# Electronic Supplementary Material (ESI) for ChemComm.
# This journal is © The Royal Society of Chemistry 2020

####################################################################### 
# 
# 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-Cr
_database_code_depnum_ccdc_archive 'CCDC 2003385'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         apx2920
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   00s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         6/3/19
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      6/4/19
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     6/4/19
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   6/5/19
_LANL_internal_validation_user   CAPG
_LANL_internal_validation_date   10/1/2020
_LANL_internal_archive_date      10/1/2020
_LANL_internal_LA-UR             ?

_audit_creation_date             2019-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H24 Cr P2'
_chemical_formula_sum            'C16 H24 Cr P2'
_chemical_formula_weight         330.29
_chemical_melting_point          ?
_chemical_oxdiff_formula         Cr(PC8H12)2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.8420(3)
_cell_length_b                   12.5620(4)
_cell_length_c                   8.8611(3)
_cell_angle_alpha                90
_cell_angle_beta                 109.444(4)
_cell_angle_gamma                90
_cell_volume                     823.13(5)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    8270
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.3420
_cell_measurement_theta_min      1.6360
_shelx_estimated_absorpt_T_max   0.779
_shelx_estimated_absorpt_T_min   0.710
_exptl_absorpt_coefficient_mu    0.874
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.80355
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.333
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             348
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From n-hexane.'
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.35
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0166
_diffrn_reflns_av_unetI/netI     0.0101
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            6774
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.349
_diffrn_reflns_theta_min         2.928
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.26 185.26   0.50   10.00    --   28.00  73.75 -25.74  366
  2  ω      2.26 185.26   0.50   10.00    --   28.00  73.75  64.26  366
  3  ω      2.26 185.26   0.50   10.00    --   28.00  73.75 154.26  366
  4  ω      2.26 185.26   0.50   10.00    --   28.00  73.75-115.74  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0416436000
_diffrn_orient_matrix_UB_12      0.0239724000
_diffrn_orient_matrix_UB_13      0.0514157000
_diffrn_orient_matrix_UB_21      0.0861304000
_diffrn_orient_matrix_UB_22      0.0076156000
_diffrn_orient_matrix_UB_23      0.0588678000
_diffrn_orient_matrix_UB_31      0.0067082000
_diffrn_orient_matrix_UB_32      0.0505270000
_diffrn_orient_matrix_UB_33      -0.0331969000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1441
_reflns_number_total             1508
_reflns_odcompleteness_completeness 100.00
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.334
_refine_diff_density_min         -0.257
_refine_diff_density_rms         0.054
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.091
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1508
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0268
_refine_ls_R_factor_gt           0.0252
_refine_ls_restrained_S_all      1.091
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0306P)²+0.7174P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0655
_refine_ls_wR_factor_ref         0.0667
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.500000 0.500000 0.500000 0.01152(13) Uani 1 2 d S T P . .
P1 P 0.64711(6) 0.33269(3) 0.51363(5) 0.01608(13) Uani 1 1 d . . . . .
C1 C 0.7595(2) 0.43632(14) 0.6523(2) 0.0163(4) Uani 1 1 d . . . . .
C2 C 0.7963(2) 0.52871(14) 0.5742(2) 0.0160(3) Uani 1 1 d . . . . .
C3 C 0.7254(2) 0.52055(13) 0.4035(2) 0.0155(3) Uani 1 1 d . . . . .
C4 C 0.6353(2) 0.42172(13) 0.3509(2) 0.0149(3) Uani 1 1 d . . . . .
C5 C 0.8183(2) 0.42210(16) 0.8326(2) 0.0243(4) Uani 1 1 d . . . . .
H5A H 0.816343 0.491174 0.883359 0.036 Uiso 1 1 calc GR . . . .
H5B H 0.941172 0.392922 0.871512 0.036 Uiso 1 1 calc GR . . . .
H5C H 0.735385 0.373029 0.859154 0.036 Uiso 1 1 calc GR . . . .
C6 C 0.8976(2) 0.62519(15) 0.6615(2) 0.0237(4) Uani 1 1 d . . . . .
H6A H 1.026994 0.616726 0.678858 0.036 Uiso 1 1 calc GR . . . .
H6B H 0.878795 0.632173 0.764976 0.036 Uiso 1 1 calc GR . . . .
H6C H 0.852678 0.689139 0.597219 0.036 Uiso 1 1 calc GR . . . .
C7 C 0.7424(3) 0.60793(15) 0.2918(2) 0.0238(4) Uani 1 1 d . . . . .
H7A H 0.868202 0.612482 0.294526 0.036 Uiso 1 1 calc GR . . . .
H7B H 0.706310 0.676023 0.325893 0.036 Uiso 1 1 calc GR . . . .
H7C H 0.663863 0.591856 0.182525 0.036 Uiso 1 1 calc GR . . . .
C8 C 0.5498(2) 0.38995(15) 0.1767(2) 0.0208(4) Uani 1 1 d . . . . .
H8A H 0.470562 0.328405 0.168987 0.031 Uiso 1 1 calc GR . . . .
H8B H 0.644924 0.371326 0.132364 0.031 Uiso 1 1 calc GR . . . .
H8C H 0.478776 0.449610 0.116221 0.031 Uiso 1 1 calc GR . . . .


_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
Cr1 P1 2.3813(4) 3_666 ?
Cr1 P1 2.3812(4) . ?
Cr1 C1 2.1846(16) . ?
Cr1 C1 2.1847(16) 3_666 ?
Cr1 C2 2.2236(16) 3_666 ?
Cr1 C2 2.2236(16) . ?
Cr1 C3 2.2196(16) 3_666 ?
Cr1 C3 2.2196(16) . ?
Cr1 C4 2.1840(16) 3_666 ?
Cr1 C4 2.1840(16) . ?
P1 C1 1.8054(18) . ?
P1 C4 1.8024(17) . ?
C1 C2 1.429(2) . ?
C1 C5 1.519(2) . ?
C2 C3 1.430(2) . ?
C2 C6 1.513(2) . ?
C3 C4 1.428(2) . ?
C3 C7 1.514(2) . ?
C4 C8 1.518(2) . ?

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
P1 Cr1 P1 180.0 . 3_666 ?
C1 Cr1 P1 46.34(5) . . ?
C1 Cr1 P1 133.66(5) . 3_666 ?
C1 Cr1 P1 133.66(5) 3_666 . ?
C1 Cr1 P1 46.34(5) 3_666 3_666 ?
C1 Cr1 C1 180.0 . 3_666 ?
C1 Cr1 C2 142.18(6) . 3_666 ?
C1 Cr1 C2 37.82(6) . . ?
C1 Cr1 C2 142.18(6) 3_666 . ?
C1 Cr1 C2 37.82(6) 3_666 3_666 ?
C1 Cr1 C3 114.64(6) 3_666 . ?
C1 Cr1 C3 65.36(6) . . ?
C1 Cr1 C3 114.64(6) . 3_666 ?
C1 Cr1 C3 65.36(6) 3_666 3_666 ?
C2 Cr1 P1 108.23(5) . 3_666 ?
C2 Cr1 P1 71.77(5) . . ?
C2 Cr1 P1 71.77(5) 3_666 3_666 ?
C2 Cr1 P1 108.23(5) 3_666 . ?
C2 Cr1 C2 180.0 . 3_666 ?
C3 Cr1 P1 108.19(4) 3_666 . ?
C3 Cr1 P1 108.19(4) . 3_666 ?
C3 Cr1 P1 71.81(4) 3_666 3_666 ?
C3 Cr1 P1 71.81(4) . . ?
C3 Cr1 C2 142.45(6) 3_666 . ?
C3 Cr1 C2 37.55(6) 3_666 3_666 ?
C3 Cr1 C2 37.55(6) . . ?
C3 Cr1 C2 142.45(6) . 3_666 ?
C3 Cr1 C3 180.0 . 3_666 ?
C4 Cr1 P1 46.26(4) 3_666 3_666 ?
C4 Cr1 P1 46.26(4) . . ?
C4 Cr1 P1 133.74(4) 3_666 . ?
C4 Cr1 P1 133.74(4) . 3_666 ?
C4 Cr1 C1 109.35(6) . 3_666 ?
C4 Cr1 C1 109.35(6) 3_666 . ?
C4 Cr1 C1 70.65(6) . . ?
C4 Cr1 C1 70.65(6) 3_666 3_666 ?
C4 Cr1 C2 65.27(6) 3_666 3_666 ?
C4 Cr1 C2 114.73(6) 3_666 . ?
C4 Cr1 C2 114.73(6) . 3_666 ?
C4 Cr1 C2 65.27(6) . . ?
C4 Cr1 C3 37.83(6) . . ?
C4 Cr1 C3 142.17(6) 3_666 . ?
C4 Cr1 C3 37.83(6) 3_666 3_666 ?
C4 Cr1 C3 142.17(6) . 3_666 ?
C4 Cr1 C4 180.0 . 3_666 ?
C1 P1 Cr1 61.09(5) . . ?
C4 P1 Cr1 61.09(5) . . ?
C4 P1 C1 88.87(8) . . ?
P1 C1 Cr1 72.58(6) . . ?
C2 C1 Cr1 72.57(9) . . ?
C2 C1 P1 112.80(12) . . ?
C2 C1 C5 124.42(16) . . ?
C5 C1 Cr1 125.96(12) . . ?
C5 C1 P1 122.65(13) . . ?
C1 C2 Cr1 69.61(9) . . ?
C1 C2 C3 112.55(15) . . ?
C1 C2 C6 123.99(16) . . ?
C3 C2 Cr1 71.07(9) . . ?
C3 C2 C6 123.46(16) . . ?
C6 C2 Cr1 126.88(12) . . ?
C2 C3 Cr1 71.38(9) . . ?
C2 C3 C7 123.47(16) . . ?
C4 C3 Cr1 69.73(9) . . ?
C4 C3 C2 112.55(15) . . ?
C4 C3 C7 123.97(15) . . ?
C7 C3 Cr1 126.25(12) . . ?
P1 C4 Cr1 72.65(6) . . ?
C3 C4 Cr1 72.44(9) . . ?
C3 C4 P1 112.97(12) . . ?
C3 C4 C8 124.31(15) . . ?
C8 C4 Cr1 126.50(11) . . ?
C8 C4 P1 122.57(13) . . ?

_olex2_exptl_crystal_mounting_method 
'From paratone on a microscope slide, onto a cryoloop.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.841
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# 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-Fe
_database_code_depnum_ccdc_archive 'CCDC 2003386'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         dq0894
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   13s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         9/1/18
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      9/4/18
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     9/4/18
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   9/4/18
_LANL_internal_validation_user   CAPG
_LANL_internal_validation_date   10/1/2020
_LANL_internal_archive_date      10/1/2020
_LANL_internal_LA-UR             ?

_audit_creation_date             2018-08-31
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H24 Fe P2'
_chemical_formula_sum            'C16 H24 Fe P2'
_chemical_formula_weight         334.14
_chemical_melting_point          ?
_chemical_oxdiff_formula         Fe(PC8H12)2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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                   14.2948(7)
_cell_length_b                   12.8549(6)
_cell_length_c                   8.8448(4)
_cell_angle_alpha                90
_cell_angle_beta                 104.364(5)
_cell_angle_gamma                90
_cell_volume                     1574.50(13)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1902
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      29.1350
_cell_measurement_theta_min      2.9210
_shelx_estimated_absorpt_T_max   0.838
_shelx_estimated_absorpt_T_min   0.732
_exptl_absorpt_coefficient_mu    1.146
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.84961
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear orange'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             704
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.16
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0322
_diffrn_reflns_av_unetI/netI     0.0267
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            6215
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         2.162
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -57.68 144.32   0.50   13.00    --  -21.13  73.72 145.93  404
  2  ω    -57.68 144.32   0.50   13.00    --  -21.13  73.72  15.16  404
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0264242000
_diffrn_orient_matrix_UB_12      -0.0371477000
_diffrn_orient_matrix_UB_13      0.0318035000
_diffrn_orient_matrix_UB_21      -0.0424620000
_diffrn_orient_matrix_UB_22      0.0303234000
_diffrn_orient_matrix_UB_23      -0.0257806000
_diffrn_orient_matrix_UB_31      -0.0110854000
_diffrn_orient_matrix_UB_32      -0.0272720000
_diffrn_orient_matrix_UB_33      -0.0719585000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1407
_reflns_number_total             1605
_reflns_odcompleteness_completeness 99.70
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.557
_refine_diff_density_min         -0.243
_refine_diff_density_rms         0.100
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.117
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     92
_refine_ls_number_reflns         1605
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0374
_refine_ls_R_factor_gt           0.0312
_refine_ls_restrained_S_all      1.117
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+0.7810P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0798
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.250000 0.250000 0.500000 0.00942(14) Uani 1 2 d S T P . .
P1 P 0.15969(3) 0.29323(4) 0.25575(5) 0.01440(15) Uani 1 1 d . . . . .
C1 C 0.28657(13) 0.27614(15) 0.2881(2) 0.0139(4) Uani 1 1 d . . . . .
C2 C 0.34062(13) 0.34196(14) 0.4068(2) 0.0129(4) Uani 1 1 d . . . . .
C3 C 0.27978(13) 0.40597(14) 0.4755(2) 0.0128(4) Uani 1 1 d . . . . .
C4 C 0.17971(13) 0.38806(14) 0.4074(2) 0.0131(4) Uani 1 1 d . . . . .
C5 C 0.33110(15) 0.20152(16) 0.1942(2) 0.0203(4) Uani 1 1 d . . . . .
H5A H 0.391360 0.173713 0.260100 0.030 Uiso 1 1 calc GR . . . .
H5B H 0.344736 0.238169 0.104904 0.030 Uiso 1 1 calc GR . . . .
H5C H 0.286114 0.144217 0.156685 0.030 Uiso 1 1 calc GR . . . .
C6 C 0.44941(13) 0.34832(16) 0.4525(2) 0.0190(4) Uani 1 1 d . . . . .
H6A H 0.471322 0.366689 0.563211 0.029 Uiso 1 1 calc GR . . . .
H6B H 0.470899 0.401596 0.389366 0.029 Uiso 1 1 calc GR . . . .
H6C H 0.476657 0.280820 0.434613 0.029 Uiso 1 1 calc GR . . . .
C7 C 0.31829(14) 0.48411(15) 0.6024(2) 0.0200(4) Uani 1 1 d . . . . .
H7A H 0.267802 0.501472 0.655600 0.030 Uiso 1 1 calc GR . . . .
H7B H 0.338101 0.547224 0.556499 0.030 Uiso 1 1 calc GR . . . .
H7C H 0.374034 0.454518 0.677763 0.030 Uiso 1 1 calc GR . . . .
C8 C 0.09788(13) 0.44327(15) 0.4534(2) 0.0189(4) Uani 1 1 d . . . . .
H8A H 0.041659 0.397097 0.435948 0.028 Uiso 1 1 calc GR . . . .
H8B H 0.080913 0.506240 0.390059 0.028 Uiso 1 1 calc GR . . . .
H8C H 0.117869 0.462352 0.564002 0.028 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 P1 2.2932(5) . ?
Fe1 P1 2.2932(5) 7_556 ?
Fe1 C1 2.0943(18) 7_556 ?
Fe1 C1 2.0943(18) . ?
Fe1 C2 2.0698(17) 7_556 ?
Fe1 C2 2.0698(17) . ?
Fe1 C3 2.0721(18) . ?
Fe1 C3 2.0721(18) 7_556 ?
Fe1 C4 2.1027(18) 7_556 ?
Fe1 C4 2.1027(18) . ?
P1 C1 1.7783(19) . ?
P1 C4 1.7826(19) . ?
C1 C2 1.419(3) . ?
C1 C5 1.509(3) . ?
C2 C3 1.437(3) . ?
C2 C6 1.509(2) . ?
C3 C4 1.426(2) . ?
C3 C7 1.505(3) . ?
C4 C8 1.508(2) . ?

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
P1 Fe1 P1 180.0 7_556 . ?
C1 Fe1 P1 132.45(5) 7_556 . ?
C1 Fe1 P1 47.55(5) 7_556 7_556 ?
C1 Fe1 P1 47.56(5) . . ?
C1 Fe1 P1 132.44(5) . 7_556 ?
C1 Fe1 C1 180.0 7_556 . ?
C1 Fe1 C4 73.58(7) . . ?
C1 Fe1 C4 106.42(7) 7_556 . ?
C1 Fe1 C4 106.42(7) . 7_556 ?
C1 Fe1 C4 73.58(7) 7_556 7_556 ?
C2 Fe1 P1 104.58(5) . 7_556 ?
C2 Fe1 P1 75.42(5) 7_556 7_556 ?
C2 Fe1 P1 75.42(5) . . ?
C2 Fe1 P1 104.58(5) 7_556 . ?
C2 Fe1 C1 140.16(7) 7_556 . ?
C2 Fe1 C1 39.84(7) . . ?
C2 Fe1 C1 39.84(7) 7_556 7_556 ?
C2 Fe1 C1 140.15(7) . 7_556 ?
C2 Fe1 C2 180.0 . 7_556 ?
C2 Fe1 C3 139.40(7) . 7_556 ?
C2 Fe1 C3 40.60(7) 7_556 7_556 ?
C2 Fe1 C3 139.40(7) 7_556 . ?
C2 Fe1 C3 40.60(7) . . ?
C2 Fe1 C4 69.44(7) 7_556 7_556 ?
C2 Fe1 C4 110.56(7) 7_556 . ?
C2 Fe1 C4 69.44(7) . . ?
C2 Fe1 C4 110.56(7) . 7_556 ?
C3 Fe1 P1 75.48(5) 7_556 7_556 ?
C3 Fe1 P1 104.52(5) 7_556 . ?
C3 Fe1 P1 75.48(5) . . ?
C3 Fe1 P1 104.52(5) . 7_556 ?
C3 Fe1 C1 110.62(7) . 7_556 ?
C3 Fe1 C1 69.38(7) 7_556 7_556 ?
C3 Fe1 C1 69.38(7) . . ?
C3 Fe1 C1 110.62(7) 7_556 . ?
C3 Fe1 C3 180.0 7_556 . ?
C3 Fe1 C4 39.94(7) . . ?
C3 Fe1 C4 140.06(7) . 7_556 ?
C3 Fe1 C4 39.94(7) 7_556 7_556 ?
C3 Fe1 C4 140.06(7) 7_556 . ?
C4 Fe1 P1 47.60(5) . . ?
C4 Fe1 P1 132.40(5) 7_556 . ?
C4 Fe1 P1 47.60(5) 7_556 7_556 ?
C4 Fe1 P1 132.40(5) . 7_556 ?
C4 Fe1 C4 180.00(11) . 7_556 ?
C1 P1 Fe1 60.35(6) . . ?
C1 P1 C4 89.80(9) . . ?
C4 P1 Fe1 60.59(6) . . ?
P1 C1 Fe1 72.10(6) . . ?
C2 C1 Fe1 69.15(10) . . ?
C2 C1 P1 113.06(13) . . ?
C2 C1 C5 124.04(17) . . ?
C5 C1 Fe1 128.57(14) . . ?
C5 C1 P1 122.87(14) . . ?
C1 C2 Fe1 71.01(10) . . ?
C1 C2 C3 112.26(16) . . ?
C1 C2 C6 124.49(16) . . ?
C3 C2 Fe1 69.79(10) . . ?
C3 C2 C6 123.20(16) . . ?
C6 C2 Fe1 129.03(13) . . ?
C2 C3 Fe1 69.61(10) . . ?
C2 C3 C7 123.35(17) . . ?
C4 C3 Fe1 71.18(10) . . ?
C4 C3 C2 112.21(16) . . ?
C4 C3 C7 124.43(17) . . ?
C7 C3 Fe1 127.91(13) . . ?
P1 C4 Fe1 71.81(6) . . ?
C3 C4 Fe1 68.87(10) . . ?
C3 C4 P1 112.65(13) . . ?
C3 C4 C8 125.05(16) . . ?
C8 C4 Fe1 128.33(12) . . ?
C8 C4 P1 122.30(13) . . ?

