# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2015

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

data_1
_database_code_depnum_ccdc_archive 'CCDC 1037786'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;

_exptl_special_details           
; 
 The crystal was 
placed in the cold stream of an Oxford 
Cryosystems open-flow nitrogen cryostat (Cosier & 
Glazer, 1986) with a nominal stability of 0.1K. 
 
Cosier, J. & Glazer, A.M., 1986. J. Appl. Cryst. 105-107. 
;
_refine_special_details          
; 
? 
;
_cell_length_a                   13.04230(10)
_cell_length_b                   24.8523(2)
_cell_length_c                   17.09450(10)
_cell_angle_alpha                90
_cell_angle_beta                 108.2053(4)
_cell_angle_gamma                90
_cell_volume                     5263.50(7)

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   'P 21/n '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
x+1/2,-y+1/2,z+1/2
-x+1/2,y+1/2,-z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Fe 0.3463 0.8444 11.7695 4.7611 7.3573 0.3072 3.5222 15.3535 2.3045 76.8805
1.0369 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
N 0.0061 0.0033 12.2126 0.0057 3.1322 9.8933 2.0125 28.9975 1.1663 0.5826
-11.5290 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
P 0.1023 0.0942 6.4345 1.9067 4.1791 27.1570 1.7800 0.5260 1.4908 68.1645
1.1149 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C51 H30 B1 Cl0.25 Fe1 N1 O1 P0.25 
# Dc =      0.95 Fooo =   2264.00 Mu =      3.36 M =    756.07
# Found Formula = C52 H57 B1 Cl8 Fe1 N1 O1 P1 
# Dc =      1.38 FOOO =   2264.00 Mu =      7.61 M =   1093.28

_chemical_formula_sum            'C52 H57 B1 Cl8 Fe1 N1 O1 P1'
_chemical_formula_moiety         'C24 H12 B Cl8, C28 H45 Fe N O P'
_chemical_compound_source        .
_chemical_formula_weight         1093.28


_cell_measurement_reflns_used    12197
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.100
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.120

_exptl_crystal_density_diffrn    1.380
_exptl_crystal_density_meas      .
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             2264
_exptl_absorpt_coefficient_mu    0.761

# Sheldrick geometric approximatio 0.91 0.93 
# No experimental values of Tmin/max available 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.91
_exptl_absorpt_correction_T_max  0.93
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

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

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        .

_diffrn_ambient_temperature      150
_diffrn_reflns_number            23500
_reflns_number_total             11969
_diffrn_reflns_av_R_equivalents  0.000
# Number of reflections without Friedels Law is 0 
# Number of reflections with Friedels Law is 11969 
# Theoretical number of reflections is about 24154 


_diffrn_reflns_theta_min         5.138
_diffrn_reflns_theta_max         27.488
_diffrn_measured_fraction_theta_max 0.991

_diffrn_reflns_theta_full        26.938
_diffrn_measured_fraction_theta_full 0.992


_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_k_max       32
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_reflns_limit_h_min              -16
_reflns_limit_h_max              16
_reflns_limit_k_min              0
_reflns_limit_k_max              32
_reflns_limit_l_min              0
_reflns_limit_l_max              22

_oxford_diffrn_Wilson_B_factor   2.16
_oxford_diffrn_Wilson_scale      19.65

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

_refine_diff_density_min         -0.65
_refine_diff_density_max         0.97


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         11969
_refine_ls_number_restraints     0
_refine_ls_number_parameters     586
_oxford_refine_ls_R_factor_ref   0.0590
_refine_ls_wR_factor_ref         0.0982
_refine_ls_goodness_of_fit_ref   0.9363
_refine_ls_shift/su_max          0.0017032
_refine_ls_shift/su_mean         0.0000715


# The values computed with all filters except I/sigma 
_oxford_reflns_number_all        11969
_refine_ls_R_factor_all          0.0590
_refine_ls_wR_factor_all         0.0982

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                9146
_refine_ls_R_factor_gt           0.0384
_refine_ls_wR_factor_gt          0.0905

