8 . . ?
C12 C11 H11 120.8 . . ?
N2 C12 C11 123.23(17) . . ?
N2 C12 H12 118.4 . . ?
C11 C12 H12 118.4 . . ?
N3 C13 C14 120.92(17) . . ?
N3 C13 C6 117.48(15) . . ?
C14 C13 C6 121.56(16) . . ?
C15 C14 C13 119.53(18) . . ?
C15 C14 H14 120.2 . . ?
C13 C14 H14 120.2 . . ?
C14 C15 C14 119.4(2) 2_556 . ?
C14 C15 H15 120.3 2_556 . ?
C14 C15 H15 120.3 . . ?
C1 N1 C5 118.19(14) . . ?
C1 N1 Ru1 123.14(11) . . ?
C5 N1 Ru1 118.59(11) . . ?
C12 N2 C8 118.34(15) . . ?
C12 N2 Ru1 121.85(12) . . ?
C8 N2 Ru1 119.63(11) . . ?
C13 N3 C13 119.5(2) . 2_556 ?
C13 N3 Ru1 120.24(10) . . ?
C13 N3 Ru1 120.24(10) 2_556 . ?
O4 N4 O3 122.02(17) . . ?
O4 N4 O2 119.02(17) . . ?
O3 N4 O2 118.86(16) . . ?
Ru1 O1 H16 126.7(13) . . ?
N3 Ru1 N2 91.29(4) . . ?
N3 Ru1 N2 91.29(4) . 2_556 ?
N2 Ru1 N2 177.42(8) . 2_556 ?
N3 Ru1 N1 87.24(4) . . ?
N2 Ru1 N1 82.59(6) . . ?
N2 Ru1 N1 97.53(6) 2_556 . ?
N3 Ru1 N1 87.24(4) . 2_556 ?
N2 Ru1 N1 97.53(6) . 2_556 ?
N2 Ru1 N1 82.59(6) 2_556 2_556 ?
N1 Ru1 N1 174.48(7) . 2_556 ?
N3 Ru1 O1 180 . . ?
N2 Ru1 O1 88.71(4) . . ?
N2 Ru1 O1 88.71(4) 2_556 . ?
N1 Ru1 O1 92.76(4) . . ?
N1 Ru1 O1 92.76(4) 2_556 . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
N1 C1 C2 C3 1.4(3) . . . . ?
C1 C2 C3 C4 0.0(3) . . . . ?
C2 C3 C4 C5 -0.7(3) . . . . ?
C3 C4 C5 N1 0.1(3) . . . . ?
C3 C4 C5 C6 179.42(15) . . . . ?
N1 C5 C6 C13 -62.38(18) . . . . ?
C4 C5 C6 C13 118.32(17) . . . . ?
N1 C5 C6 C7 178.13(15) . . . . ?
C4 C5 C6 C7 -1.2(2) . . . . ?
N1 C5 C6 C8 58.88(18) . . . . ?
C4 C5 C6 C8 -120.42(16) . . . . ?
C13 C6 C8 N2 60.88(19) . . . . ?
C7 C6 C8 N2 -176.86(14) . . . . ?
C5 C6 C8 N2 -57.89(18) . . . . ?
C13 C6 C8 C9 -124.58(17) . . . . ?
C7 C6 C8 C9 -2.3(2) . . . . ?
C5 C6 C8 C9 116.64(17) . . . . ?
N2 C8 C9 C10 4.1(3) . . . . ?
C6 C8 C9 C10 -170.26(17) . . . . ?
C8 C9 C10 C11 0.2(3) . . . . ?
C9 C10 C11 C12 -2.8(3) . . . . ?
C10 C11 C12 N2 1.3(3) . . . . ?
C7 C6 C13 N3 177.23(13) . . . . ?
C8 C6 C13 N3 -60.41(18) . . . . ?
C5 C6 C13 N3 57.92(17) . . . . ?
C7 C6 C13 C14 -0.7(2) . . . . ?
C8 C6 C13 C14 121.66(18) . . . . ?
C5 C6 C13 C14 -120.01(18) . . . . ?
N3 C13 C14 C15 -3.4(2) . . . . ?
C6 C13 C14 C15 174.41(14) . . . . ?
C13 C14 C15 C14 1.68(12) . . . 2_556 ?
C2 C1 N1 C5 -2.0(2) . . . . ?
C2 C1 N1 Ru1 174.81(13) . . . . ?
C4 C5 N1 C1 1.2(2) . . . . ?
C6 C5 N1 C1 -178.12(14) . . . . ?
C4 C5 N1 Ru1 -175.77(12) . . . . ?
C6 C5 N1 Ru1 4.92(19) . . . . ?
C11 C12 N2 C8 2.9(3) . . . . ?
C11 C12 N2 Ru1 178.05(14) . . . . ?
C9 C8 N2 C12 -5.5(2) . . . . ?
C6 C8 N2 C12 169.11(15) . . . . ?
C9 C8 N2 Ru1 179.23(12) . . . . ?
C6 C8 N2 Ru1 -6.13(19) . . . . ?
C14 C13 N3 C13 1.73(13) . . . 2_556 ?
C6 C13 N3 C13 -176.21(16) . . . 2_556 ?
C14 C13 N3 Ru1 -178.27(13) . . . . ?
C6 C13 N3 Ru1 3.79(16) . . . . ?

# The following lines are used to test the character set of files sent by
# network email or other means. They are not part of the CIF data set
# abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789
# !@#$%^&*()_+{}:"~<>?|\-=[];'`,./

# END of CIF