_olex2_exptl_crystal_mounting_method 'From paratone on a microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.130
_oxdiff_exptl_absorpt_empirical_full_min 0.909
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Fe
_database_code_depnum_ccdc_archive 'CCDC 2003388'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         dq0907
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   25s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         9/12/18
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      9/13/18
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     9/13/18
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   9/13/18
_LANL_internal_validation_user   CAPG
_LANL_internal_validation_date   10/1/2020
_LANL_internal_archive_date      10/1/2020
_LANL_internal_LA-UR             ?

_audit_creation_date             2018-09-13
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H24 Fe P2, C18 H36 K N2 O6'
_chemical_formula_sum            'C34 H60 Fe K N2 O6 P2'
_chemical_formula_weight         749.73
_chemical_melting_point          ?
_chemical_oxdiff_formula         Fe(PC8H12)2KN2O6C18H36
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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 0.0060 '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'

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

_cell_length_a                   10.1947(2)
_cell_length_b                   14.2373(4)
_cell_length_c                   15.0677(3)
_cell_angle_alpha                62.275(2)
_cell_angle_beta                 85.840(2)
_cell_angle_gamma                87.045(2)
_cell_volume                     1930.42(8)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5215
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      26.1110
_cell_measurement_theta_min      2.4590
_shelx_estimated_absorpt_T_max   0.969
_shelx_estimated_absorpt_T_min   0.860
_exptl_absorpt_coefficient_mu    0.624
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.87191
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear blue'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    blue
_exptl_crystal_density_diffrn    1.290
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             802
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF layered with hexane.'
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0359
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            25573
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.370
_diffrn_reflns_theta_min         1.616
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.27 185.27   0.50   25.00    --   28.00  73.72 -25.73  366
  2  ω      2.27 185.27   0.50   25.00    --   28.00  73.72  64.27  366
  3  ω      2.27 185.27   0.50   25.00    --   28.00  73.72 154.27  366
  4  ω      2.27 185.27   0.50   25.00    --   28.00  73.72-115.73  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0107225000
_diffrn_orient_matrix_UB_12      -0.0512785000
_diffrn_orient_matrix_UB_13      0.0036681000
_diffrn_orient_matrix_UB_21      -0.0302555000
_diffrn_orient_matrix_UB_22      -0.0229433000
_diffrn_orient_matrix_UB_23      0.0491882000
_diffrn_orient_matrix_UB_31      -0.0619514000
_diffrn_orient_matrix_UB_32      0.0036085000
_diffrn_orient_matrix_UB_33      -0.0200929000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                6351
_reflns_number_total             7807
_reflns_odcompleteness_completeness 98.96
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_refine_diff_density_max         0.618
_refine_diff_density_min         -0.256
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7807
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0540
_refine_ls_R_factor_gt           0.0400
_refine_ls_restrained_S_all      1.090
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0570P)²+0.6123P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1035
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Fe1 Fe 0.17882(3) 0.83796(2) 0.27487(2) 0.01685(9) Uani 1 1 d . . . . .
P1 P 0.18715(6) 0.94814(4) 0.35445(4) 0.02110(14) Uani 1 1 d . . . . .
P2 P 0.21224(5) 0.68326(4) 0.24957(4) 0.01866(13) Uani 1 1 d . . . . .
C1 C 0.1721(2) 1.00435(16) 0.22295(15) 0.0181(4) Uani 1 1 d . . . . .
C2 C 0.2785(2) 0.97523(16) 0.17285(16) 0.0182(4) Uani 1 1 d . . . . .
C3 C 0.3706(2) 0.90342(17) 0.24063(17) 0.0207(5) Uani 1 1 d . . . . .
C4 C 0.3294(2) 0.87414(17) 0.34203(17) 0.0229(5) Uani 1 1 d . . . . .
C5 C 0.0667(2) 1.08503(18) 0.16825(18) 0.0262(5) Uani 1 1 d . . . . .
H5A H 0.036696 1.071901 0.114741 0.039 Uiso 1 1 calc GR . . . .
H5B H 0.102475 1.156510 0.138938 0.039 Uiso 1 1 calc GR . . . .
H5C H -0.007588 1.079122 0.215516 0.039 Uiso 1 1 calc GR . . . .
C6 C 0.2991(2) 1.02313(19) 0.06004(17) 0.0280(5) Uani 1 1 d . . . . .
H6A H 0.342258 0.970614 0.042234 0.042 Uiso 1 1 calc GR . . . .
H6B H 0.354513 1.085524 0.035194 0.042 Uiso 1 1 calc GR . . . .
H6C H 0.213784 1.044326 0.029508 0.042 Uiso 1 1 calc GR . . . .
C7 C 0.4949(2) 0.86523(19) 0.2062(2) 0.0315(6) Uani 1 1 d . . . . .
H7A H 0.535940 0.808114 0.264458 0.047 Uiso 1 1 calc GR . . . .
H7B H 0.555858 0.924163 0.172147 0.047 Uiso 1 1 calc GR . . . .
H7C H 0.473827 0.838551 0.159688 0.047 Uiso 1 1 calc GR . . . .
C8 C 0.4054(3) 0.79832(19) 0.43009(19) 0.0357(6) Uani 1 1 d . . . . .
H8A H 0.348425 0.773690 0.491619 0.054 Uiso 1 1 calc GR . . . .
H8B H 0.481097 0.834408 0.435996 0.054 Uiso 1 1 calc GR . . . .
H8C H 0.436342 0.737407 0.420113 0.054 Uiso 1 1 calc GR . . . .
C9 C 0.0936(2) 0.78464(17) 0.18529(16) 0.0203(5) Uani 1 1 d . . . . .
C10 C -0.0049(2) 0.79807(18) 0.25211(18) 0.0246(5) Uani 1 1 d . . . . .
C11 C 0.0212(2) 0.73316(18) 0.35420(18) 0.0262(5) Uani 1 1 d . . . . .
C12 C 0.1409(2) 0.67452(17) 0.36570(17) 0.0239(5) Uani 1 1 d . . . . .
C13 C 0.0860(2) 0.83945(18) 0.07337(17) 0.0290(5) Uani 1 1 d . . . . .
H13A H 0.048430 0.911073 0.051547 0.043 Uiso 1 1 calc GR . . . .
H13B H 0.030052 0.799068 0.053690 0.043 Uiso 1 1 calc GR . . . .
H13C H 0.174460 0.844046 0.041706 0.043 Uiso 1 1 calc GR . . . .
C14 C -0.1269(2) 0.8675(2) 0.2177(2) 0.0384(7) Uani 1 1 d . . . . .
H14A H -0.150192 0.898590 0.262830 0.058 Uiso 1 1 calc GR . . . .
H14B H -0.199701 0.824587 0.218735 0.058 Uiso 1 1 calc GR . . . .
H14C H -0.109952 0.924318 0.149263 0.058 Uiso 1 1 calc GR . . . .
C15 C -0.0693(3) 0.7279(2) 0.4403(2) 0.0412(7) Uani 1 1 d . . . . .
H15A H -0.022227 0.694795 0.502412 0.062 Uiso 1 1 calc GR . . . .
H15B H -0.146026 0.685708 0.447536 0.062 Uiso 1 1 calc GR . . . .
H15C H -0.098227 0.799857 0.426641 0.062 Uiso 1 1 calc GR . . . .
C16 C 0.1930(3) 0.59973(19) 0.46655(17) 0.0356(6) Uani 1 1 d . . . . .
H16A H 0.286630 0.584644 0.457964 0.053 Uiso 1 1 calc GR . . . .
H16B H 0.144451 0.533402 0.495978 0.053 Uiso 1 1 calc GR . . . .
H16C H 0.181799 0.632596 0.511182 0.053 Uiso 1 1 calc GR . . . .
K1 K 0.31999(4) 0.64649(3) 0.77999(3) 0.01728(11) Uani 1 1 d . . . . .
O1 O 0.15883(14) 0.82840(11) 0.68719(11) 0.0209(3) Uani 1 1 d . . . . .
O2 O 0.08027(14) 0.63110(12) 0.70794(12) 0.0232(3) Uani 1 1 d . . . . .
O3 O 0.25392(17) 0.50205(13) 0.98689(12) 0.0326(4) Uani 1 1 d . . . . .
O4 O 0.39903(16) 0.68609(13) 0.93782(11) 0.0271(4) Uani 1 1 d . . . . .
O5 O 0.54788(14) 0.71711(12) 0.65258(11) 0.0213(3) Uani 1 1 d . . . . .
O6 O 0.47449(15) 0.50651(12) 0.72783(12) 0.0252(4) Uani 1 1 d . . . . .
N1 N 0.42558(18) 0.85830(14) 0.72600(14) 0.0219(4) Uani 1 1 d . . . . .
N2 N 0.21944(19) 0.43047(15) 0.83608(15) 0.0286(5) Uani 1 1 d . . . . .
C17 C 0.3170(2) 0.93802(18) 0.70051(19) 0.0270(5) Uani 1 1 d . . . . .
H17A H 0.354767 1.009809 0.665933 0.032 Uiso 1 1 calc R . . . .
H17B H 0.270232 0.930081 0.763453 0.032 Uiso 1 1 calc R . . . .
C18 C 0.2194(2) 0.92926(17) 0.63469(18) 0.0263(5) Uani 1 1 d . . . . .
H18A H 0.151840 0.986621 0.617649 0.032 Uiso 1 1 calc R . . . .
H18B H 0.264682 0.936546 0.571478 0.032 Uiso 1 1 calc R . . . .
C19 C 0.0545(2) 0.82007(18) 0.63273(17) 0.0236(5) Uani 1 1 d . . . . .
H19A H 0.089947 0.824795 0.567881 0.028 Uiso 1 1 calc R . . . .
H19B H -0.010513 0.878709 0.618765 0.028 Uiso 1 1 calc R . . . .
C20 C -0.0100(2) 0.71537(18) 0.69512(18) 0.0252(5) Uani 1 1 d . . . . .
H20A H -0.040112 0.709207 0.761539 0.030 Uiso 1 1 calc R . . . .
H20B H -0.087812 0.710812 0.661742 0.030 Uiso 1 1 calc R . . . .
C21 C 0.0174(2) 0.53064(19) 0.7535(2) 0.0335(6) Uani 1 1 d . . . . .
H21A H -0.052767 0.531544 0.711042 0.040 Uiso 1 1 calc R . . . .
H21B H -0.023561 0.516895 0.819965 0.040 Uiso 1 1 calc R . . . .
C22 C 0.1166(2) 0.44413(19) 0.7659(2) 0.0324(6) Uani 1 1 d . . . . .
H22A H 0.070179 0.376373 0.790828 0.039 Uiso 1 1 calc R . . . .
H22B H 0.159579 0.460422 0.699408 0.039 Uiso 1 1 calc R . . . .
C23 C 0.1654(3) 0.3802(2) 0.9397(2) 0.0416(7) Uani 1 1 d . . . . .
H23A H 0.154714 0.303698 0.961768 0.050 Uiso 1 1 calc R . . . .
H23B H 0.077065 0.411440 0.942270 0.050 Uiso 1 1 calc R . . . .
C24 C 0.2494(3) 0.3923(2) 1.0122(2) 0.0426(7) Uani 1 1 d . . . . .
H24A H 0.211706 0.351374 1.081718 0.051 Uiso 1 1 calc R . . . .
H24B H 0.339449 0.364330 1.008449 0.051 Uiso 1 1 calc R . . . .
C25 C 0.3197(3) 0.5174(2) 1.05893(18) 0.0366(6) Uani 1 1 d . . . . .
H25A H 0.410972 0.488849 1.062911 0.044 Uiso 1 1 calc R . . . .
H25B H 0.273987 0.478653 1.125898 0.044 Uiso 1 1 calc R . . . .
C26 C 0.3216(3) 0.6320(2) 1.02990(18) 0.0372(6) Uani 1 1 d . . . . .
H26A H 0.230663 0.661678 1.021298 0.045 Uiso 1 1 calc R . . . .
H26B H 0.359325 0.642222 1.083444 0.045 Uiso 1 1 calc R . . . .
C27 C 0.4129(3) 0.7949(2) 0.91164(19) 0.0339(6) Uani 1 1 d . . . . .
H27A H 0.457532 0.800766 0.965030 0.041 Uiso 1 1 calc R . . . .
H27B H 0.324941 0.829489 0.905744 0.041 Uiso 1 1 calc R . . . .
C28 C 0.4921(2) 0.85024(19) 0.81332(19) 0.0304(6) Uani 1 1 d . . . . .
H28A H 0.511865 0.922619 0.801575 0.037 Uiso 1 1 calc R . . . .
H28B H 0.576910 0.811352 0.818482 0.037 Uiso 1 1 calc R . . . .
C29 C 0.5192(2) 0.89031(18) 0.63910(18) 0.0276(5) Uani 1 1 d . . . . .
H29A H 0.567815 0.952277 0.631460 0.033 Uiso 1 1 calc R . . . .
H29B H 0.469453 0.913181 0.578083 0.033 Uiso 1 1 calc R . . . .
C30 C 0.6169(2) 0.80468(19) 0.64562(19) 0.0290(5) Uani 1 1 d . . . . .
H30A H 0.678012 0.832194 0.585258 0.035 Uiso 1 1 calc R . . . .
H30B H 0.669115 0.781900 0.705423 0.035 Uiso 1 1 calc R . . . .
C31 C 0.6345(2) 0.63967(18) 0.64445(17) 0.0263(5) Uani 1 1 d . . . . .
H31A H 0.689156 0.606346 0.703567 0.032 Uiso 1 1 calc R . . . .
H31B H 0.693902 0.674001 0.583531 0.032 Uiso 1 1 calc R . . . .
C32 C 0.5575(2) 0.55753(18) 0.63862(17) 0.0286(5) Uani 1 1 d . . . . .
H32A H 0.503232 0.590717 0.579275 0.034 Uiso 1 1 calc R . . . .
H32B H 0.617778 0.504520 0.631260 0.034 Uiso 1 1 calc R . . . .
C33 C 0.4125(3) 0.41828(19) 0.7294(2) 0.0362(6) Uani 1 1 d . . . . .
H33A H 0.480001 0.367642 0.725392 0.043 Uiso 1 1 calc R . . . .
H33B H 0.357473 0.442831 0.670784 0.043 Uiso 1 1 calc R . . . .
C34 C 0.3286(3) 0.36462(19) 0.8246(2) 0.0377(6) Uani 1 1 d . . . . .
H34A H 0.291793 0.300129 0.827585 0.045 Uiso 1 1 calc R . . . .
H34B H 0.385166 0.341568 0.882098 0.045 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Fe1 P1 2.3841(6) . ?
Fe1 P2 2.4078(6) . ?
Fe1 C1 2.120(2) . ?
Fe1 C2 2.097(2) . ?
Fe1 C3 2.134(2) . ?
Fe1 C4 2.106(2) . ?
Fe1 C9 2.085(2) . ?
Fe1 C10 2.082(2) . ?
Fe1 C11 2.132(2) . ?
Fe1 C12 2.119(2) . ?
P1 C1 1.774(2) . ?
P1 C4 1.798(2) . ?
P2 C9 1.782(2) . ?
P2 C12 1.797(2) . ?
C1 C2 1.430(3) . ?
C1 C5 1.508(3) . ?
C2 C3 1.428(3) . ?
C2 C6 1.511(3) . ?
C3 C4 1.420(3) . ?
C3 C7 1.505(3) . ?
C4 C8 1.502(3) . ?
C9 C10 1.439(3) . ?
C9 C13 1.499(3) . ?
C10 C11 1.415(3) . ?
C10 C14 1.511(3) . ?
C11 C12 1.417(3) . ?
C11 C15 1.510(3) . ?
C12 C16 1.509(3) . ?
K1 O1 2.8083(15) . ?
K1 O2 2.8037(15) . ?
K1 O3 2.8765(16) . ?
K1 O4 2.8626(16) . ?
K1 O5 2.8092(15) . ?
K1 O6 2.8328(15) . ?
K1 N1 2.9730(18) . ?
K1 N2 3.0009(19) . ?
O1 C18 1.426(3) . ?
O1 C19 1.431(3) . ?
O2 C20 1.421(3) . ?
O2 C21 1.430(3) . ?
O3 C24 1.429(3) . ?
O3 C25 1.420(3) . ?
O4 C26 1.432(3) . ?
O4 C27 1.422(3) . ?
O5 C30 1.421(3) . ?
O5 C31 1.422(3) . ?
O6 C32 1.428(3) . ?
O6 C33 1.425(3) . ?
N1 C17 1.479(3) . ?
N1 C28 1.478(3) . ?
N1 C29 1.463(3) . ?
N2 C22 1.484(3) . ?
N2 C23 1.459(3) . ?
N2 C34 1.471(3) . ?
C17 C18 1.503(3) . ?
C19 C20 1.498(3) . ?
C21 C22 1.503(3) . ?
C23 C24 1.510(4) . ?
C25 C26 1.481(4) . ?
C27 C28 1.508(4) . ?
C29 C30 1.506(3) . ?
C31 C32 1.481(4) . ?
C33 C34 1.498(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P1 Fe1 P2 158.60(2) . . ?
C1 Fe1 P1 45.92(6) . . ?
C1 Fe1 P2 152.52(6) . . ?
C1 Fe1 C3 67.97(8) . . ?
C1 Fe1 C11 125.19(9) . . ?
C2 Fe1 P1 73.18(6) . . ?
C2 Fe1 P2 116.98(6) . . ?
C2 Fe1 C1 39.63(8) . . ?
C2 Fe1 C3 39.44(8) . . ?
C2 Fe1 C4 68.11(8) . . ?
C2 Fe1 C11 160.13(9) . . ?
C2 Fe1 C12 159.14(9) . . ?
C3 Fe1 P1 73.07(6) . . ?
C3 Fe1 P2 102.35(6) . . ?
C4 Fe1 P1 46.71(6) . . ?
C4 Fe1 P2 117.07(6) . . ?
C4 Fe1 C1 72.48(8) . . ?
C4 Fe1 C3 39.13(9) . . ?
C4 Fe1 C11 125.17(9) . . ?
C4 Fe1 C12 106.19(9) . . ?
C9 Fe1 P1 153.53(6) . . ?
C9 Fe1 P2 46.04(6) . . ?
C9 Fe1 C1 116.06(8) . . ?
C9 Fe1 C2 104.65(8) . . ?
C9 Fe1 C3 122.52(9) . . ?
C9 Fe1 C4 157.92(9) . . ?
C9 Fe1 C11 68.31(9) . . ?
C9 Fe1 C12 72.83(9) . . ?
C10 Fe1 P1 118.23(6) . . ?
C10 Fe1 P2 73.28(6) . . ?
C10 Fe1 C1 106.30(8) . . ?
C10 Fe1 C2 123.77(9) . . ?
C10 Fe1 C3 159.25(9) . . ?
C10 Fe1 C4 160.56(9) . . ?
C10 Fe1 C9 40.41(9) . . ?
C10 Fe1 C11 39.23(9) . . ?
C10 Fe1 C12 68.10(9) . . ?
C11 Fe1 P1 104.50(6) . . ?
C11 Fe1 P2 72.39(6) . . ?
C11 Fe1 C3 159.85(9) . . ?
C12 Fe1 P1 118.47(6) . . ?
C12 Fe1 P2 46.22(6) . . ?
C12 Fe1 C1 160.14(8) . . ?
C12 Fe1 C3 123.91(9) . . ?
C12 Fe1 C11 38.94(9) . . ?
C1 P1 Fe1 59.17(7) . . ?
C1 P1 C4 88.77(10) . . ?
C4 P1 Fe1 58.50(7) . . ?
C9 P2 Fe1 57.37(7) . . ?
C9 P2 C12 88.44(10) . . ?
C12 P2 Fe1 58.38(7) . . ?
P1 C1 Fe1 74.91(8) . . ?
C2 C1 Fe1 69.31(12) . . ?
C2 C1 P1 113.21(15) . . ?
C2 C1 C5 123.27(19) . . ?
C5 C1 Fe1 129.72(15) . . ?
C5 C1 P1 123.13(16) . . ?
C1 C2 Fe1 71.06(12) . . ?
C1 C2 C6 123.9(2) . . ?
C3 C2 Fe1 71.66(12) . . ?
C3 C2 C1 112.63(19) . . ?
C3 C2 C6 123.21(19) . . ?
C6 C2 Fe1 129.94(15) . . ?
C2 C3 Fe1 68.89(12) . . ?
C2 C3 C7 123.0(2) . . ?
C4 C3 Fe1 69.40(12) . . ?
C4 C3 C2 111.45(18) . . ?
C4 C3 C7 125.6(2) . . ?
C7 C3 Fe1 129.19(15) . . ?
P1 C4 Fe1 74.79(8) . . ?
C3 C4 Fe1 71.47(12) . . ?
C3 C4 P1 113.31(15) . . ?
C3 C4 C8 123.5(2) . . ?
C8 C4 Fe1 127.49(16) . . ?
C8 C4 P1 122.78(18) . . ?
P2 C9 Fe1 76.59(8) . . ?
C10 C9 Fe1 69.68(12) . . ?
C10 C9 P2 112.98(17) . . ?
C10 C9 C13 123.1(2) . . ?
C13 C9 Fe1 128.34(16) . . ?
C13 C9 P2 123.35(17) . . ?
C9 C10 Fe1 69.90(12) . . ?
C9 C10 C14 124.0(2) . . ?
C11 C10 Fe1 72.31(13) . . ?
C11 C10 C9 112.1(2) . . ?
C11 C10 C14 123.8(2) . . ?
C14 C10 Fe1 128.73(16) . . ?
C10 C11 Fe1 68.47(12) . . ?
C10 C11 C12 112.31(19) . . ?
C10 C11 C15 123.2(2) . . ?
C12 C11 Fe1 70.03(13) . . ?
C12 C11 C15 124.4(2) . . ?
C15 C11 Fe1 129.49(16) . . ?
P2 C12 Fe1 75.39(8) . . ?
C11 C12 Fe1 71.03(13) . . ?
C11 C12 P2 113.14(17) . . ?
C11 C12 C16 123.3(2) . . ?
C16 C12 Fe1 128.64(17) . . ?
C16 C12 P2 122.94(18) . . ?
O1 K1 O3 117.29(5) . . ?
O1 K1 O4 97.12(5) . . ?
O1 K1 O5 99.32(4) . . ?
O1 K1 O6 138.82(5) . . ?
O1 K1 N1 60.49(5) . . ?
O1 K1 N2 120.81(5) . . ?
O2 K1 O1 60.56(4) . . ?
O2 K1 O3 95.69(5) . . ?
O2 K1 O4 135.94(5) . . ?
O2 K1 O5 121.55(5) . . ?
O2 K1 O6 98.86(5) . . ?
O2 K1 N1 120.11(5) . . ?
O2 K1 N2 61.16(5) . . ?
O3 K1 N1 119.77(5) . . ?
O3 K1 N2 59.95(5) . . ?
O4 K1 O3 59.21(5) . . ?
O4 K1 N1 61.58(5) . . ?
O4 K1 N2 117.87(5) . . ?
O5 K1 O3 137.78(5) . . ?
O5 K1 O4 98.01(5) . . ?
O5 K1 O6 59.26(4) . . ?
O5 K1 N1 60.20(5) . . ?
O5 K1 N2 119.02(5) . . ?
O6 K1 O3 98.85(5) . . ?
O6 K1 O4 119.11(5) . . ?
O6 K1 N1 118.69(5) . . ?
O6 K1 N2 60.37(5) . . ?
N1 K1 N2 178.70(5) . . ?
C18 O1 K1 118.58(12) . . ?
C18 O1 C19 111.29(16) . . ?
C19 O1 K1 115.81(12) . . ?
C20 O2 K1 113.29(12) . . ?
C20 O2 C21 111.83(17) . . ?
C21 O2 K1 118.32(13) . . ?
C24 O3 K1 116.51(15) . . ?
C25 O3 K1 115.85(13) . . ?
C25 O3 C24 111.61(19) . . ?
C26 O4 K1 113.45(13) . . ?
C27 O4 K1 115.15(13) . . ?
C27 O4 C26 111.38(18) . . ?
C30 O5 K1 120.03(12) . . ?
C30 O5 C31 111.90(17) . . ?
C31 O5 K1 118.03(12) . . ?
C32 O6 K1 114.72(12) . . ?
C33 O6 K1 118.55(14) . . ?
C33 O6 C32 110.12(18) . . ?
C17 N1 K1 109.97(13) . . ?
C28 N1 K1 108.09(13) . . ?
C28 N1 C17 110.05(18) . . ?
C29 N1 K1 109.78(12) . . ?
C29 N1 C17 108.88(18) . . ?
C29 N1 C28 110.06(18) . . ?
C22 N2 K1 107.54(13) . . ?
C23 N2 K1 110.63(15) . . ?
C23 N2 C22 110.6(2) . . ?
C23 N2 C34 109.5(2) . . ?
C34 N2 K1 108.90(14) . . ?
C34 N2 C22 109.5(2) . . ?
N1 C17 C18 113.75(18) . . ?
O1 C18 C17 108.80(18) . . ?
O1 C19 C20 108.32(18) . . ?
O2 C20 C19 110.05(17) . . ?
O2 C21 C22 109.90(19) . . ?
N2 C22 C21 113.5(2) . . ?
N2 C23 C24 113.8(2) . . ?
O3 C24 C23 109.0(2) . . ?
O3 C25 C26 109.7(2) . . ?
O4 C26 C25 109.5(2) . . ?
O4 C27 C28 110.15(19) . . ?
N1 C28 C27 113.91(19) . . ?
N1 C29 C30 114.28(19) . . ?
O5 C30 C29 108.96(18) . . ?
O5 C31 C32 109.72(19) . . ?
O6 C32 C31 109.43(18) . . ?
O6 C33 C34 109.1(2) . . ?
N2 C34 C33 114.8(2) . . ?