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    constr #undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.05P)² + 3.97P] 
 ,where P=(max(Fo²,0) + 2Fc²)/3 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_atom_site_attached_hydrogens
Fe1 Fe 0.20538(2) 0.524971(11) 0.868110(17) 0.0229 1.0000 Uani . . . . . .
P2 P 0.25337(4) 0.53702(2) 0.75309(3) 0.0197 1.0000 Uani . . . . . .
C3 C 0.38268(15) 0.57270(8) 0.76839(12) 0.0214 1.0000 Uani . . . . . .
C4 C 0.47504(16) 0.54565(8) 0.83512(12) 0.0253 1.0000 Uani . . . . . .
C5 C 0.58357(17) 0.56954(9) 0.83664(14) 0.0324 1.0000 Uani . . . . . .
C6 C 0.58586(18) 0.63035(9) 0.84846(14) 0.0354 1.0000 Uani . . . . . .
C7 C 0.49170(17) 0.65720(8) 0.78439(14) 0.0298 1.0000 Uani . . . . . .
C8 C 0.38348(16) 0.63352(8) 0.78530(13) 0.0264 1.0000 Uani . . . . . .
C9 C 0.26742(16) 0.47365(8) 0.69680(12) 0.0251 1.0000 Uani . . . . . .
C10 C 0.33970(18) 0.48055(8) 0.64153(13) 0.0285 1.0000 Uani . . . . . .
C11 C 0.3282(2) 0.43226(9) 0.58483(14) 0.0356 1.0000 Uani . . . . . .
C12 C 0.3582(2) 0.38037(9) 0.63323(15) 0.0366 1.0000 Uani . . . . . .
C13 C 0.2938(2) 0.37359(9) 0.69330(14) 0.0346 1.0000 Uani . . . . . .
C14 C 0.30029(17) 0.42370(8) 0.74788(13) 0.0289 1.0000 Uani . . . . . .
C15 C 0.15203(16) 0.57792(8) 0.67502(12) 0.0248 1.0000 Uani . . . . . .
C16 C 0.03869(16) 0.55327(9) 0.65033(13) 0.0302 1.0000 Uani . . . . . .
C17 C -0.04570(18) 0.59187(11) 0.59666(14) 0.0379 1.0000 Uani . . . . . .
C18 C -0.01703(18) 0.60842(11) 0.52040(14) 0.0396 1.0000 Uani . . . . . .
C19 C 0.09587(18) 0.63215(10) 0.54364(15) 0.0388 1.0000 Uani . . . . . .
C20 C 0.17978(17) 0.59307(9) 0.59665(13) 0.0299 1.0000 Uani . . . . . .
C21 C 0.18808(19) 0.60888(9) 0.87900(14) 0.0341 1.0000 Uani . . . . . .
C22 C 0.2656(2) 0.58903(9) 0.95019(14) 0.0364 1.0000 Uani . . . . . .
C23 C 0.2132(2) 0.55055(10) 0.98670(14) 0.0384 1.0000 Uani . . . . . .
C24 C 0.1056(2) 0.54719(9) 0.93775(15) 0.0372 1.0000 Uani . . . . . .
C25 C 0.08917(19) 0.58313(9) 0.87054(15) 0.0347 1.0000 Uani . . . . . .
C26 C 0.10680(17) 0.47233(9) 0.81727(13) 0.0288 1.0000 Uani . . . . . .
N27 N 0.04201(16) 0.43985(8) 0.78781(12) 0.0363 1.0000 Uani . . . . . .
C28 C -0.03918(19) 0.40076(10) 0.74378(15) 0.0382 1.0000 Uani . . . . . .
C29 C 0.0141(2) 0.35556(10) 0.71253(16) 0.0426 1.0000 Uani . . . . . .
C30 C -0.1230(2) 0.42958(12) 0.6731(2) 0.0583 1.0000 Uani . . . . . .
C31 C 0.31148(18) 0.48008(8) 0.91322(12) 0.0264 1.0000 Uani . . . . . .
O32 O 0.38055(13) 0.45191(7) 0.94883(9) 0.0370 1.0000 Uani . . . . . .
Cl33 Cl 0.90795(5) 0.93393(2) 0.99217(3) 0.0339 1.0000 Uani . . . . . .
C34 C 1.01974(17) 0.89883(8) 1.05498(12) 0.0249 1.0000 Uani . . . . . .
C35 C 1.02475(16) 0.84343(8) 1.04591(12) 0.0234 1.0000 Uani . . . . . .
C36 C 1.11365(16) 0.81367(8) 1.09389(12) 0.0221 1.0000 Uani . . . . . .
C37 C 1.19683(16) 0.84296(8) 1.14933(12) 0.0244 1.0000 Uani . . . . . .
C38 C 1.18866(17) 0.89815(8) 1.15804(12) 0.0269 1.0000 Uani . . . . . .
C39 C 1.10073(17) 0.92749(8) 1.11187(12) 0.0267 1.0000 Uani . . . . . .
Cl40 Cl 1.29304(4) 0.93210(2) 1.23114(4) 0.0373 1.0000 Uani . . . . . .
B41 B 1.11887(18) 0.74877(9) 1.07853(13) 0.0216 1.0000 Uani . . . . . .
C42 C 1.00187(15) 0.71945(8) 1.06510(11) 0.0218 1.0000 Uani . . . . . .
C43 C 0.97952(15) 0.66966(8) 1.02491(12) 0.0233 1.0000 Uani . . . . . .
C44 C 0.88468(16) 0.64230(8) 1.01852(12) 0.0250 1.0000 Uani . . . . . .
Cl45 Cl 0.85959(4) 0.58128(2) 0.96550(4) 0.0372 1.0000 Uani . . . . . .
C46 C 0.80764(16) 0.66179(8) 1.05147(12) 0.0269 1.0000 Uani . . . . . .
C47 C 0.83069(16) 0.71055(9) 1.09236(12) 0.0258 1.0000 Uani . . . . . .
C48 C 0.92472(16) 0.73893(8) 1.09977(12) 0.0238 1.0000 Uani . . . . . .
Cl49 Cl 0.73655(5) 0.73662(3) 1.13616(4) 0.0398 1.0000 Uani . . . . . .
C50 C 1.19869(15) 0.71684(8) 1.15839(12) 0.0216 1.0000 Uani . . . . . .
C51 C 1.20503(16) 0.73163(8) 1.23904(12) 0.0236 1.0000 Uani . . . . . .
C52 C 1.26477(16) 0.70201(9) 1.30604(12) 0.0262 1.0000 Uani . . . . . .
Cl53 Cl 1.26803(5) 0.72253(3) 1.40450(3) 0.0385 1.0000 Uani . . . . . .
C54 C 1.31933(16) 0.65572(9) 1.29762(13) 0.0298 1.0000 Uani . . . . . .
C55 C 1.30989(17) 0.63981(9) 1.21847(13) 0.0297 1.0000 Uani . . . . . .
C56 C 1.25263(16) 0.66930(8) 1.15014(12) 0.0268 1.0000 Uani . . . . . .
Cl57 Cl 1.37022(6) 0.57908(3) 1.20426(4) 0.0526 1.0000 Uani . . . . . .
C58 C 1.15983(16) 0.74314(7) 0.99750(12) 0.0232 1.0000 Uani . . . . . .
C59 C 1.08804(17) 0.74006(8) 0.91740(12) 0.0263 1.0000 Uani . . . . . .
C60 C 1.12582(19) 0.73948(8) 0.84991(13) 0.0304 1.0000 Uani . . . . . .
Cl61 Cl 1.03345(6) 0.73475(3) 0.75092(3) 0.0509 1.0000 Uani . . . . . .
C62 C 1.23443(19) 0.74189(8) 0.85772(14) 0.0323 1.0000 Uani . . . . . .
C63 C 1.30514(18) 0.74507(8) 0.93677(14) 0.0307 1.0000 Uani . . . . . .
C64 C 1.27000(17) 0.74608(8) 1.00545(13) 0.0279 1.0000 Uani . . . . . .
Cl65 Cl 1.44369(5) 0.74685(3) 0.95029(4) 0.0487 1.0000 Uani . . . . . .
H31 H 0.4007 0.5682 0.7177 0.0263 1.0000 Uiso R . . . . .