_olex2_exptl_crystal_mounting_method 'From paratone on a microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.080
_oxdiff_exptl_absorpt_empirical_full_min 0.915
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Heat-sensitive
####################################################################### 
# 
# 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_8
_database_code_depnum_ccdc_archive 'CCDC 2017381'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         dq0919
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   20s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         9/27/18
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      9/27/18
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     9/28/18
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   9/28/18
_LANL_internal_validation_user   ?
_LANL_internal_validation_date   ?
_LANL_internal_archive_date      ?
_LANL_internal_LA-UR             ?

_refine_special_details          
;
Positional disorder was identified about atoms K1 and K2, and a model was 
constructed with 2 complete K(crypt) moieties at each site. These were refined 
competetively, converging at ratios (FVAR3 and 4) of 0.88(1):0.12(1) and 
0.91(1):0.09(1). The C, O, and N atoms on these moieties were refined with very 
low occupancies thus bond distances are not statistically significant. 
Similarity restraints (SIMU) were applied to all K(crypt) units. 

Additionally, disorder was identified at TMP unit P2, C27-C34, which was 
modelled over two sites and refined competetively, converging at a ratio 
(FVAR2) of 0.82(1):0.18(1), and similarity restraints (SIMU) were applied to 
both moieties. 

Finally, THF molecule O13, C53-C56 was found to be disordered over two 
positions which were refined competetively, converging at a ratio (FVAR5) of 
o.83(1):0.17(1), and both moieties had similarity restraints (SIMU) applied. 

No twinning was observed by inspection of the reflections using the 
EwaldExplorer in CrysAlisPro, or by PLATON's TWINROTMAT tool.'
;

_audit_creation_date             2018-09-28
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         '2(C8 H12 P), C4 H8 O, 2(C18 H36 K N2 O6)'
_chemical_formula_sum            'C56 H104 K2 N4 O13 P2'
_chemical_formula_weight         1181.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         KN2O6C18H36PC8H13
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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 0.0060 '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'

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

_cell_length_a                   12.7189(8)
_cell_length_b                   15.9437(10)
_cell_length_c                   17.8937(12)
_cell_angle_alpha                64.066(6)
_cell_angle_beta                 85.655(5)
_cell_angle_gamma                86.321(5)
_cell_volume                     3251.9(4)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    3339
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      24.5100
_cell_measurement_theta_min      2.0230
_shelx_estimated_absorpt_T_max   0.987
_shelx_estimated_absorpt_T_min   0.912
_exptl_absorpt_coefficient_mu    0.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.82591
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.207
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF.'
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.05
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0646
_diffrn_reflns_av_unetI/netI     0.0934
_diffrn_reflns_Laue_measured_fraction_full 0.985
_diffrn_reflns_Laue_measured_fraction_max 0.981
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            31744
_diffrn_reflns_point_group_measured_fraction_full 0.985
_diffrn_reflns_point_group_measured_fraction_max 0.981
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.993
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.981
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.27 185.27   0.50   20.00    --   28.00  73.72 -25.73  366
  2  ω      2.27 185.27   0.50   20.00    --   28.00  73.72  64.27  366
  3  ω      2.27 185.27   0.50   20.00    --   28.00  73.72 154.27  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0555311000
_diffrn_orient_matrix_UB_12      -0.0013645000
_diffrn_orient_matrix_UB_13      -0.0073585000
_diffrn_orient_matrix_UB_21      0.0037526000
_diffrn_orient_matrix_UB_22      -0.0430916000
_diffrn_orient_matrix_UB_23      0.0360408000
_diffrn_orient_matrix_UB_31      -0.0058233000
_diffrn_orient_matrix_UB_32      -0.0243193000
_diffrn_orient_matrix_UB_33      -0.0243997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                8417
_reflns_number_total             13040
_reflns_odcompleteness_completeness 98.10
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.726
_refine_diff_density_min         -0.543
_refine_diff_density_rms         0.099
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1310
_refine_ls_number_reflns         13040
_refine_ls_number_restraints     2121
_refine_ls_R_factor_all          0.1063
_refine_ls_R_factor_gt           0.0673
_refine_ls_restrained_S_all      1.016
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0743P)²+0.3849P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1648
_refine_ls_wR_factor_ref         0.1979