H42 H 0.4627 0.5519 0.8876 0.0303 1.0000 Uiso R . . . . .
H41 H 0.4774 0.5073 0.8278 0.0304 1.0000 Uiso R . . . . .
H51 H 0.6386 0.5528 0.8810 0.0391 1.0000 Uiso R . . . . .
H52 H 0.5955 0.5605 0.7845 0.0380 1.0000 Uiso R . . . . .
H62 H 0.5790 0.6368 0.9039 0.0421 1.0000 Uiso R . . . . .
H61 H 0.6537 0.6450 0.8451 0.0435 1.0000 Uiso R . . . . .
H71 H 0.4920 0.6951 0.7930 0.0340 1.0000 Uiso R . . . . .
H72 H 0.4982 0.6515 0.7294 0.0355 1.0000 Uiso R . . . . .
H82 H 0.3756 0.6399 0.8393 0.0320 1.0000 Uiso R . . . . .
H81 H 0.3262 0.6524 0.7424 0.0329 1.0000 Uiso R . . . . .
H91 H 0.1942 0.4663 0.6604 0.0314 1.0000 Uiso R . . . . .
H102 H 0.4167 0.4831 0.6777 0.0349 1.0000 Uiso R . . . . .
H101 H 0.3203 0.5140 0.6067 0.0350 1.0000 Uiso R . . . . .
H111 H 0.3720 0.4368 0.5491 0.0435 1.0000 Uiso R . . . . .
H112 H 0.2514 0.4300 0.5503 0.0429 1.0000 Uiso R . . . . .
H122 H 0.4357 0.3814 0.6648 0.0455 1.0000 Uiso R . . . . .
H121 H 0.3440 0.3507 0.5947 0.0448 1.0000 Uiso R . . . . .
H132 H 0.3225 0.3438 0.7292 0.0413 1.0000 Uiso R . . . . .
H131 H 0.2164 0.3682 0.6622 0.0417 1.0000 Uiso R . . . . .
H141 H 0.3745 0.4265 0.7873 0.0348 1.0000 Uiso R . . . . .
H142 H 0.2503 0.4181 0.7811 0.0342 1.0000 Uiso R . . . . .
H151 H 0.1478 0.6123 0.7035 0.0312 1.0000 Uiso R . . . . .
H162 H 0.0167 0.5435 0.6978 0.0366 1.0000 Uiso R . . . . .
H161 H 0.0395 0.5200 0.6186 0.0367 1.0000 Uiso R . . . . .
H172 H -0.0490 0.6258 0.6276 0.0468 1.0000 Uiso R . . . . .
H171 H -0.1185 0.5740 0.5784 0.0471 1.0000 Uiso R . . . . .
H181 H -0.0665 0.6350 0.4907 0.0484 1.0000 Uiso R . . . . .
H182 H -0.0188 0.5773 0.4850 0.0474 1.0000 Uiso R . . . . .
H192 H 0.0954 0.6649 0.5750 0.0460 1.0000 Uiso R . . . . .
H191 H 0.1173 0.6400 0.4938 0.0469 1.0000 Uiso R . . . . .
H201 H 0.2472 0.6094 0.6091 0.0334 1.0000 Uiso R . . . . .
H202 H 0.1802 0.5622 0.5640 0.0365 1.0000 Uiso R . . . . .
H211 H 0.2016 0.6371 0.8438 0.0407 1.0000 Uiso R . . . . .
H221 H 0.3424 0.5997 0.9706 0.0438 1.0000 Uiso R . . . . .
H231 H 0.2439 0.5320 1.0369 0.0461 1.0000 Uiso R . . . . .
H241 H 0.0499 0.5237 0.9474 0.0459 1.0000 Uiso R . . . . .
H251 H 0.0235 0.5893 0.8297 0.0422 1.0000 Uiso R . . . . .
H281 H -0.0714 0.3857 0.7829 0.0465 1.0000 Uiso R . . . . .
H293 H -0.0414 0.3286 0.6876 0.0642 1.0000 Uiso R . . . . .
H292 H 0.0749 0.3400 0.7559 0.0647 1.0000 Uiso R . . . . .
H291 H 0.0432 0.3712 0.6709 0.0648 1.0000 Uiso R . . . . .
H301 H -0.1729 0.4025 0.6412 0.0878 1.0000 Uiso R . . . . .
H303 H -0.1631 0.4547 0.6973 0.0894 1.0000 Uiso R . . . . .
H302 H -0.0869 0.4477 0.6374 0.0882 1.0000 Uiso R . . . . .
H351 H 0.9651 0.8264 1.0048 0.0284 1.0000 Uiso R . . . . .
H371 H 1.2618 0.8256 1.1809 0.0296 1.0000 Uiso R . . . . .
H391 H 1.0999 0.9652 1.1214 0.0320 1.0000 Uiso R . . . . .
H431 H 1.0293 0.6542 1.0009 0.0278 1.0000 Uiso R . . . . .
H461 H 0.7443 0.6434 1.0464 0.0340 1.0000 Uiso R . . . . .
H481 H 0.9364 0.7722 1.1276 0.0285 1.0000 Uiso R . . . . .
H511 H 1.1684 0.7618 1.2478 0.0283 1.0000 Uiso R . . . . .
H541 H 1.3572 0.6366 1.3429 0.0360 1.0000 Uiso R . . . . .
H561 H 1.2512 0.6567 1.0980 0.0310 1.0000 Uiso R . . . . .
H591 H 1.0108 0.7390 0.9069 0.0317 1.0000 Uiso R . . . . .
H621 H 1.2552 0.7424 0.8098 0.0378 1.0000 Uiso R . . . . .
H641 H 1.3216 0.7478 1.0589 0.0332 1.0000 Uiso R . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.17937(6)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
Fe1 . P2 . 2.2619(5) yes
Fe1 . C21 . 2.112(2) yes
Fe1 . C22 . 2.105(2) yes
Fe1 . C23 . 2.096(2) yes
Fe1 . C24 . 2.093(2) yes
Fe1 . C25 . 2.104(2) yes
Fe1 . C26 . 1.850(2) yes
Fe1 . C31 . 1.757(2) yes
P2 . C3 . 1.8503(19) yes
P2 . C9 . 1.884(2) yes
P2 . C15 . 1.860(2) yes
C3 . C4 . 1.532(3) yes
C3 . C8 . 1.538(3) yes
C3 . H31 . 0.973 no
C4 . C5 . 1.528(3) yes
C4 . H42 . 0.973 no
C4 . H41 . 0.964 no
C5 . C6 . 1.524(3) yes
C5 . H51 . 0.961 no
C5 . H52 . 0.977 no
C6 . C7 . 1.521(3) yes
C6 . H62 . 0.993 no
C6 . H61 . 0.975 no
C7 . C8 . 1.534(3) yes
C7 . H71 . 0.953 no
C7 . H72 . 0.980 no
C8 . H82 . 0.972 no
C8 . H81 . 0.986 no
C9 . C10 . 1.539(3) yes
C9 . C14 . 1.501(3) yes
C9 . H91 . 0.981 no
C10 . C11 . 1.520(3) yes
C10 . H102 . 1.003 no
C10 . H101 . 1.008 no
C11 . C12 . 1.516(3) yes
C11 . H111 . 0.964 no
C11 . H112 . 0.992 no
C12 . C13 . 1.525(3) yes
C12 . H122 . 0.986 no
C12 . H121 . 0.966 no
C13 . C14 . 1.543(3) yes
C13 . H132 . 0.959 no
C13 . H131 . 0.992 no
C14 . H141 . 0.994 no
C14 . H142 . 0.999 no
C15 . C16 . 1.533(3) yes
C15 . C20 . 1.540(3) yes
C15 . H151 . 0.994 no
C16 . C17 . 1.530(3) yes
C16 . H162 . 0.972 no
C16 . H161 . 0.991 no
C17 . C18 . 1.521(3) yes
C17 . H172 . 1.003 no
C17 . H171 . 1.006 no
C18 . C19 . 1.519(3) yes
C18 . H181 . 0.952 no
C18 . H182 . 0.978 no
C19 . C20 . 1.530(3) yes
C19 . H192 . 0.977 no
C19 . H191 . 0.995 no
C20 . H201 . 0.930 no
C20 . H202 . 0.949 no
C21 . C22 . 1.406(3) yes
C21 . C25 . 1.406(3) yes
C21 . H211 . 0.975 no
C22 . C23 . 1.427(3) yes
C22 . H221 . 0.989 no
C23 . C24 . 1.394(4) yes
C23 . H231 . 0.945 no