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 O13A-C56A \\sim O13A-C53A \\sim O13B-C56B \\sim O13B-C53B
 with sigma of 0.005
 C55B-C54B \\sim C55A-C54A
 with sigma of 0.005
 C56B-C55B \\sim C54B-C53B \\sim C54A-C53A \\sim C56A-C55A
 with sigma of 0.005
3. Uiso/Uaniso restraints and constraints
P2A \\sim C27A \\sim C28A \\sim C29A \\sim C30A \\sim C31A \\sim C32A \\sim
C33A \\sim C34A \\sim P2B \\sim C27B \\sim C28B \\sim C29B \\sim C30B \\sim
C31B \\sim C32B \\sim C33B \\sim C34B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.01
K2A \\sim O7A \\sim O8A \\sim O9A \\sim O10A \\sim O11A \\sim O12A \\sim N3A
\\sim N4A \\sim C35A \\sim C36A \\sim C37A \\sim C38A \\sim C39A \\sim C40A
\\sim C41A \\sim C42A \\sim C43A \\sim C44A \\sim C45A \\sim C46A \\sim C47A
\\sim C48A \\sim C49A \\sim C50A \\sim C51A \\sim C52A \\sim K2B \\sim O7B
\\sim O8B \\sim O9B \\sim O10B \\sim O11B \\sim O12B \\sim N3B \\sim N4B \\sim
C35B \\sim C36B \\sim C37B \\sim C38B \\sim C39B \\sim C40B \\sim C41B \\sim
C42B \\sim C43B \\sim C44B \\sim C45B \\sim C46B \\sim C47B \\sim C48B \\sim
C49B \\sim C50B \\sim C51B \\sim C52B: within 2A with sigma of 0.005 and sigma
for terminal atoms of 0.005
O6B \\sim K1B \\sim O1B \\sim O2B \\sim O3B \\sim O5B \\sim O4B \\sim N1B \\sim
N2B \\sim C10B \\sim C11B \\sim C24B \\sim C25B \\sim C12B \\sim C13B \\sim
C16B \\sim C17B \\sim C22B \\sim C23B \\sim C18B \\sim C19B \\sim C9B \\sim
C20B \\sim C21B \\sim C14B \\sim C15B \\sim C26B \\sim C23A \\sim K1A \\sim O1A
\\sim O6A \\sim O2A \\sim O3A \\sim O4A \\sim O5A \\sim N1A \\sim N2A \\sim
C10A \\sim C11A \\sim C24A \\sim C25A \\sim C12A \\sim C13A \\sim C16A \\sim
C17A \\sim C18A \\sim C19A \\sim C22A \\sim C9A \\sim C20A \\sim C21A \\sim
C14A \\sim C15A \\sim C26A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
C56A \\sim O13A \\sim C53A \\sim C54A \\sim C55A: within 2A with sigma of 0.005
and sigma for terminal atoms of 0.005
C56B \\sim C53B \\sim O13B \\sim C54B \\sim C55B \\sim C55A \\sim O13A \\sim
C53A \\sim C56A \\sim C54A: within 2A with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Sof(P2B)=Sof(C27B)=Sof(C28B)=Sof(C29B)=Sof(C30B)=Sof(C31B)=Sof(H31D)=
 Sof(H31E)=Sof(H31F)=Sof(C32B)=Sof(H32D)=Sof(H32E)=Sof(H32F)=Sof(C33B)=
 Sof(H33D)=Sof(H33E)=Sof(H33F)=Sof(C34B)=Sof(H34D)=Sof(H34E)=Sof(H34F)=1-FVAR(1)
 Sof(P2A)=Sof(C27A)=Sof(C28A)=Sof(C29A)=Sof(C30A)=Sof(C31A)=Sof(H31A)=
 Sof(H31B)=Sof(H31C)=Sof(C32A)=Sof(H32A)=Sof(H32B)=Sof(H32C)=Sof(C33A)=
 Sof(H33A)=Sof(H33B)=Sof(H33C)=Sof(C34A)=Sof(H34A)=Sof(H34B)=Sof(H34C)=FVAR(1)
 Sof(K2B)=Sof(O7B)=Sof(O8B)=Sof(O9B)=Sof(O10B)=Sof(O11B)=Sof(O12B)=Sof(N3B)=
 Sof(N4B)=Sof(C35B)=Sof(H35C)=Sof(H35D)=Sof(C36B)=Sof(H36C)=Sof(H36D)=Sof(C37B)=
 Sof(H37C)=Sof(H37D)=Sof(C38B)=Sof(H38C)=Sof(H38D)=Sof(C39B)=Sof(H39C)=
 Sof(H39D)=Sof(C40B)=Sof(H40C)=Sof(H40D)=Sof(C41B)=Sof(H41C)=Sof(H41D)=
 Sof(C42B)=Sof(H42C)=Sof(H42D)=Sof(C43B)=Sof(H43C)=Sof(H43D)=Sof(C44B)=
 Sof(H44C)=Sof(H44D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=Sof(C46B)=Sof(H46C)=
 Sof(H46D)=Sof(C47B)=Sof(H47C)=Sof(H47D)=Sof(C48B)=Sof(H48C)=Sof(H48D)=
 Sof(C49B)=Sof(H49C)=Sof(H49D)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=
 Sof(H51C)=Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=1-FVAR(2)
 Sof(K2A)=Sof(O7A)=Sof(O8A)=Sof(O9A)=Sof(O10A)=Sof(O11A)=Sof(O12A)=Sof(N3A)=
 Sof(N4A)=Sof(C35A)=Sof(H35A)=Sof(H35B)=Sof(C36A)=Sof(H36A)=Sof(H36B)=Sof(C37A)=
 Sof(H37A)=Sof(H37B)=Sof(C38A)=Sof(H38A)=Sof(H38B)=Sof(C39A)=Sof(H39A)=
 Sof(H39B)=Sof(C40A)=Sof(H40A)=Sof(H40B)=Sof(C41A)=Sof(H41A)=Sof(H41B)=
 Sof(C42A)=Sof(H42A)=Sof(H42B)=Sof(C43A)=Sof(H43A)=Sof(H43B)=Sof(C44A)=
 Sof(H44A)=Sof(H44B)=Sof(C45A)=Sof(H45A)=Sof(H45B)=Sof(C46A)=Sof(H46A)=
 Sof(H46B)=Sof(C47A)=Sof(H47A)=Sof(H47B)=Sof(C48A)=Sof(H48A)=Sof(H48B)=
 Sof(C49A)=Sof(H49A)=Sof(H49B)=Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C51A)=
 Sof(H51A)=Sof(H51B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=FVAR(2)
 Sof(K1B)=Sof(O1B)=Sof(O2B)=Sof(O3B)=Sof(O4B)=Sof(O5B)=Sof(O6B)=Sof(N1B)=
 Sof(N2B)=Sof(C9B)=Sof(H9BA)=Sof(H9BB)=Sof(C10B)=Sof(H10A)=Sof(H10B)=Sof(C11B)=
 Sof(H11A)=Sof(H11B)=Sof(C12B)=Sof(H12A)=Sof(H12B)=Sof(C13B)=Sof(H13A)=
 Sof(H13B)=Sof(C14B)=Sof(H14A)=Sof(H14B)=Sof(C15B)=Sof(H15A)=Sof(H15B)=
 Sof(C16B)=Sof(H16A)=Sof(H16B)=Sof(C17B)=Sof(H17A)=Sof(H17B)=Sof(C18B)=
 Sof(H18A)=Sof(H18B)=Sof(C19B)=Sof(H19A)=Sof(H19B)=Sof(C20B)=Sof(H20A)=
 Sof(H20B)=Sof(C21B)=Sof(H21A)=Sof(H21B)=Sof(C22B)=Sof(H22A)=Sof(H22B)=
 Sof(C23B)=Sof(H23A)=Sof(H23B)=Sof(C24B)=Sof(H24A)=Sof(H24B)=Sof(C25B)=
 Sof(H25A)=Sof(H25B)=Sof(C26B)=Sof(H26A)=Sof(H26B)=1-FVAR(3)
 Sof(K1A)=Sof(O1A)=Sof(O2A)=Sof(O3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(N1A)=
 Sof(N2A)=Sof(C9A)=Sof(H9AA)=Sof(H9AB)=Sof(C10A)=Sof(H10C)=Sof(H10D)=Sof(C11A)=
 Sof(H11C)=Sof(H11D)=Sof(C12A)=Sof(H12C)=Sof(H12D)=Sof(C13A)=Sof(H13C)=
 Sof(H13D)=Sof(C14A)=Sof(H14C)=Sof(H14D)=Sof(C15A)=Sof(H15C)=Sof(H15D)=
 Sof(C16A)=Sof(H16C)=Sof(H16D)=Sof(C17A)=Sof(H17C)=Sof(H17D)=Sof(C18A)=
 Sof(H18C)=Sof(H18D)=Sof(C19A)=Sof(H19C)=Sof(H19D)=Sof(C20A)=Sof(H20C)=
 Sof(H20D)=Sof(C21A)=Sof(H21C)=Sof(H21D)=Sof(C22A)=Sof(H22C)=Sof(H22D)=
 Sof(C23A)=Sof(H23C)=Sof(H23D)=Sof(C24A)=Sof(H24C)=Sof(H24D)=Sof(C25A)=
 Sof(H25C)=Sof(H25D)=Sof(C26A)=Sof(H26C)=Sof(H26D)=FVAR(3)
 Sof(C53B)=Sof(H53C)=Sof(H53D)=Sof(O13B)=Sof(C56B)=Sof(H56C)=Sof(H56D)=
 Sof(C54B)=Sof(H54C)=Sof(H54D)=Sof(C55B)=Sof(H55C)=Sof(H55D)=1-FVAR(4)
 Sof(O13A)=Sof(C53A)=Sof(H53A)=Sof(H53B)=Sof(C54A)=Sof(H54A)=Sof(H54B)=
 Sof(C55A)=Sof(H55A)=Sof(H55B)=Sof(C56A)=Sof(H56A)=Sof(H56B)=FVAR(4)
5.a Secondary CH2 refined with riding coordinates:
 C53A(H53A,H53B), C54A(H54A,H54B), C55A(H55A,H55B), C56A(H56A,H56B), C9B(H9BA,
 H9BB), C10B(H10A,H10B), C11B(H11A,H11B), C12B(H12A,H12B), C13B(H13A,H13B),
 C14B(H14A,H14B), C15B(H15A,H15B), C16B(H16A,H16B), C17B(H17A,H17B), C18B(H18A,
 H18B), C19B(H19A,H19B), C20B(H20A,H20B), C21B(H21A,H21B), C22B(H22A,H22B),
 C23B(H23A,H23B), C24B(H24A,H24B), C25B(H25A,H25B), C26B(H26A,H26B), C9A(H9AA,
 H9AB), C10A(H10C,H10D), C11A(H11C,H11D), C12A(H12C,H12D), C13A(H13C,H13D),
 C14A(H14C,H14D), C15A(H15C,H15D), C16A(H16C,H16D), C17A(H17C,H17D), C18A(H18C,
 H18D), C19A(H19C,H19D), C20A(H20C,H20D), C21A(H21C,H21D), C22A(H22C,H22D),
 C23A(H23C,H23D), C24A(H24C,H24D), C25A(H25C,H25D), C26A(H26C,H26D), C35A(H35A,
 H35B), C36A(H36A,H36B), C37A(H37A,H37B), C38A(H38A,H38B), C39A(H39A,H39B),
 C40A(H40A,H40B), C41A(H41A,H41B), C42A(H42A,H42B), C43A(H43A,H43B), C44A(H44A,
 H44B), C45A(H45A,H45B), C46A(H46A,H46B), C47A(H47A,H47B), C48A(H48A,H48B),
 C49A(H49A,H49B), C50A(H50A,H50B), C51A(H51A,H51B), C52A(H52A,H52B), C35B(H35C,
 H35D), C36B(H36C,H36D), C37B(H37C,H37D), C38B(H38C,H38D), C39B(H39C,H39D),
 C40B(H40C,H40D), C41B(H41C,H41D), C42B(H42C,H42D), C43B(H43C,H43D), C44B(H44C,
 H44D), C45B(H45C,H45D), C46B(H46C,H46D), C47B(H47C,H47D), C48B(H48C,H48D),
 C49B(H49C,H49D), C50B(H50C,H50D), C51B(H51C,H51D), C52B(H52C,H52D), C53B(H53C,
 H53D), C56B(H56C,H56D), C54B(H54C,H54D), C55B(H55C,H55D)
5.b Me refined with riding coordinates:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C31A(H31A,
 H31B,H31C), C32A(H32A,H32B,H32C), C33A(H33A,H33B,H33C), C34A(H34A,H34B,H34C),
 C31B(H31D,H31E,H31F), C32B(H32D,H32E,H32F), C33B(H33D,H33E,H33F), C34B(H34D,
 H34E,H34F)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.32797(7) 0.78267(6) 0.36179(5) 0.0239(2) Uani 1 1 d . . . . .
C1 C 0.3529(2) 0.6614(2) 0.4005(2) 0.0236(7) Uani 1 1 d . . . . .
C2 C 0.3544(2) 0.6323(2) 0.3382(2) 0.0268(8) Uani 1 1 d . . . . .
C3 C 0.3351(3) 0.7055(2) 0.2596(2) 0.0275(8) Uani 1 1 d . . . . .
C4 C 0.3179(3) 0.7926(2) 0.2610(2) 0.0268(8) Uani 1 1 d . . . . .
C5 C 0.3676(3) 0.5980(2) 0.4916(2) 0.0363(9) Uani 1 1 d . . . . .
H5A H 0.363228 0.635258 0.523118 0.054 Uiso 1 1 calc R . . . .
H5B H 0.312207 0.551960 0.512840 0.054 Uiso 1 1 calc R . . . .
H5C H 0.436830 0.565626 0.497651 0.054 Uiso 1 1 calc R . . . .
C6 C 0.3791(3) 0.5325(2) 0.3516(2) 0.0384(9) Uani 1 1 d . . . . .
H6A H 0.375576 0.528247 0.298845 0.058 Uiso 1 1 calc R . . . .
H6B H 0.450171 0.513409 0.372064 0.058 Uiso 1 1 calc R . . . .
H6C H 0.327590 0.491243 0.392615 0.058 Uiso 1 1 calc R . . . .
C7 C 0.3373(3) 0.6956(3) 0.1781(2) 0.0483(11) Uani 1 1 d . . . . .
H7A H 0.350252 0.629956 0.189674 0.072 Uiso 1 1 calc R . . . .
H7B H 0.269407 0.717671 0.152492 0.072 Uiso 1 1 calc R . . . .
H7C H 0.393796 0.733014 0.140064 0.072 Uiso 1 1 calc R . . . .
C8 C 0.2899(3) 0.8829(3) 0.1870(2) 0.0374(9) Uani 1 1 d . . . . .
H8A H 0.282089 0.933692 0.204112 0.056 Uiso 1 1 calc R . . . .
H8B H 0.346149 0.896970 0.143111 0.056 Uiso 1 1 calc R . . . .
H8C H 0.223435 0.876567 0.165942 0.056 Uiso 1 1 calc R . . . .
O13A O 0.8052(3) 0.5983(2) 0.22867(19) 0.0489(9) Uani 0.835(4) 1 d D U P A 1
C53A C 0.7909(4) 0.5088(3) 0.2949(3) 0.0444(11) Uani 0.835(4) 1 d D U P A 1
H53A H 0.782804 0.513370 0.348525 0.053 Uiso 0.835(4) 1 calc R . P A 1
H53B H 0.853158 0.467544 0.296699 0.053 Uiso 0.835(4) 1 calc R . P A 1
C54A C 0.6921(4) 0.4687(3) 0.2814(3) 0.0408(10) Uani 0.835(4) 1 d D U P A 1
H54A H 0.629189 0.480871 0.311752 0.049 Uiso 0.835(4) 1 calc R . P A 1
H54B H 0.701124 0.400687 0.298507 0.049 Uiso 0.835(4) 1 calc R . P A 1
C55A C 0.6842(5) 0.5248(4) 0.1841(5) 0.0482(11) Uani 0.835(4) 1 d D U P A 1
H55A H 0.685311 0.482356 0.156851 0.058 Uiso 0.835(4) 1 calc R . P A 1
H55B H 0.619723 0.565623 0.169773 0.058 Uiso 0.835(4) 1 calc R . P A 1
C56A C 0.7838(4) 0.5816(3) 0.1602(3) 0.0426(10) Uani 0.835(4) 1 d D U P A 1
H56A H 0.843749 0.546568 0.147174 0.051 Uiso 0.835(4) 1 calc R . P A 1
H56B H 0.772639 0.641435 0.110487 0.051 Uiso 0.835(4) 1 calc R . P A 1
K1B K 0.6358(16) 0.1923(15) 0.2698(10) 0.026(3) Uani 0.090(4) 1 d . U P B 2
O1B O 0.445(2) 0.308(2) 0.268(2) 0.0293(19) Uani 0.090(4) 1 d . U P B 2
O2B O 0.571(3) 0.218(3) 0.406(3) 0.0298(17) Uani 0.090(4) 1 d . U P B 2
O3B O 0.618(4) -0.010(3) 0.363(2) 0.0229(19) Uani 0.090(4) 1 d . U P B 2
O4B O 0.541(5) 0.100(4) 0.188(3) 0.0234(19) Uani 0.090(4) 1 d . U P B 2
O5B O 0.740(3) 0.323(3) 0.132(2) 0.0272(19) Uani 0.090(4) 1 d . U P B 2
O6B O 0.856(3) 0.208(3) 0.280(3) 0.0273(19) Uani 0.090(4) 1 d . U P B 2
N1B N 0.533(3) 0.299(3) 0.104(2) 0.0268(17) Uani 0.090(4) 1 d . U P B 2
N2B N 0.744(5) 0.082(4) 0.422(4) 0.0277(16) Uani 0.090(4) 1 d . U P B 2
C9B C 0.419(3) 0.346(3) 0.121(3) 0.0254(17) Uani 0.090(4) 1 d . U P B 2
H9BA H 0.397218 0.399580 0.069208 0.030 Uiso 0.090(4) 1 calc R . P B 2
H9BB H 0.363222 0.299168 0.139218 0.030 Uiso 0.090(4) 1 calc R . P B 2
C10B C 0.429(3) 0.380(3) 0.190(3) 0.0280(19) Uani 0.090(4) 1 d . U P B 2
H10A H 0.489581 0.421929 0.174129 0.034 Uiso 0.090(4) 1 calc R . P B 2
H10B H 0.364789 0.416394 0.193731 0.034 Uiso 0.090(4) 1 calc R . P B 2
C11B C 0.440(3) 0.322(4) 0.336(3) 0.0295(19) Uani 0.090(4) 1 d . U P B 2
H11A H 0.366842 0.343076 0.343087 0.035 Uiso 0.090(4) 1 calc R . P B 2
H11B H 0.485591 0.374754 0.324025 0.035 Uiso 0.090(4) 1 calc R . P B 2
C12B C 0.470(3) 0.244(3) 0.421(3) 0.0301(19) Uani 0.090(4) 1 d . U P B 2
H12A H 0.466412 0.267720 0.464071 0.036 Uiso 0.090(4) 1 calc R . P B 2
H12B H 0.422242 0.190866 0.439701 0.036 Uiso 0.090(4) 1 calc R . P B 2
C13B C 0.601(4) 0.152(3) 0.481(3) 0.0282(19) Uani 0.090(4) 1 d . U P B 2
H13A H 0.556669 0.097303 0.498214 0.034 Uiso 0.090(4) 1 calc R . P B 2
H13B H 0.586274 0.177291 0.523005 0.034 Uiso 0.090(4) 1 calc R . P B 2
C14B C 0.709(4) 0.121(3) 0.485(3) 0.0282(19) Uani 0.090(4) 1 d . U P B 2
H14A H 0.720931 0.071928 0.541785 0.034 Uiso 0.090(4) 1 calc R . P B 2
H14B H 0.753577 0.173866 0.475036 0.034 Uiso 0.090(4) 1 calc R . P B 2
C15B C 0.725(4) -0.025(3) 0.455(3) 0.0281(19) Uani 0.090(4) 1 d . U P B 2
H15A H 0.785943 -0.058887 0.487841 0.034 Uiso 0.090(4) 1 calc R . P B 2
H15B H 0.662481 -0.038581 0.495119 0.034 Uiso 0.090(4) 1 calc R . P B 2
C16B C 0.708(4) -0.063(4) 0.400(3) 0.0258(19) Uani 0.090(4) 1 d . U P B 2
H16A H 0.768519 -0.053337 0.359224 0.031 Uiso 0.090(4) 1 calc R . P B 2
H16B H 0.693960 -0.130427 0.429918 0.031 Uiso 0.090(4) 1 calc R . P B 2
C17B C 0.586(5) -0.047(5) 0.315(4) 0.0241(18) Uani 0.090(4) 1 d . U P B 2
H17A H 0.558783 -0.108880 0.353695 0.029 Uiso 0.090(4) 1 calc R . P B 2
H17B H 0.650293 -0.059053 0.285909 0.029 Uiso 0.090(4) 1 calc R . P B 2
C18B C 0.512(4) -0.004(4) 0.256(3) 0.0225(19) Uani 0.090(4) 1 d . U P B 2
H18A H 0.443810 -0.000241 0.285245 0.027 Uiso 0.090(4) 1 calc R . P B 2
H18B H 0.503640 -0.042636 0.227033 0.027 Uiso 0.090(4) 1 calc R . P B 2
C19B C 0.459(4) 0.149(3) 0.134(3) 0.0245(19) Uani 0.090(4) 1 d . U P B 2
H19A H 0.396430 0.157551 0.166526 0.029 Uiso 0.090(4) 1 calc R . P B 2
H19B H 0.438783 0.112106 0.105174 0.029 Uiso 0.090(4) 1 calc R . P B 2
C20B C 0.501(4) 0.248(3) 0.068(3) 0.0265(17) Uani 0.090(4) 1 d . U P B 2
H20A H 0.560603 0.237896 0.033080 0.032 Uiso 0.090(4) 1 calc R . P B 2
H20B H 0.444012 0.282862 0.030473 0.032 Uiso 0.090(4) 1 calc R . P B 2
C21B C 0.651(4) 0.362(3) 0.019(3) 0.0277(18) Uani 0.090(4) 1 d . U P B 2
H21A H 0.660448 0.336726 -0.022445 0.033 Uiso 0.090(4) 1 calc R . P B 2
H21B H 0.637137 0.430169 -0.009381 0.033 Uiso 0.090(4) 1 calc R . P B 2
C22B C 0.737(4) 0.341(3) 0.066(3) 0.0276(18) Uani 0.090(4) 1 d . U P B 2
H22A H 0.774311 0.288715 0.058688 0.033 Uiso 0.090(4) 1 calc R . P B 2
H22B H 0.782456 0.395387 0.037355 0.033 Uiso 0.090(4) 1 calc R . P B 2
C23B C 0.870(4) 0.309(4) 0.141(3) 0.0262(18) Uani 0.090(4) 1 d . U P B 2
H23A H 0.897002 0.259999 0.124576 0.031 Uiso 0.090(4) 1 calc R . P B 2
H23B H 0.903916 0.368226 0.103230 0.031 Uiso 0.090(4) 1 calc R . P B 2
C24B C 0.895(4) 0.285(4) 0.223(3) 0.0266(17) Uani 0.090(4) 1 d . U P B 2
H24A H 0.972623 0.279638 0.224744 0.032 Uiso 0.090(4) 1 calc R . P B 2
H24B H 0.870469 0.336906 0.236607 0.032 Uiso 0.090(4) 1 calc R . P B 2
C25B C 0.877(4) 0.157(3) 0.351(3) 0.0273(19) Uani 0.090(4) 1 d . U P B 2
H25A H 0.857557 0.191818 0.384328 0.033 Uiso 0.090(4) 1 calc R . P B 2
H25B H 0.955178 0.148744 0.350731 0.033 Uiso 0.090(4) 1 calc R . P B 2
C26B C 0.841(5) 0.073(4) 0.394(4) 0.0277(19) Uani 0.090(4) 1 d . U P B 2
H26A H 0.840600 0.039872 0.358510 0.033 Uiso 0.090(4) 1 calc R . P B 2
H26B H 0.885381 0.036279 0.441438 0.033 Uiso 0.090(4) 1 calc R . P B 2
K1A K 0.62628(14) 0.19806(12) 0.24489(9) 0.0176(3) Uani 0.910(4) 1 d . U P B 1
O1A O 0.4521(2) 0.31413(19) 0.2248(2) 0.0253(6) Uani 0.910(4) 1 d . U P B 1
O2A O 0.5558(2) 0.2430(2) 0.37649(18) 0.0277(7) Uani 0.910(4) 1 d . U P B 1
O3A O 0.5983(3) 0.0058(2) 0.34343(19) 0.0230(8) Uani 0.910(4) 1 d . U P B 1
O4A O 0.5361(4) 0.0900(3) 0.1757(3) 0.0212(8) Uani 0.910(4) 1 d . U P B 1
O5A O 0.7456(3) 0.3282(3) 0.1054(2) 0.0260(8) Uani 0.910(4) 1 d . U P B 1
O6A O 0.8393(3) 0.2172(3) 0.2577(2) 0.0254(8) Uani 0.910(4) 1 d . U P B 1
N1A N 0.5313(3) 0.2953(2) 0.0750(2) 0.0243(7) Uani 0.910(4) 1 d . U P B 1
N2A N 0.7258(4) 0.0973(4) 0.4126(4) 0.0268(8) Uani 0.910(4) 1 d . U P B 1
C9A C 0.4287(3) 0.3380(3) 0.0860(3) 0.0277(8) Uani 0.910(4) 1 d . U P B 1
H9AA H 0.375329 0.289250 0.108003 0.033 Uiso 0.910(4) 1 calc R . P B 1
H9AB H 0.406932 0.385324 0.030996 0.033 Uiso 0.910(4) 1 calc R . P B 1
C10A C 0.4296(3) 0.3838(3) 0.1438(3) 0.0271(8) Uani 0.910(4) 1 d . U P B 1
H10C H 0.484038 0.431612 0.123666 0.033 Uiso 0.910(4) 1 calc R . P B 1
H10D H 0.360180 0.414779 0.145680 0.033 Uiso 0.910(4) 1 calc R . P B 1
C11A C 0.4322(3) 0.3503(3) 0.2852(3) 0.0290(8) Uani 0.910(4) 1 d . U P B 1
H11C H 0.359005 0.376469 0.281971 0.035 Uiso 0.910(4) 1 calc R . P B 1
H11D H 0.480957 0.401066 0.273619 0.035 Uiso 0.910(4) 1 calc R . P B 1
C12A C 0.4477(3) 0.2737(3) 0.3705(3) 0.0307(8) Uani 0.910(4) 1 d . U P B 1
H12C H 0.427426 0.296722 0.412918 0.037 Uiso 0.910(4) 1 calc R . P B 1
H12D H 0.402469 0.221031 0.380683 0.037 Uiso 0.910(4) 1 calc R . P B 1
C13A C 0.5768(3) 0.1772(3) 0.4580(3) 0.0286(8) Uani 0.910(4) 1 d . U P B 1
H13C H 0.534273 0.121514 0.473919 0.034 Uiso 0.910(4) 1 calc R . P B 1
H13D H 0.557298 0.204590 0.497460 0.034 Uiso 0.910(4) 1 calc R . P B 1
C14A C 0.6933(4) 0.1493(3) 0.4619(3) 0.0297(9) Uani 0.910(4) 1 d . U P B 1
H14C H 0.734952 0.206264 0.441317 0.036 Uiso 0.910(4) 1 calc R . P B 1
H14D H 0.709504 0.110236 0.520702 0.036 Uiso 0.910(4) 1 calc R . P B 1
C15A C 0.6916(4) -0.0001(3) 0.4572(3) 0.0287(9) Uani 0.910(4) 1 d . U P B 1
H15C H 0.623706 -0.001079 0.488421 0.034 Uiso 0.910(4) 1 calc R . P B 1
H15D H 0.744382 -0.037370 0.498020 0.034 Uiso 0.910(4) 1 calc R . P B 1
C16A C 0.6786(4) -0.0446(3) 0.3999(3) 0.0264(9) Uani 0.910(4) 1 d . U P B 1
H16C H 0.746072 -0.044060 0.368293 0.032 Uiso 0.910(4) 1 calc R . P B 1
H16D H 0.658670 -0.110304 0.432796 0.032 Uiso 0.910(4) 1 calc R . P B 1
C17A C 0.5665(4) -0.0462(4) 0.3010(3) 0.0237(10) Uani 0.910(4) 1 d . U P B 1
H17C H 0.535499 -0.105335 0.341738 0.028 Uiso 0.910(4) 1 calc R . P B 1
H17D H 0.628699 -0.061446 0.271874 0.028 Uiso 0.910(4) 1 calc R . P B 1
C18A C 0.4865(3) 0.0113(3) 0.2391(3) 0.0249(9) Uani 0.910(4) 1 d . U P B 1
H18C H 0.457604 -0.026677 0.214510 0.030 Uiso 0.910(4) 1 calc R . P B 1
H18D H 0.427503 0.031811 0.267255 0.030 Uiso 0.910(4) 1 calc R . P B 1
C19A C 0.4678(3) 0.1370(3) 0.1090(2) 0.0247(8) Uani 0.910(4) 1 d . U P B 1
H19C H 0.399488 0.153377 0.130584 0.030 Uiso 0.910(4) 1 calc R . P B 1
H19D H 0.454106 0.095392 0.083133 0.030 Uiso 0.910(4) 1 calc R . P B 1
C20A C 0.5184(3) 0.2246(3) 0.0448(3) 0.0271(8) Uani 0.910(4) 1 d . U P B 1
H20C H 0.588556 0.207530 0.026473 0.032 Uiso 0.910(4) 1 calc R . P B 1
H20D H 0.474644 0.252196 -0.004341 0.032 Uiso 0.910(4) 1 calc R . P B 1
C21A C 0.5999(4) 0.3685(3) 0.0172(3) 0.0296(9) Uani 0.910(4) 1 d . U P B 1
H21C H 0.586291 0.425026 0.026691 0.036 Uiso 0.910(4) 1 calc R . P B 1
H21D H 0.581660 0.384471 -0.040362 0.036 Uiso 0.910(4) 1 calc R . P B 1
C22A C 0.7172(3) 0.3416(3) 0.0255(3) 0.0279(8) Uani 0.910(4) 1 d . U P B 1
H22C H 0.731782 0.283355 0.018885 0.033 Uiso 0.910(4) 1 calc R . P B 1
H22D H 0.759118 0.391554 -0.018431 0.033 Uiso 0.910(4) 1 calc R . P B 1
C23A C 0.8565(3) 0.3187(3) 0.1119(3) 0.0270(9) Uani 0.910(4) 1 d . U P B 1
H23C H 0.890108 0.375696 0.069695 0.032 Uiso 0.910(4) 1 calc R . P B 1
H23D H 0.884064 0.265106 0.101376 0.032 Uiso 0.910(4) 1 calc R . P B 1
C24A C 0.8827(4) 0.3035(3) 0.1969(3) 0.0298(10) Uani 0.910(4) 1 d . U P B 1
H24C H 0.960279 0.300807 0.200453 0.036 Uiso 0.910(4) 1 calc R . P B 1
H24D H 0.853165 0.355995 0.208204 0.036 Uiso 0.910(4) 1 calc R . P B 1
C25A C 0.8857(4) 0.1905(3) 0.3365(3) 0.0269(9) Uani 0.910(4) 1 d . U P B 1
H25C H 0.868029 0.238465 0.356973 0.032 Uiso 0.910(4) 1 calc R . P B 1
H25D H 0.963477 0.185029 0.329726 0.032 Uiso 0.910(4) 1 calc R . P B 1
C26A C 0.8426(4) 0.0976(3) 0.3981(3) 0.0292(10) Uani 0.910(4) 1 d . U P B 1
H26C H 0.864360 0.050098 0.377793 0.035 Uiso 0.910(4) 1 calc R . P B 1
H26D H 0.875012 0.078696 0.451951 0.035 Uiso 0.910(4) 1 calc R . P B 1
K2A K 0.86543(16) -0.19727(14) 0.23357(9) 0.0185(3) Uani 0.881(4) 1 d . U P C 1
O7A O 0.8802(3) 0.0043(2) 0.1491(2) 0.0202(7) Uani 0.881(4) 1 d . U P C 1
O8A O 0.9596(5) -0.0953(4) 0.3123(3) 0.0225(9) Uani 0.881(4) 1 d . U P C 1
O9A O 0.7544(3) -0.3255(3) 0.37700(19) 0.0210(8) Uani 0.881(4) 1 d . U P C 1
O10A O 0.6474(3) -0.2044(3) 0.2322(3) 0.0179(7) Uani 0.881(4) 1 d . U P C 1
O11A O 0.9262(2) -0.2131(2) 0.0871(2) 0.0244(7) Uani 0.881(4) 1 d . U P C 1
O12A O 1.0485(2) -0.30072(19) 0.2307(2) 0.0246(6) Uani 0.881(4) 1 d . U P C 1
N3A N 0.7514(3) -0.0778(3) 0.0708(2) 0.0212(7) Uani 0.881(4) 1 d . U P C 1
N4A N 0.9790(3) -0.3026(2) 0.3937(2) 0.0224(7) Uani 0.881(4) 1 d . U P C 1
C35A C 0.7810(3) 0.0208(3) 0.0351(3) 0.0237(8) Uani 0.881(4) 1 d . U P C 1
H35A H 0.725621 0.060237 -0.001929 0.028 Uiso 0.881(4) 1 calc R . P C 1
H35B H 0.847620 0.028333 0.000650 0.028 Uiso 0.881(4) 1 calc R . P C 1
C36A C 0.7952(3) 0.0541(3) 0.0991(3) 0.0224(9) Uani 0.881(4) 1 d . U P C 1
H36A H 0.809421 0.121589 0.071524 0.027 Uiso 0.881(4) 1 calc R . P C 1
H36B H 0.729526 0.045431 0.134713 0.027 Uiso 0.881(4) 1 calc R . P C 1
C37A C 0.9091(3) 0.0486(3) 0.1978(3) 0.0212(9) Uani 0.881(4) 1 d . U P C 1
H37A H 0.847904 0.052395 0.233953 0.025 Uiso 0.881(4) 1 calc R . P C 1
H37B H 0.931154 0.112826 0.161036 0.025 Uiso 0.881(4) 1 calc R . P C 1
C38A C 0.9979(5) -0.0061(3) 0.2501(3) 0.0237(9) Uani 0.881(4) 1 d . U P C 1
H38A H 1.055841 -0.016523 0.214660 0.028 Uiso 0.881(4) 1 calc R . P C 1
H38B H 1.025499 0.029050 0.277917 0.028 Uiso 0.881(4) 1 calc R . P C 1
C39A C 1.0413(3) -0.1457(3) 0.3665(3) 0.0265(8) Uani 0.881(4) 1 d . U P C 1
H39A H 1.063581 -0.109301 0.395069 0.032 Uiso 0.881(4) 1 calc R . P C 1
H39B H 1.103180 -0.155571 0.333858 0.032 Uiso 0.881(4) 1 calc R . P C 1
C40A C 1.0016(3) -0.2389(3) 0.4302(3) 0.0269(8) Uani 0.881(4) 1 d . U P C 1
H40A H 1.055174 -0.269418 0.472182 0.032 Uiso 0.881(4) 1 calc R . P C 1
H40B H 0.936490 -0.228189 0.459238 0.032 Uiso 0.881(4) 1 calc R . P C 1
C41A C 0.9124(3) -0.3776(3) 0.4531(3) 0.0260(8) Uani 0.881(4) 1 d . U P C 1
H41A H 0.939353 -0.399959 0.509299 0.031 Uiso 0.881(4) 1 calc R . P C 1
H41B H 0.918444 -0.430487 0.437840 0.031 Uiso 0.881(4) 1 calc R . P C 1
C42A C 0.7965(4) -0.3484(3) 0.4562(3) 0.0257(9) Uani 0.881(4) 1 d . U P C 1
H42A H 0.757148 -0.400006 0.500685 0.031 Uiso 0.881(4) 1 calc R . P C 1
H42B H 0.789183 -0.293589 0.468734 0.031 Uiso 0.881(4) 1 calc R . P C 1
C43A C 0.6435(5) -0.3057(4) 0.3772(3) 0.0222(10) Uani 0.881(4) 1 d . U P C 1
H43A H 0.628290 -0.250266 0.388031 0.027 Uiso 0.881(4) 1 calc R . P C 1
H43B H 0.607277 -0.359271 0.422018 0.027 Uiso 0.881(4) 1 calc R . P C 1
C44A C 0.6032(3) -0.2878(3) 0.2943(2) 0.0202(8) Uani 0.881(4) 1 d . U P C 1
H44A H 0.623699 -0.340896 0.281009 0.024 Uiso 0.881(4) 1 calc R . P C 1
H44B H 0.525248 -0.281051 0.296338 0.024 Uiso 0.881(4) 1 calc R . P C 1
C45A C 0.6035(4) -0.1804(3) 0.1539(2) 0.0215(9) Uani 0.881(4) 1 d . U P C 1
H45A H 0.525547 -0.181411 0.160968 0.026 Uiso 0.881(4) 1 calc R . P C 1
H45B H 0.628151 -0.226508 0.132709 0.026 Uiso 0.881(4) 1 calc R . P C 1
C46A C 0.6365(3) -0.0855(4) 0.0933(3) 0.0228(9) Uani 0.881(4) 1 d . U P C 1
H46A H 0.598287 -0.066533 0.041907 0.027 Uiso 0.881(4) 1 calc R . P C 1
H46B H 0.614928 -0.041006 0.117055 0.027 Uiso 0.881(4) 1 calc R . P C 1
C47A C 0.7820(3) -0.1183(3) 0.0124(2) 0.0239(8) Uani 0.881(4) 1 d . U P C 1
H47A H 0.761107 -0.073983 -0.043914 0.029 Uiso 0.881(4) 1 calc R . P C 1
H47B H 0.743294 -0.176288 0.029203 0.029 Uiso 0.881(4) 1 calc R . P C 1
C48A C 0.8991(3) -0.1405(3) 0.0091(3) 0.0259(8) Uani 0.881(4) 1 d . U P C 1
H48A H 0.917271 -0.160536 -0.035611 0.031 Uiso 0.881(4) 1 calc R . P C 1
H48B H 0.939064 -0.084306 -0.003152 0.031 Uiso 0.881(4) 1 calc R . P C 1
C49A C 1.0318(3) -0.2461(3) 0.0856(3) 0.0276(8) Uani 0.881(4) 1 d . U P C 1
H49A H 1.080417 -0.196056 0.076610 0.033 Uiso 0.881(4) 1 calc R . P C 1
H49B H 1.044706 -0.263988 0.039138 0.033 Uiso 0.881(4) 1 calc R . P C 1
C50A C 1.0523(3) -0.3298(3) 0.1674(3) 0.0266(8) Uani 0.881(4) 1 d . U P C 1
H50A H 0.998369 -0.376827 0.179759 0.032 Uiso 0.881(4) 1 calc R . P C 1
H50B H 1.122514 -0.358824 0.163784 0.032 Uiso 0.881(4) 1 calc R . P C 1
C51A C 1.0691(3) -0.3784(3) 0.3092(3) 0.0267(8) Uani 0.881(4) 1 d . U P C 1
H51A H 1.135391 -0.412024 0.303950 0.032 Uiso 0.881(4) 1 calc R . P C 1
H51B H 1.010895 -0.422515 0.326472 0.032 Uiso 0.881(4) 1 calc R . P C 1
C52A C 1.0786(3) -0.3424(3) 0.3736(3) 0.0254(8) Uani 0.881(4) 1 d . U P C 1
H52A H 1.103696 -0.394285 0.425157 0.030 Uiso 0.881(4) 1 calc R . P C 1
H52B H 1.132360 -0.293993 0.352908 0.030 Uiso 0.881(4) 1 calc R . P C 1
P2A P 0.1706(2) 0.2113(2) 0.15971(15) 0.0208(4) Uani 0.816(7) 1 d . U P D 1
C27A C 0.1500(4) 0.3320(4) 0.1340(3) 0.0224(10) Uani 0.816(7) 1 d . U P D 1
C28A C 0.1480(3) 0.3476(4) 0.2051(4) 0.0212(9) Uani 0.816(7) 1 d . U P D 1
C29A C 0.1640(3) 0.2637(4) 0.2780(3) 0.0222(9) Uani 0.816(7) 1 d . U P D 1
C30A C 0.1785(4) 0.1854(4) 0.2654(3) 0.0210(9) Uani 0.816(7) 1 d . U P D 1
C31A C 0.1361(4) 0.4059(4) 0.0461(3) 0.0359(12) Uani 0.816(7) 1 d . U P D 1
H31A H 0.140887 0.376462 0.007881 0.054 Uiso 0.816(7) 1 calc R . P D 1
H31B H 0.066886 0.437613 0.043035 0.054 Uiso 0.816(7) 1 calc R . P D 1
H31C H 0.191564 0.451398 0.030300 0.054 Uiso 0.816(7) 1 calc R . P D 1
C32A C 0.1262(3) 0.4445(3) 0.2005(3) 0.0336(12) Uani 0.816(7) 1 d . U P D 1
H32A H 0.128063 0.441480 0.256310 0.050 Uiso 0.816(7) 1 calc R . P D 1
H32B H 0.180126 0.486582 0.163552 0.050 Uiso 0.816(7) 1 calc R . P D 1
H32C H 0.056476 0.467840 0.178812 0.050 Uiso 0.816(7) 1 calc R . P D 1
C33A C 0.1582(4) 0.2599(4) 0.3660(3) 0.0351(12) Uani 0.816(7) 1 d . U P D 1
H33A H 0.147450 0.323241 0.361730 0.053 Uiso 0.816(7) 1 calc R . P D 1
H33B H 0.099170 0.221755 0.399171 0.053 Uiso 0.816(7) 1 calc R . P D 1
H33C H 0.224212 0.232274 0.392982 0.053 Uiso 0.816(7) 1 calc R . P D 1
C34A C 0.2020(6) 0.0873(4) 0.3321(4) 0.0336(14) Uani 0.816(7) 1 d . U P D 1
H34A H 0.208993 0.043609 0.306790 0.050 Uiso 0.816(7) 1 calc R . P D 1
H34B H 0.267985 0.086459 0.357430 0.050 Uiso 0.816(7) 1 calc R . P D 1
H34C H 0.144204 0.068796 0.374942 0.050 Uiso 0.816(7) 1 calc R . P D 1
K2B K 0.8741(13) -0.1982(11) 0.2582(8) 0.023(2) Uani 0.119(4) 1 d . U P C 2
O7B O 0.906(2) -0.011(2) 0.158(2) 0.0222(18) Uani 0.119(4) 1 d . U P C 2
O8B O 0.958(5) -0.091(4) 0.328(3) 0.0238(19) Uani 0.119(4) 1 d . U P C 2
O9B O 0.763(3) -0.329(3) 0.399(2) 0.0232(19) Uani 0.119(4) 1 d . U P C 2
O10B O 0.670(3) -0.215(3) 0.244(2) 0.0202(18) Uani 0.119(4) 1 d . U P C 2
O11B O 0.9431(18) -0.2394(16) 0.1224(15) 0.0270(18) Uani 0.119(4) 1 d . U P C 2
O12B O 1.0483(17) -0.3171(17) 0.2748(16) 0.0277(18) Uani 0.119(4) 1 d . U P C 2
N3B N 0.778(2) -0.096(2) 0.087(2) 0.0228(16) Uani 0.119(4) 1 d . U P C 2
N4B N 0.971(2) -0.296(2) 0.4270(17) 0.0250(16) Uani 0.119(4) 1 d . U P C 2
C35B C 0.817(3) -0.001(2) 0.039(2) 0.0231(18) Uani 0.119(4) 1 d . U P C 2
H35C H 0.766424 0.038716 -0.002733 0.028 Uiso 0.119(4) 1 calc R . P C 2
H35D H 0.885973 -0.002593 0.010337 0.028 Uiso 0.119(4) 1 calc R . P C 2
C36B C 0.830(3) 0.043(3) 0.114(2) 0.0222(17) Uani 0.119(4) 1 d . U P C 2
H36C H 0.848969 0.109416 0.086935 0.027 Uiso 0.119(4) 1 calc R . P C 2
H36D H 0.763555 0.036721 0.148873 0.027 Uiso 0.119(4) 1 calc R . P C 2
C37B C 0.940(3) 0.036(3) 0.212(2) 0.0212(19) Uani 0.119(4) 1 d . U P C 2
H37C H 0.977553 0.094117 0.176382 0.025 Uiso 0.119(4) 1 calc R . P C 2
H37D H 0.876820 0.053193 0.239101 0.025 Uiso 0.119(4) 1 calc R . P C 2
C38B C 1.005(4) -0.025(3) 0.271(3) 0.0220(19) Uani 0.119(4) 1 d . U P C 2
H38C H 1.060030 -0.049597 0.243532 0.026 Uiso 0.119(4) 1 calc R . P C 2
H38D H 1.039926 0.010017 0.295806 0.026 Uiso 0.119(4) 1 calc R . P C 2
C39B C 1.030(3) -0.139(2) 0.399(2) 0.0262(19) Uani 0.119(4) 1 d . U P C 2
H39C H 1.041964 -0.097773 0.425325 0.031 Uiso 0.119(4) 1 calc R . P C 2
H39D H 1.099670 -0.155379 0.378224 0.031 Uiso 0.119(4) 1 calc R . P C 2
C40B C 0.975(3) -0.227(2) 0.460(2) 0.026(2) Uani 0.119(4) 1 d . U P C 2
H40C H 1.013047 -0.254876 0.512033 0.031 Uiso 0.119(4) 1 calc R . P C 2
H40D H 0.902500 -0.209319 0.473299 0.031 Uiso 0.119(4) 1 calc R . P C 2
C41B C 0.894(2) -0.364(2) 0.482(2) 0.0255(19) Uani 0.119(4) 1 d . U P C 2
H41C H 0.909318 -0.381312 0.540335 0.031 Uiso 0.119(4) 1 calc R . P C 2
H41D H 0.902924 -0.420609 0.472520 0.031 Uiso 0.119(4) 1 calc R . P C 2
C42B C 0.784(3) -0.3283(15) 0.4684(18) 0.0246(19) Uani 0.119(4) 1 d . U P C 2
H42C H 0.736514 -0.369233 0.514576 0.030 Uiso 0.119(4) 1 calc R . P C 2
H42D H 0.776747 -0.264287 0.464307 0.030 Uiso 0.119(4) 1 calc R . P C 2
C43B C 0.648(4) -0.322(3) 0.398(3) 0.0214(19) Uani 0.119(4) 1 d . U P C 2
H43C H 0.618705 -0.382836 0.435978 0.026 Uiso 0.119(4) 1 calc R . P C 2
H43D H 0.621299 -0.275407 0.418011 0.026 Uiso 0.119(4) 1 calc R . P C 2
C44B C 0.615(3) -0.297(2) 0.324(2) 0.0205(19) Uani 0.119(4) 1 d . U P C 2
H44C H 0.539474 -0.279448 0.325586 0.025 Uiso 0.119(4) 1 calc R . P C 2
H44D H 0.619981 -0.353664 0.313723 0.025 Uiso 0.119(4) 1 calc R . P C 2
C45B C 0.620(3) -0.198(3) 0.176(2) 0.0214(17) Uani 0.119(4) 1 d . U P C 2
H45C H 0.542938 -0.192638 0.186488 0.026 Uiso 0.119(4) 1 calc R . P C 2
H45D H 0.634842 -0.249212 0.159063 0.026 Uiso 0.119(4) 1 calc R . P C 2
C46B C 0.670(3) -0.086(3) 0.094(3) 0.0222(18) Uani 0.119(4) 1 d . U P C 2
H46C H 0.639829 -0.072301 0.039966 0.027 Uiso 0.119(4) 1 calc R . P C 2
H46D H 0.649741 -0.034324 0.108722 0.027 Uiso 0.119(4) 1 calc R . P C 2
C47B C 0.815(3) -0.148(2) 0.0371(19) 0.0244(17) Uani 0.119(4) 1 d . U P C 2
H47C H 0.768644 -0.201967 0.052970 0.029 Uiso 0.119(4) 1 calc R . P C 2
H47D H 0.805940 -0.106957 -0.022614 0.029 Uiso 0.119(4) 1 calc R . P C 2
C48B C 0.924(3) -0.183(3) 0.048(3) 0.0265(19) Uani 0.119(4) 1 d . U P C 2
H48C H 0.941127 -0.214868 0.011471 0.032 Uiso 0.119(4) 1 calc R . P C 2
H48D H 0.970040 -0.129164 0.028920 0.032 Uiso 0.119(4) 1 calc R . P C 2
C49B C 1.050(2) -0.279(3) 0.131(2) 0.0259(17) Uani 0.119(4) 1 d . U P C 2
H49C H 1.100328 -0.228380 0.117545 0.031 Uiso 0.119(4) 1 calc R . P C 2
H49D H 1.065565 -0.306360 0.091622 0.031 Uiso 0.119(4) 1 calc R . P C 2
C50B C 1.068(2) -0.356(2) 0.222(2) 0.0277(18) Uani 0.119(4) 1 d . U P C 2
H50C H 1.019808 -0.408097 0.236640 0.033 Uiso 0.119(4) 1 calc R . P C 2
H50D H 1.141461 -0.381604 0.226526 0.033 Uiso 0.119(4) 1 calc R . P C 2
C51B C 1.074(2) -0.379(2) 0.360(2) 0.0262(19) Uani 0.119(4) 1 d . U P C 2
H51C H 1.027182 -0.432908 0.381371 0.031 Uiso 0.119(4) 1 calc R . P C 2
H51D H 1.147419 -0.403951 0.359221 0.031 Uiso 0.119(4) 1 calc R . P C 2
C52B C 1.065(2) -0.338(2) 0.417(2) 0.0262(19) Uani 0.119(4) 1 d . U P C 2
H52C H 1.082812 -0.387999 0.472338 0.031 Uiso 0.119(4) 1 calc R . P C 2
H52D H 1.120429 -0.291495 0.399872 0.031 Uiso 0.119(4) 1 calc R . P C 2
P2B P 0.1654(12) 0.2192(10) 0.1369(7) 0.0279(17) Uani 0.184(7) 1 d . U P D 2
C27B C 0.144(2) 0.336(2) 0.1065(15) 0.0252(18) Uani 0.184(7) 1 d . U P D 2
C28B C 0.1410(18) 0.3590(17) 0.1702(16) 0.0251(18) Uani 0.184(7) 1 d . U P D 2
C29B C 0.1552(18) 0.298(2) 0.2484(17) 0.0252(16) Uani 0.184(7) 1 d . U P D 2
C30B C 0.176(2) 0.2004(18) 0.2357(14) 0.0254(17) Uani 0.184(7) 1 d . U P D 2
C31B C 0.126(2) 0.3963(17) 0.0119(15) 0.036(4) Uani 0.184(7) 1 d . U P D 2
H31D H 0.134748 0.356463 -0.017302 0.055 Uiso 0.184(7) 1 calc R . P D 2
H31E H 0.053939 0.423896 0.005638 0.055 Uiso 0.184(7) 1 calc R . P D 2
H31F H 0.176706 0.446057 -0.011899 0.055 Uiso 0.184(7) 1 calc R . P D 2
C32B C 0.1131(13) 0.4649(13) 0.1426(13) 0.025(3) Uani 0.184(7) 1 d . U P D 2
H32D H 0.106634 0.496079 0.082214 0.038 Uiso 0.184(7) 1 calc R . P D 2
H32E H 0.046143 0.471764 0.170598 0.038 Uiso 0.184(7) 1 calc R . P D 2
H32F H 0.169120 0.493162 0.157696 0.038 Uiso 0.184(7) 1 calc R . P D 2
C33B C 0.1602(19) 0.3017(17) 0.3297(14) 0.033(3) Uani 0.184(7) 1 d . U P D 2
H33D H 0.172244 0.238580 0.373665 0.049 Uiso 0.184(7) 1 calc R . P D 2
H33E H 0.218226 0.340945 0.326442 0.049 Uiso 0.184(7) 1 calc R . P D 2
H33F H 0.093506 0.328241 0.342445 0.049 Uiso 0.184(7) 1 calc R . P D 2
C34B C 0.205(3) 0.117(2) 0.3103(17) 0.028(4) Uani 0.184(7) 1 d . U P D 2
H34D H 0.215103 0.063573 0.296811 0.042 Uiso 0.184(7) 1 calc R . P D 2
H34E H 0.270218 0.127290 0.330072 0.042 Uiso 0.184(7) 1 calc R . P D 2
H34F H 0.148191 0.104241 0.353811 0.042 Uiso 0.184(7) 1 calc R . P D 2
C53B C 0.7136(15) 0.4305(19) 0.3139(10) 0.0495(19) Uani 0.165(4) 1 d D U P A 2
H53C H 0.710622 0.371906 0.365929 0.059 Uiso 0.165(4) 1 calc R . P A 2
H53D H 0.658123 0.473338 0.320995 0.059 Uiso 0.165(4) 1 calc R . P A 2
O13B O 0.6813(13) 0.4089(11) 0.2510(9) 0.054(2) Uani 0.165(4) 1 d D U P A 2
C56B C 0.696(2) 0.5032(15) 0.195(2) 0.0477(18) Uani 0.165(4) 1 d D U P A 2
H56C H 0.641163 0.544292 0.206082 0.057 Uiso 0.165(4) 1 calc R . P A 2
H56D H 0.694033 0.513118 0.136907 0.057 Uiso 0.165(4) 1 calc R . P A 2
C54B C 0.8189(17) 0.4731(18) 0.3111(13) 0.0482(19) Uani 0.165(4) 1 d D U P A 2
H54C H 0.879273 0.427638 0.329154 0.058 Uiso 0.165(4) 1 calc R . P A 2
H54D H 0.816374 0.516502 0.337385 0.058 Uiso 0.165(4) 1 calc R . P A 2
C55B C 0.8052(18) 0.5215(18) 0.2141(13) 0.0476(16) Uani 0.165(4) 1 d D U P A 2
H55C H 0.813912 0.589577 0.192230 0.057 Uiso 0.165(4) 1 calc R . P A 2
H55D H 0.860096 0.496659 0.186157 0.057 Uiso 0.165(4) 1 calc R . P A 2