C24 . C25 . 1.418(3) yes
C24 . H241 . 0.986 no
C25 . H251 . 0.933 no
C26 . N27 . 1.163(3) yes
N27 . C28 . 1.461(3) yes
C28 . C29 . 1.504(3) yes
C28 . C30 . 1.531(4) yes
C28 . H281 . 0.969 no
C29 . H293 . 0.981 no
C29 . H292 . 0.980 no
C29 . H291 . 0.984 no
C30 . H301 . 0.975 no
C30 . H303 . 0.985 no
C30 . H302 . 0.987 no
C31 . O32 . 1.153(3) yes
Cl33 . C34 . 1.750(2) yes
C34 . C35 . 1.389(3) yes
C34 . C39 . 1.388(3) yes
C35 . C36 . 1.403(3) yes
C35 . H351 . 0.967 no
C36 . C37 . 1.401(3) yes
C36 . B41 . 1.639(3) yes
C37 . C38 . 1.387(3) yes
C37 . H371 . 0.953 no
C38 . C39 . 1.380(3) yes
C38 . Cl40 . 1.750(2) yes
C39 . H391 . 0.952 no
B41 . C42 . 1.641(3) yes
B41 . C50 . 1.640(3) yes
B41 . C58 . 1.639(3) yes
C42 . C43 . 1.401(3) yes
C42 . C48 . 1.404(3) yes
C43 . C44 . 1.386(3) yes
C43 . H431 . 0.951 no
C44 . Cl45 . 1.745(2) yes
C44 . C46 . 1.384(3) yes
C46 . C47 . 1.384(3) yes
C46 . H461 . 0.924 no
C47 . C48 . 1.386(3) yes
C47 . Cl49 . 1.750(2) yes
C48 . H481 . 0.943 no
C50 . C51 . 1.404(3) yes
C50 . C56 . 1.405(3) yes
C51 . C52 . 1.380(3) yes
C51 . H511 . 0.926 no
C52 . Cl53 . 1.746(2) yes
C52 . C54 . 1.384(3) yes
C54 . C55 . 1.378(3) yes
C54 . H541 . 0.911 no
C55 . C56 . 1.384(3) yes
C55 . Cl57 . 1.754(2) yes
C56 . H561 . 0.940 no
C58 . C59 . 1.399(3) yes
C58 . C64 . 1.402(3) yes
C59 . C60 . 1.389(3) yes
C59 . H591 . 0.967 no
C60 . Cl61 . 1.748(2) yes
C60 . C62 . 1.382(3) yes
C62 . C63 . 1.380(3) yes
C62 . H621 . 0.939 no
C63 . C64 . 1.388(3) yes
C63 . Cl65 . 1.749(2) yes
C64 . H641 . 0.952 no
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
P2 . Fe1 . C21 . 90.70(6) yes
P2 . Fe1 . C22 . 109.41(7) yes
C21 . Fe1 . C22 . 38.96(9) yes
P2 . Fe1 . C23 . 149.01(7) yes
C21 . Fe1 . C23 . 65.77(9) yes
C22 . Fe1 . C23 . 39.72(9) yes
P2 . Fe1 . C24 . 148.13(7) yes
C21 . Fe1 . C24 . 65.60(9) yes
C22 . Fe1 . C24 . 65.81(9) yes
C23 . Fe1 . C24 . 38.86(10) yes
P2 . Fe1 . C25 . 108.84(7) yes
C21 . Fe1 . C25 . 38.97(9) yes
C22 . Fe1 . C25 . 65.70(9) yes
C23 . Fe1 . C25 . 65.83(10) yes
C24 . Fe1 . C25 . 39.48(9) yes
P2 . Fe1 . C26 . 91.47(6) yes
C21 . Fe1 . C26 . 131.45(9) yes
C22 . Fe1 . C26 . 155.21(9) yes
C23 . Fe1 . C26 . 119.05(9) yes
C24 . Fe1 . C26 . 89.40(9) yes
P2 . Fe1 . C31 . 94.11(6) yes
C21 . Fe1 . C31 . 132.80(9) yes
C22 . Fe1 . C31 . 96.26(10) yes
C23 . Fe1 . C31 . 88.52(9) yes
C24 . Fe1 . C31 . 117.52(9) yes
C25 . Fe1 . C26 . 95.50(9) yes
C25 . Fe1 . C31 . 154.27(9) yes
C26 . Fe1 . C31 . 95.37(10) yes
Fe1 . P2 . C3 . 115.35(6) yes
Fe1 . P2 . C9 . 115.52(6) yes
C3 . P2 . C9 . 104.07(9) yes
Fe1 . P2 . C15 . 111.62(7) yes
C3 . P2 . C15 . 104.57(9) yes
C9 . P2 . C15 . 104.54(9) yes
P2 . C3 . C4 . 111.40(13) yes
P2 . C3 . C8 . 116.74(13) yes
C4 . C3 . C8 . 109.50(16) yes
P2 . C3 . H31 . 106.4 no
C4 . C3 . H31 . 105.1 no
C8 . C3 . H31 . 106.9 no
C3 . C4 . C5 . 110.55(16) yes
C3 . C4 . H42 . 107.4 no
C5 . C4 . H42 . 110.0 no
C3 . C4 . H41 . 112.8 no
C5 . C4 . H41 . 108.6 no
H42 . C4 . H41 . 107.5 no
C4 . C5 . C6 . 111.55(18) yes
C4 . C5 . H51 . 107.8 no
C6 . C5 . H51 . 110.3 no
C4 . C5 . H52 . 107.8 no
C6 . C5 . H52 . 110.3 no
H51 . C5 . H52 . 109.1 no
C5 . C6 . C7 . 111.21(18) yes
C5 . C6 . H62 . 106.4 no
C7 . C6 . H62 . 108.9 no
C5 . C6 . H61 . 110.1 no
C7 . C6 . H61 . 109.6 no
H62 . C6 . H61 . 110.5 no
C6 . C7 . C8 . 111.28(17) yes
C6 . C7 . H71 . 111.0 no
C8 . C7 . H71 . 109.7 no
C6 . C7 . H72 . 109.5 no
C8 . C7 . H72 . 108.0 no
H71 . C7 . H72 . 107.2 no
C3 . C8 . C7 . 109.11(16) yes
C3 . C8 . H82 . 109.9 no
C7 . C8 . H82 . 108.5 no
C3 . C8 . H81 . 111.6 no
C7 . C8 . H81 . 107.3 no
H82 . C8 . H81 . 110.4 no
P2 . C9 . C10 . 113.36(14) yes
P2 . C9 . C14 . 116.73(14) yes
C10 . C9 . C14 . 109.33(17) yes
P2 . C9 . H91 . 104.4 no
C10 . C9 . H91 . 107.0 no
C14 . C9 . H91 . 105.0 no
C9 . C10 . C11 . 110.25(17) yes
C9 . C10 . H102 . 108.5 no
C11 . C10 . H102 . 108.8 no
C9 . C10 . H101 . 111.5 no
C11 . C10 . H101 . 108.5 no
H102 . C10 . H101 . 109.3 no
C10 . C11 . C12 . 111.49(18) yes
C10 . C11 . H111 . 110.6 no
C12 . C11 . H111 . 110.0 no
C10 . C11 . H112 . 107.6 no
C12 . C11 . H112 . 108.5 no
H111 . C11 . H112 . 108.5 no
C11 . C12 . C13 . 111.05(18) yes
C11 . C12 . H122 . 108.8 no
C13 . C12 . H122 . 108.7 no
C11 . C12 . H121 . 108.3 no
C13 . C12 . H121 . 110.2 no
H122 . C12 . H121 . 109.7 no
C12 . C13 . C14 . 112.37(18) yes
C12 . C13 . H132 . 109.3 no
C14 . C13 . H132 . 107.4 no
C12 . C13 . H131 . 109.7 no
C14 . C13 . H131 . 106.7 no
H132 . C13 . H131 . 111.5 no
C13 . C14 . C9 . 111.35(17) yes
C13 . C14 . H141 . 109.0 no
C9 . C14 . H141 . 112.1 no
C13 . C14 . H142 . 108.0 no
C9 . C14 . H142 . 109.1 no
H141 . C14 . H142 . 107.1 no
P2 . C15 . C16 . 112.79(14) yes
P2 . C15 . C20 . 116.78(14) yes
C16 . C15 . C20 . 109.07(17) yes
P2 . C15 . H151 . 104.8 no
C16 . C15 . H151 . 106.4 no
C20 . C15 . H151 . 106.3 no
C15 . C16 . C17 . 111.45(18) yes
C15 . C16 . H162 . 112.4 no
C17 . C16 . H162 . 108.2 no
C15 . C16 . H161 . 108.0 no
C17 . C16 . H161 . 108.9 no
H162 . C16 . H161 . 107.8 no