_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
P1 C1 1.762(3) . ?
P1 C4 1.754(3) . ?
C1 C2 1.381(4) . ?
C1 C5 1.514(5) . ?
C2 C3 1.407(5) . ?
C2 C6 1.517(4) . ?
C3 C4 1.403(5) . ?
C3 C7 1.532(4) . ?
C4 C8 1.513(5) . ?
O13A C53A 1.413(4) . ?
O13A C56A 1.412(4) . ?
C53A C54A 1.528(5) . ?
C54A C55A 1.579(9) . ?
C55A C56A 1.528(5) . ?
K1B O1B 2.95(4) . ?
K1B O2B 2.71(4) . ?
K1B O3B 2.92(5) . ?
K1B O4B 2.85(5) . ?
K1B O5B 2.74(4) . ?
K1B O6B 2.85(5) . ?
K1B N1B 3.05(4) . ?
K1B N2B 2.91(6) . ?
O1B C10B 1.38(5) . ?
O1B C11B 1.33(5) . ?
O2B C12B 1.37(5) . ?
O2B C13B 1.36(5) . ?
O3B C16B 1.40(5) . ?
O3B C17B 1.33(7) . ?
O4B C18B 1.61(8) . ?
O4B C19B 1.42(7) . ?
O5B C22B 1.10(6) . ?
O5B C23B 1.67(6) . ?
O6B C24B 1.31(6) . ?
O6B C25B 1.21(6) . ?
N1B C9B 1.67(6) . ?
N1B C20B 1.34(5) . ?
N1B C21B 2.01(6) . ?
N2B C14B 1.54(8) . ?
N2B C15B 1.56(8) . ?
N2B C26B 1.31(9) . ?
C9B C10B 1.57(5) . ?
C11B C12B 1.54(6) . ?
C13B C14B 1.42(7) . ?
C15B C16B 1.41(7) . ?
C17B C18B 1.38(6) . ?
C19B C20B 1.61(6) . ?
C21B C22B 1.36(6) . ?
C23B C24B 1.39(6) . ?
C25B C26B 1.31(7) . ?
K1A O1A 2.734(3) . ?
K1A O2A 2.817(3) . ?
K1A O3A 2.819(4) . ?
K1A O4A 2.854(3) . ?
K1A O5A 2.854(4) . ?
K1A O6A 2.783(4) . ?
K1A N1A 3.049(3) . ?
K1A N2A 3.047(5) . ?
O1A C10A 1.424(5) . ?
O1A C11A 1.432(5) . ?
O2A C12A 1.426(5) . ?
O2A C13A 1.408(5) . ?
O3A C16A 1.431(5) . ?
O3A C17A 1.437(6) . ?
O4A C18A 1.417(7) . ?
O4A C19A 1.426(6) . ?
O5A C22A 1.422(5) . ?
O5A C23A 1.417(5) . ?
O6A C24A 1.442(6) . ?
O6A C25A 1.445(5) . ?
N1A C9A 1.473(5) . ?
N1A C20A 1.471(5) . ?
N1A C21A 1.460(5) . ?
N2A C14A 1.477(7) . ?
N2A C15A 1.479(7) . ?
N2A C26A 1.488(8) . ?
C9A C10A 1.505(5) . ?
C11A C12A 1.498(6) . ?
C13A C14A 1.517(6) . ?
C15A C16A 1.503(6) . ?
C17A C18A 1.505(5) . ?
C19A C20A 1.512(5) . ?
C21A C22A 1.525(5) . ?
C23A C24A 1.492(6) . ?
C25A C26A 1.515(6) . ?
K2A O7A 2.905(4) . ?
K2A O8A 2.927(5) . ?
K2A O9A 2.827(4) . ?
K2A O10A 2.785(4) . ?
K2A O11A 2.788(3) . ?
K2A O12A 2.777(3) . ?
K2A N3A 3.106(3) . ?
K2A N4A 3.037(3) . ?
O7A C36A 1.420(4) . ?
O7A C37A 1.419(6) . ?
O8A C38A 1.456(8) . ?
O8A C39A 1.425(7) . ?
O9A C42A 1.438(5) . ?
O9A C43A 1.426(7) . ?
O10A C44A 1.425(6) . ?
O10A C45A 1.429(5) . ?
O11A C48A 1.420(4) . ?
O11A C49A 1.413(5) . ?
O12A C50A 1.395(5) . ?
O12A C51A 1.439(5) . ?
N3A C35A 1.477(6) . ?
N3A C46A 1.484(5) . ?
N3A C47A 1.469(5) . ?
N4A C40A 1.478(5) . ?
N4A C41A 1.469(5) . ?
N4A C52A 1.472(5) . ?
C35A C36A 1.484(6) . ?
C37A C38A 1.493(5) . ?
C39A C40A 1.514(5) . ?
C41A C42A 1.521(6) . ?
C43A C44A 1.506(6) . ?
C45A C46A 1.489(7) . ?
C47A C48A 1.511(5) . ?
C49A C50A 1.516(6) . ?
C51A C52A 1.509(5) . ?
P2A C27A 1.779(6) . ?
P2A C30A 1.760(4) . ?
C27A C28A 1.398(6) . ?
C27A C31A 1.512(6) . ?
C28A C29A 1.417(6) . ?
C28A C32A 1.519(6) . ?
C29A C30A 1.362(7) . ?
C29A C33A 1.546(6) . ?
C30A C34A 1.524(6) . ?
K2B O7B 2.77(4) . ?
K2B O8B 2.81(5) . ?
K2B O9B 2.81(4) . ?
K2B O10B 2.68(4) . ?
K2B O11B 2.85(3) . ?
K2B O12B 2.77(3) . ?
K2B N3B 3.08(3) . ?
K2B N4B 3.04(3) . ?
O7B C36B 1.31(4) . ?
O7B C37B 1.57(5) . ?
O8B C38B 1.25(7) . ?
O8B C39B 1.51(6) . ?
O9B C42B 1.30(5) . ?
O9B C43B 1.47(6) . ?
O10B C44B 1.60(5) . ?
O10B C45B 1.32(4) . ?
O11B C48B 1.28(4) . ?
O11B C49B 1.45(4) . ?
O12B C50B 1.34(4) . ?
O12B C51B 1.46(4) . ?
N3B C35B 1.47(5) . ?
N3B C46B 1.37(4) . ?
N3B C47B 1.51(5) . ?
N4B C40B 1.46(4) . ?
N4B C41B 1.46(4) . ?
N4B C52B 1.39(4) . ?
C35B C36B 1.78(5) . ?
C37B C38B 1.37(4) . ?
C39B C40B 1.52(4) . ?
C41B C42B 1.47(5) . ?
C43B C44B 1.30(5) . ?
C45B C46B 1.86(6) . ?
C47B C48B 1.45(5) . ?
C49B C50B 1.58(4) . ?
C51B C52B 1.42(4) . ?
P2B C27B 1.71(3) . ?
P2B C30B 1.67(2) . ?
C27B C28B 1.34(3) . ?
C27B C31B 1.57(3) . ?
C28B C29B 1.33(3) . ?
C28B C32B 1.56(3) . ?
C29B C30B 1.66(4) . ?
C29B C33B 1.49(3) . ?
C30B C34B 1.47(3) . ?
C53B O13B 1.409(6) . ?
C53B C54B 1.528(6) . ?
O13B C56B 1.410(6) . ?
C56B C55B 1.529(6) . ?
C54B C55B 1.580(10) . ?