C16 . C17 . C18 . 111.10(19) yes
C16 . C17 . H172 . 110.6 no
C18 . C17 . H172 . 106.7 no
C16 . C17 . H171 . 109.9 no
C18 . C17 . H171 . 108.4 no
H172 . C17 . H171 . 110.0 no
C17 . C18 . C19 . 111.02(19) yes
C17 . C18 . H181 . 109.7 no
C19 . C18 . H181 . 108.1 no
C17 . C18 . H182 . 110.6 no
C19 . C18 . H182 . 107.6 no
H181 . C18 . H182 . 109.8 no
C18 . C19 . C20 . 111.34(19) yes
C18 . C19 . H192 . 107.2 no
C20 . C19 . H192 . 109.3 no
C18 . C19 . H191 . 111.2 no
C20 . C19 . H191 . 106.9 no
H192 . C19 . H191 . 111.0 no
C15 . C20 . C19 . 110.58(18) yes
C15 . C20 . H201 . 111.7 no
C19 . C20 . H201 . 108.0 no
C15 . C20 . H202 . 111.2 no
C19 . C20 . H202 . 107.3 no
H201 . C20 . H202 . 107.9 no
Fe1 . C21 . C22 . 70.25(13) yes
Fe1 . C21 . C25 . 70.21(12) yes
C22 . C21 . C25 . 108.5(2) yes
Fe1 . C21 . H211 . 127.6 no
C22 . C21 . H211 . 124.5 no
C25 . C21 . H211 . 126.9 no
Fe1 . C22 . C21 . 70.79(13) yes
Fe1 . C22 . C23 . 69.81(12) yes
C21 . C22 . C23 . 107.5(2) yes
Fe1 . C22 . H221 . 124.4 no
C21 . C22 . H221 . 125.9 no
C23 . C22 . H221 . 126.6 no
Fe1 . C23 . C22 . 70.47(12) yes
Fe1 . C23 . C24 . 70.45(12) yes
C22 . C23 . C24 . 107.9(2) yes
Fe1 . C23 . H231 . 127.5 no
C22 . C23 . H231 . 126.8 no
C24 . C23 . H231 . 125.2 no
Fe1 . C24 . C23 . 70.69(12) yes
Fe1 . C24 . C25 . 70.68(12) yes
C23 . C24 . C25 . 108.5(2) yes
Fe1 . C24 . H241 . 124.1 no
C23 . C24 . H241 . 126.3 no
C25 . C24 . H241 . 125.2 no
Fe1 . C25 . C24 . 69.85(12) yes
Fe1 . C25 . C21 . 70.82(12) yes
C24 . C25 . C21 . 107.5(2) yes
Fe1 . C25 . H251 . 126.6 no
C24 . C25 . H251 . 125.5 no
C21 . C25 . H251 . 126.9 no
Fe1 . C26 . N27 . 176.74(18) yes
C26 . N27 . C28 . 175.0(2) yes
N27 . C28 . C29 . 109.78(19) yes
N27 . C28 . C30 . 108.7(2) yes
C29 . C28 . C30 . 111.4(2) yes
N27 . C28 . H281 . 107.5 no
C29 . C28 . H281 . 107.8 no
C30 . C28 . H281 . 111.6 no
C28 . C29 . H293 . 107.7 no
C28 . C29 . H292 . 112.3 no
H293 . C29 . H292 . 111.8 no
C28 . C29 . H291 . 106.7 no
H293 . C29 . H291 . 110.8 no
H292 . C29 . H291 . 107.4 no
C28 . C30 . H301 . 107.8 no
C28 . C30 . H303 . 107.8 no
H301 . C30 . H303 . 108.9 no
C28 . C30 . H302 . 109.8 no
H301 . C30 . H302 . 109.5 no
H303 . C30 . H302 . 113.0 no
Fe1 . C31 . O32 . 174.54(18) yes
Cl33 . C34 . C35 . 119.00(16) yes
Cl33 . C34 . C39 . 118.67(15) yes
C35 . C34 . C39 . 122.33(19) yes
C34 . C35 . C36 . 121.06(18) yes
C34 . C35 . H351 . 117.3 no
C36 . C35 . H351 . 121.7 no
C35 . C36 . C37 . 116.45(18) yes
C35 . C36 . B41 . 119.54(17) yes
C37 . C36 . B41 . 123.88(17) yes
C36 . C37 . C38 . 121.13(19) yes
C36 . C37 . H371 . 120.7 no
C38 . C37 . H371 . 118.2 no
C37 . C38 . C39 . 122.62(19) yes
C37 . C38 . Cl40 . 118.98(17) yes
C39 . C38 . Cl40 . 118.40(16) yes
C34 . C39 . C38 . 116.36(18) yes
C34 . C39 . H391 . 125.3 no
C38 . C39 . H391 . 118.3 no
C36 . B41 . C42 . 112.08(16) yes
C36 . B41 . C50 . 112.96(16) yes
C42 . B41 . C50 . 102.85(15) yes
C36 . B41 . C58 . 105.08(15) yes
C42 . B41 . C58 . 112.22(16) yes
C50 . B41 . C58 . 111.87(16) yes
B41 . C42 . C43 . 120.17(17) yes
B41 . C42 . C48 . 123.07(17) yes
C43 . C42 . C48 . 116.41(18) yes
C42 . C43 . C44 . 121.05(18) yes
C42 . C43 . H431 . 120.2 no
C44 . C43 . H431 . 118.7 no
C43 . C44 . Cl45 . 119.04(16) yes
C43 . C44 . C46 . 122.69(19) yes
Cl45 . C44 . C46 . 118.26(15) yes
C44 . C46 . C47 . 116.17(18) yes
C44 . C46 . H461 . 122.0 no
C47 . C46 . H461 . 121.8 no
C46 . C47 . C48 . 122.56(18) yes
C46 . C47 . Cl49 . 118.00(15) yes
C48 . C47 . Cl49 . 119.44(16) yes
C42 . C48 . C47 . 121.10(19) yes
C42 . C48 . H481 . 119.5 no
C47 . C48 . H481 . 119.4 no
B41 . C50 . C51 . 121.21(17) yes
B41 . C50 . C56 . 122.08(17) yes
C51 . C50 . C56 . 116.17(18) yes
C50 . C51 . C52 . 121.36(18) yes
C50 . C51 . H511 . 119.7 no
C52 . C51 . H511 . 119.0 no
C51 . C52 . Cl53 . 118.80(16) yes
C51 . C52 . C54 . 122.18(19) yes
Cl53 . C52 . C54 . 118.98(16) yes
C52 . C54 . C55 . 116.73(19) yes
C52 . C54 . H541 . 120.3 no
C55 . C54 . H541 . 122.9 no
C54 . C55 . C56 . 122.42(19) yes
C54 . C55 . Cl57 . 118.48(17) yes
C56 . C55 . Cl57 . 119.08(16) yes
C50 . C56 . C55 . 121.07(19) yes
C50 . C56 . H561 . 120.8 no
C55 . C56 . H561 . 118.1 no
B41 . C58 . C59 . 122.47(18) yes
B41 . C58 . C64 . 120.55(17) yes
C59 . C58 . C64 . 116.73(18) yes
C58 . C59 . C60 . 120.7(2) yes
C58 . C59 . H591 . 121.6 no
C60 . C59 . H591 . 117.7 no
C59 . C60 . Cl61 . 119.26(18) yes
C59 . C60 . C62 . 122.6(2) yes
Cl61 . C60 . C62 . 118.17(16) yes
C60 . C62 . C63 . 116.64(19) yes
C60 . C62 . H621 . 118.8 no
C63 . C62 . H621 . 124.5 no
C62 . C63 . C64 . 122.2(2) yes
C62 . C63 . Cl65 . 118.53(16) yes
C64 . C63 . Cl65 . 119.24(18) yes
C58 . C64 . C63 . 121.1(2) yes
C58 . C64 . H641 . 119.4 no
C63 . C64 . H641 . 119.5 no
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_site_symmetry_D
_geom_hbond_atom_site_label_H
_geom_hbond_site_symmetry_H
_geom_hbond_atom_site_label_A
_geom_hbond_site_symmetry_A
_geom_hbond_angle_DHA
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_publ_flag
C14 . H142 . C26 . 136.62 0.999 2.535 3.333(3) yes


_iucr_refine_instructions_details_constraints 
;
#
# Punched on 12/11/14 at 13:13:57
#
#LIST     12                                                                    
BLOCK SCALE X'S, U'S 
RIDE C   (   3,X'S) H   (  31,X'S) 
RIDE C   (   4,X'S) H   (  42,X'S) H   (  41,X'S) 
RIDE C   (   5,X'S) H   (  51,X'S) H   (  52,X'S) 
RIDE C   (   6,X'S) H   (  62,X'S) H   (  61,X'S) 
RIDE C   (   7,X'S) H   (  71,X'S) H   (  72,X'S) 
RIDE C   (   8,X'S) H   (  82,X'S) H   (  81,X'S) 
RIDE C   (   9,X'S) H   (  91,X'S) 
RIDE C   (  10,X'S) H   ( 102,X'S) H   ( 101,X'S) 
RIDE C   (  11,X'S) H   ( 111,X'S) H   ( 112,X'S) 
RIDE C   (  12,X'S) H   ( 122,X'S) H   ( 121,X'S) 
RIDE C   (  13,X'S) H   ( 132,X'S) H   ( 131,X'S) 
RIDE C   (  14,X'S) H   ( 141,X'S) H   ( 142,X'S) 
RIDE C   (  15,X'S) H   ( 151,X'S) 
RIDE C   (  16,X'S) H   ( 162,X'S) H   ( 161,X'S) 
RIDE C   (  17,X'S) H   ( 172,X'S) H   ( 171,X'S) 
RIDE C   (  18,X'S) H   ( 181,X'S) H   ( 182,X'S) 
RIDE C   (  19,X'S) H   ( 192,X'S) H   ( 191,X'S) 
RIDE C   (  20,X'S) H   ( 201,X'S) H   ( 202,X'S) 
RIDE C   (  21,X'S) H   ( 211,X'S) 
RIDE C   (  22,X'S) H   ( 221,X'S) 
RIDE C   (  23,X'S) H   ( 231,X'S) 
RIDE C   (  24,X'S) H   ( 241,X'S) 
RIDE C   (  25,X'S) H   ( 251,X'S) 
RIDE C   (  28,X'S) H   ( 281,X'S) 
RIDE C   (  29,X'S) H   ( 293,X'S) H   ( 292,X'S) H   ( 291,X'S) 
RIDE C   (  30,X'S) H   ( 301,X'S) H   ( 303,X'S) H   ( 302,X'S) 
RIDE C   (  35,X'S) H   ( 351,X'S) 
RIDE C   (  37,X'S) H   ( 371,X'S) 
RIDE C   (  39,X'S) H   ( 391,X'S) 
RIDE C   (  43,X'S) H   ( 431,X'S) 
RIDE C   (  46,X'S) H   ( 461,X'S) 
RIDE C   (  48,X'S) H   ( 481,X'S) 
RIDE C   (  51,X'S) H   ( 511,X'S) 
RIDE C   (  54,X'S) H   ( 541,X'S) 
RIDE C   (  56,X'S) H   ( 561,X'S) 
RIDE C   (  59,X'S) H   ( 591,X'S) 
RIDE C   (  62,X'S) H   ( 621,X'S) 
RIDE C   (  64,X'S) H   ( 641,X'S) 
END                                                                             
;