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
C4 P1 C1 91.00(15) . . ?
C2 C1 P1 111.6(2) . . ?
C2 C1 C5 125.1(3) . . ?
C5 C1 P1 123.3(2) . . ?
C1 C2 C3 113.2(3) . . ?
C1 C2 C6 123.8(3) . . ?
C3 C2 C6 123.0(3) . . ?
C2 C3 C7 125.1(3) . . ?
C4 C3 C2 113.4(3) . . ?
C4 C3 C7 121.4(3) . . ?
C3 C4 P1 110.8(2) . . ?
C3 C4 C8 125.3(3) . . ?
C8 C4 P1 123.9(2) . . ?
C56A O13A C53A 100.9(4) . . ?
O13A C53A C54A 108.5(4) . . ?
C53A C54A C55A 101.2(4) . . ?
C56A C55A C54A 101.3(4) . . ?
O13A C56A C55A 107.4(4) . . ?
O1B K1B N1B 62.8(11) . . ?
O2B K1B O1B 59.8(11) . . ?
O2B K1B O3B 91.4(13) . . ?
O2B K1B O4B 131.2(17) . . ?
O2B K1B O5B 123.8(15) . . ?
O2B K1B O6B 96.5(13) . . ?
O2B K1B N1B 122.1(13) . . ?
O2B K1B N2B 62.8(16) . . ?
O3B K1B O1B 116.9(13) . . ?
O3B K1B N1B 121.0(13) . . ?
O4B K1B O1B 93.5(15) . . ?
O4B K1B O3B 63.5(15) . . ?
O4B K1B O6B 127.2(18) . . ?
O4B K1B N1B 57.8(14) . . ?
O4B K1B N2B 119(2) . . ?
O5B K1B O1B 97.2(12) . . ?
O5B K1B O3B 140.9(15) . . ?
O5B K1B O4B 97.7(16) . . ?
O5B K1B O6B 63.1(13) . . ?
O5B K1B N1B 57.3(13) . . ?
O5B K1B N2B 121.1(18) . . ?
O6B K1B O1B 135.0(14) . . ?
O6B K1B O3B 99.8(14) . . ?
O6B K1B N1B 119.8(14) . . ?
O6B K1B N2B 58.1(16) . . ?
N2B K1B O1B 122.0(16) . . ?
N2B K1B O3B 56.9(17) . . ?
N2B K1B N1B 175.2(18) . . ?
C10B O1B K1B 113(2) . . ?
C11B O1B K1B 108(3) . . ?
C11B O1B C10B 122(4) . . ?
C12B O2B K1B 124(3) . . ?
C13B O2B K1B 118(3) . . ?
C13B O2B C12B 105(4) . . ?
C16B O3B K1B 118(3) . . ?
C17B O3B K1B 111(3) . . ?
C17B O3B C16B 106(4) . . ?
C18B O4B K1B 108(3) . . ?
C19B O4B K1B 118(3) . . ?
C19B O4B C18B 115(4) . . ?
C22B O5B K1B 132(5) . . ?
C22B O5B C23B 99(4) . . ?
C23B O5B K1B 111(2) . . ?
C24B O6B K1B 114(3) . . ?
C25B O6B K1B 107(4) . . ?
C25B O6B C24B 134(5) . . ?
C9B N1B K1B 108(2) . . ?
C9B N1B C21B 128(3) . . ?
C20B N1B K1B 116(3) . . ?
C20B N1B C9B 101(3) . . ?
C20B N1B C21B 97(3) . . ?
C21B N1B K1B 106(2) . . ?
C14B N2B K1B 108(3) . . ?
C14B N2B C15B 113(5) . . ?
C15B N2B K1B 112(4) . . ?
C26B N2B K1B 103(4) . . ?
C26B N2B C14B 128(6) . . ?
C26B N2B C15B 93(4) . . ?
C10B C9B N1B 110(3) . . ?
O1B C10B C9B 113(4) . . ?
O1B C11B C12B 122(4) . . ?
O2B C12B C11B 103(3) . . ?
O2B C13B C14B 116(4) . . ?
C13B C14B N2B 114(4) . . ?
C16B C15B N2B 120(5) . . ?
O3B C16B C15B 99(4) . . ?
O3B C17B C18B 123(6) . . ?
C17B C18B O4B 115(5) . . ?
O4B C19B C20B 109(4) . . ?
N1B C20B C19B 113(4) . . ?
C22B C21B N1B 103(3) . . ?
O5B C22B C21B 129(5) . . ?
C24B C23B O5B 111(4) . . ?
O6B C24B C23B 117(5) . . ?
O6B C25B K1B 53(3) . . ?
O6B C25B C26B 124(6) . . ?
C26B C25B K1B 81(4) . . ?
N2B C26B K1B 55(4) . . ?
N2B C26B C25B 108(5) . . ?
C25B C26B K1B 77(3) . . ?
O1A K1A O2A 61.45(9) . . ?
O1A K1A O3A 117.02(11) . . ?
O1A K1A O4A 94.31(12) . . ?
O1A K1A O5A 95.22(10) . . ?
O1A K1A O6A 133.27(12) . . ?
O1A K1A N1A 60.43(9) . . ?
O1A K1A N2A 121.35(13) . . ?
O2A K1A O3A 92.54(10) . . ?
O2A K1A O4A 131.76(14) . . ?
O2A K1A O5A 119.91(11) . . ?
O2A K1A N1A 121.38(10) . . ?
O2A K1A N2A 60.41(12) . . ?
O3A K1A O4A 60.34(12) . . ?
O3A K1A O5A 143.08(12) . . ?
O3A K1A N1A 119.94(11) . . ?
O3A K1A N2A 59.36(13) . . ?
O4A K1A N1A 60.22(12) . . ?
O4A K1A N2A 118.80(16) . . ?
O5A K1A O4A 102.15(13) . . ?
O5A K1A N1A 59.70(10) . . ?
O5A K1A N2A 119.69(15) . . ?
O6A K1A O2A 95.21(10) . . ?
O6A K1A O3A 102.89(11) . . ?
O6A K1A O4A 127.61(14) . . ?
O6A K1A O5A 60.14(11) . . ?
O6A K1A N1A 119.23(11) . . ?
O6A K1A N2A 59.92(13) . . ?
N2A K1A N1A 178.21(14) . . ?
C10A O1A K1A 119.5(2) . . ?
C10A O1A C11A 110.6(3) . . ?
C11A O1A K1A 116.4(2) . . ?
C12A O2A K1A 111.5(2) . . ?
C13A O2A K1A 117.7(2) . . ?
C13A O2A C12A 111.3(3) . . ?
C16A O3A K1A 117.0(3) . . ?
C16A O3A C17A 111.0(3) . . ?
C17A O3A K1A 116.2(3) . . ?
C18A O4A K1A 110.7(2) . . ?
C18A O4A C19A 110.2(4) . . ?
C19A O4A K1A 117.9(3) . . ?
C22A O5A K1A 116.4(2) . . ?
C23A O5A K1A 115.2(2) . . ?
C23A O5A C22A 111.5(3) . . ?
C24A O6A K1A 115.0(2) . . ?
C24A O6A C25A 109.4(3) . . ?
C25A O6A K1A 122.8(3) . . ?
C9A N1A K1A 107.6(2) . . ?
C20A N1A K1A 108.0(2) . . ?
C20A N1A C9A 111.1(3) . . ?
C21A N1A K1A 110.2(2) . . ?
C21A N1A C9A 109.0(3) . . ?
C21A N1A C20A 110.8(3) . . ?
C14A N2A K1A 107.6(2) . . ?
C14A N2A C15A 110.1(5) . . ?
C14A N2A C26A 109.9(5) . . ?
C15A N2A K1A 111.3(3) . . ?
C15A N2A C26A 109.4(3) . . ?
C26A N2A K1A 108.6(4) . . ?
N1A C9A C10A 113.7(3) . . ?
O1A C10A C9A 108.8(3) . . ?
O1A C11A C12A 109.5(3) . . ?
O2A C12A C11A 109.0(3) . . ?
O2A C13A C14A 109.4(4) . . ?
N2A C14A C13A 113.1(4) . . ?
N2A C15A C16A 112.9(4) . . ?
O3A C16A C15A 109.5(3) . . ?
O3A C17A C18A 109.3(4) . . ?
O4A C18A C17A 108.9(4) . . ?
O4A C19A C20A 109.6(3) . . ?
N1A C20A C19A 113.8(3) . . ?
N1A C21A C22A 113.8(3) . . ?
O5A C22A C21A 108.7(3) . . ?
O5A C23A C24A 109.7(4) . . ?
O6A C24A C23A 109.4(4) . . ?
O6A C25A C26A 108.4(3) . . ?
N2A C26A C25A 114.7(4) . . ?
O7A K2A O8A 59.02(14) . . ?
O7A K2A N3A 58.24(11) . . ?
O7A K2A N4A 118.18(11) . . ?
O8A K2A N3A 116.55(15) . . ?
O8A K2A N4A 59.78(14) . . ?
O9A K2A O7A 135.69(14) . . ?
O9A K2A O8A 97.34(13) . . ?
O9A K2A N3A 121.08(12) . . ?
O9A K2A N4A 60.41(9) . . ?
O10A K2A O7A 97.56(12) . . ?
O10A K2A O8A 121.22(18) . . ?
O10A K2A O9A 61.02(11) . . ?
O10A K2A O11A 99.86(12) . . ?
O10A K2A N3A 60.28(11) . . ?
O10A K2A N4A 120.76(12) . . ?
O11A K2A O7A 91.35(11) . . ?
O11A K2A O8A 130.36(15) . . ?
O11A K2A O9A 128.34(12) . . ?
O11A K2A N3A 59.44(10) . . ?
O11A K2A N4A 122.78(11) . . ?
O12A K2A O7A 116.31(11) . . ?
O12A K2A O8A 94.63(15) . . ?
O12A K2A O9A 101.40(12) . . ?
O12A K2A O10A 140.49(14) . . ?
O12A K2A O11A 61.75(9) . . ?
O12A K2A N3A 120.52(11) . . ?
O12A K2A N4A 61.29(9) . . ?
N4A K2A N3A 176.31(12) . . ?
C36A O7A K2A 116.1(3) . . ?
C37A O7A K2A 116.4(2) . . ?
C37A O7A C36A 110.9(3) . . ?
C38A O8A K2A 111.0(3) . . ?
C39A O8A K2A 114.8(3) . . ?
C39A O8A C38A 109.9(5) . . ?
C42A O9A K2A 117.4(3) . . ?
C43A O9A K2A 113.2(2) . . ?
C43A O9A C42A 112.3(3) . . ?
C44A O10A K2A 114.6(2) . . ?
C44A O10A C45A 110.2(4) . . ?
C45A O10A K2A 117.5(3) . . ?
C48A O11A K2A 120.0(2) . . ?
C49A O11A K2A 112.9(2) . . ?
C49A O11A C48A 112.1(3) . . ?
C50A O12A K2A 112.6(2) . . ?
C50A O12A C51A 110.5(3) . . ?
C51A O12A K2A 114.1(2) . . ?
C35A N3A K2A 111.2(2) . . ?
C35A N3A C46A 110.2(3) . . ?
C46A N3A K2A 106.6(3) . . ?
C47A N3A K2A 107.0(2) . . ?
C47A N3A C35A 110.6(3) . . ?
C47A N3A C46A 111.1(3) . . ?
C40A N4A K2A 110.5(2) . . ?
C41A N4A K2A 109.1(2) . . ?
C41A N4A C40A 109.7(3) . . ?
C41A N4A C52A 110.0(3) . . ?
C52A N4A K2A 107.9(2) . . ?
C52A N4A C40A 109.6(3) . . ?
N3A C35A C36A 113.2(3) . . ?
O7A C36A C35A 110.6(3) . . ?
O7A C37A C38A 109.4(4) . . ?
O8A C38A C37A 109.1(5) . . ?
O8A C39A C40A 109.6(4) . . ?
N4A C40A C39A 113.4(3) . . ?
N4A C41A C42A 113.8(3) . . ?
O9A C42A C41A 108.8(3) . . ?
O9A C43A C44A 109.8(4) . . ?
O10A C44A C43A 108.6(4) . . ?
O10A C45A C46A 109.5(4) . . ?
N3A C46A C45A 114.7(4) . . ?
N3A C47A C48A 112.8(3) . . ?
O11A C48A C47A 108.8(3) . . ?
O11A C49A C50A 109.5(3) . . ?
O12A C50A C49A 109.1(3) . . ?
O12A C51A C52A 108.9(3) . . ?
N4A C52A C51A 113.6(3) . . ?
C30A P2A C27A 90.7(2) . . ?
C28A C27A P2A 110.9(3) . . ?
C28A C27A C31A 125.9(5) . . ?
C31A C27A P2A 123.2(4) . . ?
C27A C28A C29A 112.0(4) . . ?
C27A C28A C32A 121.3(5) . . ?
C29A C28A C32A 126.6(4) . . ?
C28A C29A C33A 122.8(4) . . ?
C30A C29A C28A 115.0(4) . . ?
C30A C29A C33A 122.1(4) . . ?
C29A C30A P2A 111.4(3) . . ?
C29A C30A C34A 125.7(4) . . ?
C34A C30A P2A 122.9(4) . . ?
O7B K2B O8B 61.6(13) . . ?
O7B K2B O9B 146.0(12) . . ?
O7B K2B O11B 89.5(10) . . ?
O7B K2B N3B 58.1(10) . . ?
O7B K2B N4B 120.8(10) . . ?
O8B K2B O9B 100.4(13) . . ?
O8B K2B O11B 132.9(13) . . ?
O8B K2B N3B 118.4(13) . . ?
O8B K2B N4B 60.5(12) . . ?
O9B K2B O11B 120.9(10) . . ?
O9B K2B N3B 122.7(11) . . ?
O9B K2B N4B 58.0(9) . . ?
O10B K2B O7B 103.1(11) . . ?
O10B K2B O8B 126.7(16) . . ?
O10B K2B O9B 62.9(11) . . ?
O10B K2B O11B 94.1(11) . . ?
O10B K2B O12B 132.0(12) . . ?
O10B K2B N3B 60.2(10) . . ?
O10B K2B N4B 120.3(11) . . ?
O11B K2B N3B 58.3(8) . . ?
O11B K2B N4B 122.2(9) . . ?
O12B K2B O7B 115.8(10) . . ?
O12B K2B O8B 97.1(13) . . ?
O12B K2B O9B 93.7(10) . . ?
O12B K2B O11B 61.1(7) . . ?
O12B K2B N3B 119.0(9) . . ?
O12B K2B N4B 61.5(8) . . ?
N4B K2B N3B 178.9(10) . . ?
C36B O7B K2B 120(3) . . ?
C36B O7B C37B 105(3) . . ?
C37B O7B K2B 109(2) . . ?
C38B O8B K2B 108(3) . . ?
C38B O8B C39B 109(4) . . ?
C39B O8B K2B 119(3) . . ?
C42B O9B K2B 114(2) . . ?
C42B O9B C43B 105(3) . . ?
C43B O9B K2B 116(2) . . ?
C44B O10B K2B 113.6(18) . . ?
C45B O10B K2B 129(3) . . ?
C45B O10B C44B 111(3) . . ?
C48B O11B K2B 121(2) . . ?
C48B O11B C49B 114(3) . . ?
C49B O11B K2B 111.3(18) . . ?
C50B O12B K2B 120.6(19) . . ?
C50B O12B C51B 113(3) . . ?
C51B O12B K2B 115.6(18) . . ?
C35B N3B K2B 113(2) . . ?
C35B N3B C47B 106(3) . . ?
C46B N3B K2B 112(2) . . ?
C46B N3B C35B 106(3) . . ?
C46B N3B C47B 113(3) . . ?
C47B N3B K2B 107.1(18) . . ?
C40B N4B K2B 107.5(18) . . ?
C41B N4B K2B 106.2(18) . . ?
C41B N4B C40B 106(2) . . ?
C52B N4B K2B 108.1(19) . . ?
C52B N4B C40B 117(3) . . ?
C52B N4B C41B 112(3) . . ?
N3B C35B C36B 105(3) . . ?
O7B C36B C35B 102(3) . . ?
C38B C37B O7B 109(3) . . ?
O8B C38B K2B 51(3) . . ?
O8B C38B C37B 114(5) . . ?
C37B C38B K2B 86(3) . . ?
O8B C39B C40B 106(3) . . ?
N4B C40B C39B 112(3) . . ?
N4B C41B C42B 113(2) . . ?
O9B C42B C41B 105(3) . . ?
C44B C43B O9B 112(4) . . ?
C43B C44B O10B 121(3) . . ?
O10B C45B C46B 107(3) . . ?
N3B C46B C45B 108(3) . . ?
C48B C47B N3B 115(3) . . ?
O11B C48B C47B 114(3) . . ?
O11B C49B C50B 112(3) . . ?
O12B C50B C49B 108(3) . . ?
C52B C51B O12B 116(3) . . ?
N4B C52B C51B 119(3) . . ?
C30B P2B C27B 91.3(13) . . ?
C28B C27B P2B 112.6(18) . . ?
C28B C27B C31B 131(2) . . ?
C31B C27B P2B 115.7(18) . . ?
C27B C28B C32B 112(2) . . ?
C29B C28B C27B 124(2) . . ?
C29B C28B C32B 124(3) . . ?
C28B C29B C30B 100(2) . . ?
C28B C29B C33B 136(3) . . ?
C33B C29B C30B 124(2) . . ?
C29B C30B P2B 112.3(16) . . ?
C34B C30B P2B 132(2) . . ?
C34B C30B C29B 115(2) . . ?
O13B C53B C54B 124.4(14) . . ?
C53B O13B K1B 126.4(14) . . ?
C53B O13B C56B 87(2) . . ?
C56B O13B K1B 146(2) . . ?
O13B C56B C55B 103.3(17) . . ?
C53B C54B C55B 83.5(14) . . ?
C56B C55B C54B 110(2) . . ?