_iucr_refine_instructions_details_restraints 
;
#
# Punched on 12/11/14 at 13:13:57
#
#LIST     16                                                                    
NO 
REM   HREST   START (DO NOT REMOVE THIS LINE) 
REM   HREST   END (DO NOT REMOVE THIS LINE) 
END                                                                             
;
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_056jndv10
_database_code_depnum_ccdc_archive 'CCDC 1037787'
_audit_update_record             
;
2014-12-04 deposited with the CCDC.
2015-02-10 downloaded from the CCDC.
;
_audit_creation_date             10-07-01
_audit_creation_method           CRYSTALS_ver_14.03

_oxford_structure_analysis_title 056jndv10
_chemical_name_systematic        .
_chemical_melting_point          .


_cell_length_a                   7.8866(4)
_cell_length_b                   11.0772(5)
_cell_length_c                   12.3944(6)
_cell_angle_alpha                90
_cell_angle_beta                 97.450(2)
_cell_angle_gamma                90
_cell_volume                     1073.65(9)

_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   'P 1 21/n 1 '
_symmetry_space_group_name_Hall  '-P 2yn'
loop_
_symmetry_equiv_pos_as_xyz
x,y,z
-x,-y,-z
-x+1/2,y+1/2,-z+1/2
x+1/2,-y+1/2,z+1/2

loop_
_atom_type_symbol
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_Cromer_Mann_a1
_atom_type_scat_Cromer_Mann_b1
_atom_type_scat_Cromer_Mann_a2
_atom_type_scat_Cromer_Mann_b2
_atom_type_scat_Cromer_Mann_a3
_atom_type_scat_Cromer_Mann_b3
_atom_type_scat_Cromer_Mann_a4
_atom_type_scat_Cromer_Mann_b4
_atom_type_scat_Cromer_Mann_c
_atom_type_scat_source
C 0.0033 0.0016 2.3100 20.8439 1.0200 10.2075 1.5886 0.5687 0.8650 51.6512
0.2156 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
H 0.0000 0.0000 0.4930 10.5109 0.3229 26.1257 0.1402 3.1424 0.0408 57.7998
0.0030 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
B 0.0013 0.0007 2.0545 23.2185 1.3326 1.0210 1.0979 60.3498 0.7068 0.1403
-0.1932 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
Cl 0.1484 0.1585 11.4604 0.0104 7.1964 1.1662 6.2556 18.5194 1.6455 47.7784
-9.5574 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
O 0.0106 0.0060 3.0485 13.2771 2.2868 5.7011 1.5463 0.3239 0.8670 32.9089
0.2508 'International Tables Vol C 4.2.6.8 and 6.1.1.4'
W -0.8490 6.8722 29.0818 1.7203 15.4300 9.2259 14.4327 0.3217 5.1198 57.0560
9.8875 'International Tables Vol C 4.2.6.8 and 6.1.1.4'


_cell_formula_units_Z            4

# Given Formula = C8 H5 B1 Cl2 O3 W1 
# Dc =      2.57 Fooo =    760.00 Mu =    112.35 M =    414.69
# Found Formula = C8 H5 B1 Cl2 O3 W1 
# Dc =      2.57 FOOO =    760.00 Mu =    112.35 M =    414.69

_chemical_formula_sum            'C8 H5 B1 Cl2 O3 W1'
_chemical_formula_moiety         'C8 H5 B1 Cl2 O3 W1'
_chemical_compound_source        ?
_chemical_formula_weight         414.69


_cell_measurement_reflns_used    2467
_cell_measurement_theta_min      5
_cell_measurement_theta_max      27
_cell_measurement_temperature    150

_exptl_crystal_description       plate
_exptl_crystal_colour            yellow
_exptl_crystal_size_min          0.030
_exptl_crystal_size_mid          0.120
_exptl_crystal_size_max          0.150

_exptl_crystal_density_diffrn    2.565
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
# Non-dispersive F(000): 
_exptl_crystal_F_000             760
_exptl_absorpt_coefficient_mu    11.235

# Sheldrick geometric approximatio 0.26 0.71 
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'DENZO/SCALEPACK (Otwinowski & Minor, 1997)'
_exptl_absorpt_correction_T_min  0.38
_exptl_absorpt_correction_T_max  0.71
# For a Kappa CCD, set Tmin to 1.0 and 
# Tmax to the ratio of max:min frame scales in scale_all.log 
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_device       Area
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_measurement_method       ω

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

_diffrn_standards_interval_time  .
_diffrn_standards_interval_count .
_diffrn_standards_number         0
_diffrn_standards_decay_%        ?

_diffrn_ambient_temperature      150
_diffrn_reflns_number            11681
_reflns_number_total             2427
_diffrn_reflns_av_R_equivalents  0.069
# Number of reflections without Friedels Law is 4430 
# Number of reflections with Friedels Law is 2427 
# Theoretical number of reflections is about 2456 


_diffrn_reflns_theta_min         5.215
_diffrn_reflns_theta_max         27.458
_diffrn_measured_fraction_theta_max 0.989

_diffrn_reflns_theta_full        26.909
_diffrn_measured_fraction_theta_full 0.993


_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_reflns_limit_h_min              -10
_reflns_limit_h_max              10
_reflns_limit_k_min              0
_reflns_limit_k_max              14
_reflns_limit_l_min              0
_reflns_limit_l_max              16

_oxford_diffrn_Wilson_B_factor   2.54
_oxford_diffrn_Wilson_scale      238.34

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

_refine_diff_density_min         -4.01
_refine_diff_density_max         3.87


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


# The values actually used during refinement 
_oxford_reflns_threshold_expression_ref I>-3.0\s(I)
_refine_ls_number_reflns         2425
_refine_ls_number_restraints     0
_refine_ls_number_parameters     136
_oxford_refine_ls_R_factor_ref   0.0834
_refine_ls_wR_factor_ref         0.1558
_refine_ls_goodness_of_fit_ref   1.0061
_refine_ls_shift/su_max          0.0009613
_refine_ls_shift/su_mean         4.0901890


# The values computed from all data 
_oxford_reflns_number_all        2425
_refine_ls_R_factor_all          0.0834
_refine_ls_wR_factor_all         0.1558

# The values computed with a 2 sigma cutoff - a la SHELX 
_reflns_threshold_expression     I>2.0σ(I)
_reflns_number_gt                1732
_refine_ls_R_factor_gt           0.0578
_refine_ls_wR_factor_gt          0.1389

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


_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_hydrogen_treatment    none # none, undef, noref, refall,
# refxyz, refU, constr or mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
;
 Method= Modified Sheldrick 
 w=1/[σ²(F²) + ( 0.10P)² + 0.00P] 
 ,where P=p(6)*max(Fo²,0) + (1-p(6))Fc² 
;

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

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

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


loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_occupancy
_atom_site_adp_type
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
_oxford_atom_site_special_shape
_atom_site_attached_hydrogens
W1 W 0.87007(5) 0.22357(5) 0.61774(3) 0.0301 1.0000 Uani . . . . . . .
C2 C 1.123(2) 0.2499(13) 0.6318(9) 0.0488 1.0000 Uani . . . . . . .
O3 O 1.2674(11) 0.2602(10) 0.6363(8) 0.0512 1.0000 Uani . . . . . . .
C4 C 0.6137(15) 0.1406(16) 0.5326(10) 0.0536 1.0000 Uani . . . . . . .
C5 C 0.7483(15) 0.0694(11) 0.5027(10) 0.0395 1.0000 Uani . . . . . . .
C6 C 0.8427(14) 0.1457(12) 0.4406(8) 0.0389 1.0000 Uani . . . . . . .
C7 C 0.7712(17) 0.2627(14) 0.4351(9) 0.0459 1.0000 Uani . . . . . . .
C8 C 0.6277(17) 0.2552(14) 0.4911(10) 0.0450 1.0000 Uani . . . . . . .
C9 C 0.9620(13) 0.0966(10) 0.7292(8) 0.0293 1.0000 Uani . . . . . . .
O10 O 1.0135(11) 0.0270(8) 0.7892(7) 0.0456 1.0000 Uani . . . . . . .
C11 C 0.7846(15) 0.2837(11) 0.7511(9) 0.0355 1.0000 Uani . . . . . . .
O12 O 0.7356(11) 0.3185(9) 0.8285(7) 0.0467 1.0000 Uani . . . . . . .
B13 B 0.9124(16) 0.4210(14) 0.6394(10) 0.0336 1.0000 Uani . . . . . . .
Cl14 Cl 0.7968(4) 0.5292(3) 0.5534(2) 0.0442 1.0000 Uani . . . . . . .
Cl15 Cl 1.0618(4) 0.4943(3) 0.7397(2) 0.0476 1.0000 Uani . . . . . . .
H41 H 0.5193 0.1104 0.5722 0.0640 1.0000 Uiso . . . . . . .
H51 H 0.7659 -0.0185 0.5160 0.0472 1.0000 Uiso . . . . . . .
H61 H 0.9384 0.1195 0.4022 0.0480 1.0000 Uiso . . . . . . .
H71 H 0.8053 0.3322 0.3923 0.0552 1.0000 Uiso . . . . . . .
H81 H 0.5432 0.3211 0.4959 0.0541 1.0000 Uiso . . . . . . .

_refine_ls_extinction_method     None
_oxford_refine_ls_scale          0.06257(3)
loop_
_geom_bond_atom_site_label_1
_geom_bond_site_symmetry_1
_geom_bond_atom_site_label_2
_geom_bond_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
W1 . C2 . 2.005(17) yes
W1 . C4 . 2.344(12) yes
W1 . C5 . 2.349(11) yes
W1 . C6 . 2.343(9) yes
W1 . C7 . 2.337(11) yes
W1 . C8 . 2.337(13) yes
W1 . C9 . 2.038(12) yes
W1 . C11 . 1.980(11) yes
W1 . B13 . 2.223(14) yes
C2 . O3 . 1.135(18) yes
C4 . C5 . 1.411(18) yes
C4 . C8 . 1.38(2) yes
C4 . H41 . 1.001 no
C5 . C6 . 1.417(17) yes
C5 . H51 . 0.994 no
C6 . C7 . 1.41(2) yes
C6 . H61 . 0.987 no
C7 . C8 . 1.405(19) yes
C7 . H71 . 0.992 no
C8 . H81 . 0.996 no
C9 . O10 . 1.111(13) yes
C11 . O12 . 1.146(14) yes
B13 . Cl14 . 1.775(15) yes
B13 . Cl15 . 1.793(12) yes
loop_
_geom_angle_atom_site_label_1
_geom_angle_site_symmetry_1
_geom_angle_atom_site_label_2
_geom_angle_site_symmetry_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C2 . W1 . C4 . 152.6(5) yes
C2 . W1 . C5 . 118.9(5) yes
C4 . W1 . C5 . 35.0(5) yes
C2 . W1 . C6 . 96.0(4) yes
C4 . W1 . C6 . 57.6(4) yes
C5 . W1 . C6 . 35.2(4) yes
C2 . W1 . C7 . 105.1(5) yes
C4 . W1 . C7 . 58.4(5) yes
C5 . W1 . C7 . 59.2(5) yes
C6 . W1 . C7 . 35.1(5) yes
C2 . W1 . C8 . 139.1(5) yes
C4 . W1 . C8 . 34.3(5) yes
C5 . W1 . C8 . 57.8(5) yes
C6 . W1 . C8 . 57.2(4) yes
C7 . W1 . C8 . 35.0(5) yes
C2 . W1 . C9 . 77.2(5) yes
C4 . W1 . C9 . 104.2(5) yes
C5 . W1 . C9 . 89.5(4) yes
C6 . W1 . C9 . 111.2(4) yes
C7 . W1 . C9 . 146.0(5) yes
C2 . W1 . C11 . 108.8(5) yes
C4 . W1 . C11 . 98.1(5) yes
C5 . W1 . C11 . 126.5(5) yes
C6 . W1 . C11 . 155.0(5) yes
C7 . W1 . C11 . 129.8(5) yes
C2 . W1 . B13 . 73.4(5) yes
C4 . W1 . B13 . 123.2(6) yes
C5 . W1 . B13 . 146.3(4) yes
C6 . W1 . B13 . 118.0(5) yes
C7 . W1 . B13 . 87.7(5) yes
C8 . W1 . C9 . 138.3(5) yes
C8 . W1 . C11 . 100.0(5) yes
C9 . W1 . C11 . 78.2(4) yes
C8 . W1 . B13 . 91.8(5) yes
C9 . W1 . B13 . 124.2(4) yes
C11 . W1 . B13 . 68.3(4) yes
W1 . C2 . O3 . 176.6(12) yes
W1 . C4 . C5 . 72.7(6) yes
W1 . C4 . C8 . 72.6(8) yes
C5 . C4 . C8 . 108.5(11) yes
W1 . C4 . H41 . 124.3 no
C5 . C4 . H41 . 125.1 no
C8 . C4 . H41 . 126.2 no
W1 . C5 . C4 . 72.3(7) yes
W1 . C5 . C6 . 72.2(6) yes
C4 . C5 . C6 . 106.0(11) yes
W1 . C5 . H51 . 125.0 no
C4 . C5 . H51 . 126.7 no
C6 . C5 . H51 . 127.1 no
W1 . C6 . C5 . 72.6(6) yes
W1 . C6 . C7 . 72.2(6) yes
C5 . C6 . C7 . 109.8(10) yes
W1 . C6 . H61 . 125.2 no
C5 . C6 . H61 . 125.1 no
C7 . C6 . H61 . 124.9 no
W1 . C7 . C6 . 72.7(6) yes
W1 . C7 . C8 . 72.5(7) yes
C6 . C7 . C8 . 105.3(12) yes
W1 . C7 . H71 . 125.7 no
C6 . C7 . H71 . 127.2 no
C8 . C7 . H71 . 127.0 no
W1 . C8 . C7 . 72.5(7) yes
W1 . C8 . C4 . 73.1(7) yes
C7 . C8 . C4 . 110.3(13) yes
W1 . C8 . H81 . 124.4 no
C7 . C8 . H81 . 125.1 no
C4 . C8 . H81 . 124.5 no
W1 . C9 . O10 . 179.2(9) yes
W1 . C11 . O12 . 179.8(11) yes
W1 . B13 . Cl14 . 122.3(6) yes
W1 . B13 . Cl15 . 127.2(8) yes
Cl14 . B13 . Cl15 . 110.6(8) yes