_olex2_exptl_crystal_mounting_method 'From paratone on a microscope slide.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.198
_oxdiff_exptl_absorpt_empirical_full_min 0.852
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive,Pyrophoric
####################################################################### 
# 
# 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_6
_database_code_depnum_ccdc_archive 'CCDC 2003390'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_manchester_internal_coll_name   ldpm35
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 1/2s
_manchester_internal_coll_frame_width 0.7
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   29/1/18
_manchester_internal_process_user CAPG
_manchester_internal_process_date 30/1/18
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 30/1/18
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 30/1/18
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 10/1/2020
_manchester_internal_archive_date 10/1/2020

_audit_creation_date             2018-01-30
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C14 H17 P'
_chemical_formula_sum            'C14 H17 P'
_chemical_formula_weight         216.24
_chemical_melting_point          ?
_chemical_oxdiff_formula         N
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.2955 0.4335 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   8.0727(2)
_cell_length_b                   8.74422(19)
_cell_length_c                   18.4065(4)
_cell_angle_alpha                103.1739(17)
_cell_angle_beta                 92.6248(19)
_cell_angle_gamma                100.705(2)
_cell_volume                     1237.81(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    7494
_cell_measurement_temperature    150.00(1)
_cell_measurement_theta_max      70.8880
_cell_measurement_theta_min      5.0090
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.664
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.703
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.160
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             464
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 3 -1 0.0664
-5 -1 -2 0.0332
-4 4 -6 0.0612
2 -5 6 0.0859
1 -1 -11 0.0664
-1 2 10 0.1082
-4 4 4 0.0540
5 -2 4 0.0421
-5 0 -2 0.0305
-2 -2 11 0.0797
-4 -2 -4 0.0290

_exptl_crystal_recrystallization_method 'Neat compound.'
_exptl_crystal_size_max          0.194
_exptl_crystal_size_mid          0.176
_exptl_crystal_size_min          0.089
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.9957 3.0030 -1.0088 -0.9357 0.3311 -0.2760
-4.9952 -1.0029 -1.9906 0.7741 -0.3075 0.6620
-3.9974 3.9995 -5.9951 -0.0383 0.0340 1.0377
1.9994 -5.0008 5.9992 0.4366 -0.1735 -0.8453
1.0008 -1.0026 -11.0022 -0.3137 -0.9366 0.1865
-1.0011 2.0029 10.0016 0.1746 0.9888 -0.0777
-3.9986 4.0017 4.0057 0.2204 0.7765 0.6809
4.9961 -1.9984 3.9922 -0.3825 0.0768 -0.9528
-4.9956 -0.0023 -1.9911 0.6608 -0.1811 0.7352
-1.9989 -1.9995 11.0054 0.7961 0.5509 -0.2732
-3.9955 -2.0035 -3.9921 0.6931 -0.5759 0.5275

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0190
_diffrn_reflns_av_unetI/netI     0.0218
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            13067
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         68.247
_diffrn_reflns_theta_min         2.476
_diffrn_ambient_temperature      150.00(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean ?
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.987
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     39.00  71.20   0.70    1.00    --    0.00  14.00-120.00   46
  2  ω    -86.00 -20.90   0.70    1.00    --    0.00  14.00-120.00   93
  3  ω     -1.00  25.60   0.70    1.00    --    0.00  14.00-120.00   38
  4  ω     58.00 142.00   0.70    2.00    --   55.00  60.00 -90.00  120
  5  ω    118.00 142.50   0.70    2.00    --   55.00  43.00   0.00   35
  6  ω      4.00  54.40   0.70    2.00    --   55.00  60.00 -60.00   72
  7  ω      8.00 141.70   0.70    2.00    --   55.00  29.00 -90.00  191
  8  ω    -30.00  -3.40   0.70    2.00    --   55.00  60.00 -90.00   38
  9  ω     52.00  94.70   0.70    2.00    --   55.00  43.00   0.00   61
 10  ω     36.00 143.10   0.70    2.00    --   55.00  60.00 150.00  153
 11  ω     83.00 142.50   0.70    2.00    --   55.00  43.00 150.00   85
 12  ω     39.00  79.60   0.70    2.00    --   55.00  43.00 150.00   58
 13  ω     13.00 143.20   0.70    2.00    --   55.00  60.00  30.00  186
 14  ω    140.00 175.00   0.70    2.00    --  110.00  60.00 120.00   50
 15  ω     88.00 118.10   0.70    2.00    --  110.00  60.00 120.00   43
 16  ω    101.00 133.90   0.70    2.00    --  110.00  29.00-180.00   47
 17  ω     35.00  61.60   0.70    2.00    --  110.00  60.00 120.00   38
 18  ω     81.00 123.00   0.70    2.00    --  110.00  48.00-180.00   60
 19  ω     63.00  89.60   0.70    2.00    --  110.00  48.00  30.00   38
 20  ω     65.00 196.60   0.70    2.00    --  110.00  60.00   0.00  188
 21  ω     35.00 116.20   0.70    2.00    --  110.00  57.00 -60.00  116
 22  ω    100.00 125.90   0.70    2.00    --  110.00  60.00-150.00   37
 23  ω     55.00  80.90   0.70    2.00    --  110.00  38.00 -60.00   37
 24  ω    135.00 160.90   0.70    2.00    --  110.00  48.00  30.00   37
 25  ω    167.00 198.50   0.70    2.00    --  110.00  48.00  30.00   45
 26  ω     22.00  60.50   0.70    2.00    --  110.00  60.00   0.00   55
 27  ω    136.00 194.10   0.70    2.00    --  110.00  60.00  60.00   83
 28  ω     48.00  99.10   0.70    2.00    --  110.00  19.00   0.00   73
 29  ω    131.00 183.50   0.70    2.00    --  110.00  19.00   0.00   75
 30  ω     74.00 165.00   0.70    2.00    --  110.00  60.00-180.00  130
 31  ω     21.00 144.20   0.70    2.00    --  110.00  10.00-180.00  176
 32  ω     88.00 196.50   0.70    2.00    --  110.00  38.00-120.00  155
 33  ω    109.00 186.70   0.70    2.00    --  110.00  57.00-120.00  111
 34  ω     27.00  53.60   0.70    2.00    --  110.00  48.00   0.00   38
 35  ω    119.00 175.00   0.70    2.00    --  110.00  60.00 -30.00   80
 36  ω    133.00 157.50   0.70    2.00    --  110.00  60.00  90.00   35
 37  ω     29.00 117.20   0.70    2.00    --  110.00  60.00  90.00  126
 38  ω     94.00 174.50   0.70    2.00    --  110.00  60.00-120.00  115
 39  ω    125.00 149.50   0.70    2.00    --  110.00  38.00 -90.00   35
 40  ω    154.00 178.50   0.70    2.00    --  110.00   0.00-150.00   35
 41  ω     36.00  61.20   0.70    2.00    --  110.00  10.00 -60.00   36
 42  ω     93.00 118.20   0.70    2.00    --  110.00  10.00 -60.00   36
 43  ω     62.00  87.20   0.70    2.00    --  110.00   0.00-150.00   36
 44  ω    142.00 166.50   0.70    2.00    --  110.00  60.00-150.00   35
 45  ω     57.00  82.20   0.70    2.00    --  110.00  38.00 -90.00   36
 46  ω    146.00 170.50   0.70    2.00    --  110.00  57.00 -60.00   35
 47  ω    163.00 187.50   0.70    2.00    --  110.00  29.00-180.00   35
 48  ω     39.00  64.20   0.70    2.00    --  110.00  57.00-120.00   36
 49  ω     96.00 122.60   0.70    2.00    --  110.00  38.00 -30.00   38
 50  ω    134.00 183.00   0.70    2.00    --  110.00  38.00 -30.00   70
 51  ω    134.00 158.50   0.70    2.00    --  110.00  29.00 -90.00   35
 52  ω     53.00 195.80   0.70    2.00    --  110.00  10.00  30.00  204
 53  ω    133.00 182.70   0.70    2.00    --  110.00  48.00 -30.00   71
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB AFC11 (RINC): quarter-chi single'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1425395000
_diffrn_orient_matrix_UB_12      -0.1132538000
_diffrn_orient_matrix_UB_13      0.0258707000
_diffrn_orient_matrix_UB_21      0.0066191000
_diffrn_orient_matrix_UB_22      0.1263664000
_diffrn_orient_matrix_UB_23      0.0742172000
_diffrn_orient_matrix_UB_31      -0.1329706000
_diffrn_orient_matrix_UB_32      0.0730339000
_diffrn_orient_matrix_UB_33      -0.0357025000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Cu) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4211
_reflns_number_total             4482
_reflns_odcompleteness_completeness 96.45
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     71.77
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.325
_refine_diff_density_min         -0.265
_refine_diff_density_rms         0.039
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.036
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         4482
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0344
_refine_ls_R_factor_gt           0.0329
_refine_ls_restrained_S_all      1.036
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0451P)²+0.4714P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0899
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H,H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(H5D)=Sof(H5E)=Sof(H5F)=1-FVAR(1)
 Sof(H5A)=Sof(H5B)=Sof(H5C)=FVAR(1)
 Sof(H22D)=Sof(H22E)=Sof(H22F)=1-FVAR(2)
 Sof(H22A)=Sof(H22B)=Sof(H22C)=FVAR(2)
 Sof(H21D)=Sof(H21E)=Sof(H21F)=1-FVAR(3)
 Sof(H21A)=Sof(H21B)=Sof(H21C)=FVAR(3)
3.a Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C24(H24), C25(H25),
 C26(H26), C27(H27), C28(H28)
3.b Disordered Me refined with riding coordinates:
 C5(H5A,H5B,H5C,H5D,H5E,H5F), C22(H22A,H22B,H22C,H22D,H22E,H22F), C21(H21A,
 H21B,H21C,H21D,H21E,H21F)
3.c Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C19(H19A,H19B,H19C),
 C20(H20A,H20B,H20C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     heavy
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
P1 P 0.62277(5) 0.75882(4) 0.56708(2) 0.02932(11) Uani 1 1 d . . . . .
C1 C 0.71302(19) 0.97002(16) 0.59241(8) 0.0307(3) Uani 1 1 d . . . . .
C2 C 0.88383(19) 0.99102(17) 0.59621(8) 0.0316(3) Uani 1 1 d . . . . .
C3 C 0.94915(19) 0.84186(18) 0.58941(8) 0.0325(3) Uani 1 1 d . . . . .
C4 C 0.82750(19) 0.70894(18) 0.58033(8) 0.0319(3) Uani 1 1 d . . . . .
C5 C 0.6090(2) 1.09802(19) 0.59942(10) 0.0409(4) Uani 1 1 d . . . . .
H5A H 0.488436 1.048319 0.594427 0.049 Uiso 0.616(19) 1 calc R . P . .
H5B H 0.638651 1.173643 0.648518 0.049 Uiso 0.616(19) 1 calc R . P . .
H5C H 0.632067 1.155368 0.559866 0.049 Uiso 0.616(19) 1 calc R . P . .
H5D H 0.684334 1.203234 0.607447 0.049 Uiso 0.384(19) 1 calc R . P . .
H5E H 0.534118 1.077911 0.553356 0.049 Uiso 0.384(19) 1 calc R . P . .
H5F H 0.540702 1.096185 0.642008 0.049 Uiso 0.384(19) 1 calc R . P . .
C6 C 1.0036(2) 1.1499(2) 0.60803(9) 0.0429(4) Uani 1 1 d . . . . .
H6A H 0.938733 1.234833 0.610139 0.064 Uiso 1 1 calc GR . . . .
H6B H 1.075362 1.147497 0.566435 0.064 Uiso 1 1 calc GR . . . .
H6C H 1.074715 1.170960 0.655219 0.064 Uiso 1 1 calc GR . . . .
C7 C 1.1365(2) 0.8478(2) 0.59403(10) 0.0470(4) Uani 1 1 d . . . . .
H7A H 1.184160 0.885696 0.551771 0.071 Uiso 1 1 calc GR . . . .
H7B H 1.157756 0.740213 0.592154 0.071 Uiso 1 1 calc GR . . . .
H7C H 1.189996 0.921203 0.641172 0.071 Uiso 1 1 calc GR . . . .
C8 C 0.8472(2) 0.5405(2) 0.57710(10) 0.0458(4) Uani 1 1 d . . . . .
H8A H 0.787586 0.501812 0.616683 0.069 Uiso 1 1 calc GR . . . .
H8B H 0.967645 0.538127 0.584376 0.069 Uiso 1 1 calc GR . . . .
H8C H 0.799250 0.471284 0.528145 0.069 Uiso 1 1 calc GR . . . .
C9 C 0.51702(17) 0.71478(16) 0.64804(8) 0.0275(3) Uani 1 1 d . . . . .
C10 C 0.41952(19) 0.56158(17) 0.64043(9) 0.0346(3) Uani 1 1 d . . . . .
H10 H 0.409199 0.484259 0.594039 0.042 Uiso 1 1 calc R . . . .
C11 C 0.3377(2) 0.52143(19) 0.69994(9) 0.0387(3) Uani 1 1 d . . . . .
H11 H 0.273863 0.415999 0.694532 0.046 Uiso 1 1 calc R . . . .
C12 C 0.34839(19) 0.63357(19) 0.76709(9) 0.0371(3) Uani 1 1 d . . . . .
H12 H 0.290778 0.605993 0.807602 0.044 Uiso 1 1 calc R . . . .
C13 C 0.4433(2) 0.78616(18) 0.77515(9) 0.0363(3) Uani 1 1 d . . . . .
H13 H 0.450629 0.863609 0.821318 0.044 Uiso 1 1 calc R . . . .
C14 C 0.52775(18) 0.82689(17) 0.71621(8) 0.0312(3) Uani 1 1 d . . . . .
H14 H 0.593346 0.931874 0.722357 0.037 Uiso 1 1 calc R . . . .
P2 P 0.10814(4) 0.21874(4) 0.83397(2) 0.02904(11) Uani 1 1 d . . . . .
C15 C 0.18984(17) 0.29842(17) 0.93118(8) 0.0299(3) Uani 1 1 d . . . . .
C16 C 0.21411(17) 0.17655(17) 0.96159(8) 0.0288(3) Uani 1 1 d . . . . .
C17 C 0.14835(17) 0.01585(17) 0.91264(8) 0.0278(3) Uani 1 1 d . . . . .
C18 C 0.07426(17) 0.01635(17) 0.84518(8) 0.0287(3) Uani 1 1 d . . . . .
C19 C 0.2358(2) 0.47459(19) 0.96631(10) 0.0429(4) Uani 1 1 d . . . . .
H19A H 0.343790 0.519964 0.949800 0.064 Uiso 1 1 calc GR . . . .
H19B H 0.246497 0.492198 1.020985 0.064 Uiso 1 1 calc GR . . . .
H19C H 0.147233 0.526949 0.951148 0.064 Uiso 1 1 calc GR . . . .
C20 C 0.3002(2) 0.1961(2) 1.03826(8) 0.0383(3) Uani 1 1 d . . . . .
H20A H 0.333504 0.310389 1.062990 0.057 Uiso 1 1 calc GR . . . .
H20B H 0.401032 0.148359 1.033685 0.057 Uiso 1 1 calc GR . . . .
H20C H 0.222102 0.142153 1.068102 0.057 Uiso 1 1 calc GR . . . .
C22 C -0.0097(2) -0.12608(19) 0.78413(9) 0.0378(3) Uani 1 1 d . . . . .
H22A H -0.051987 -0.089436 0.741677 0.045 Uiso 0.660(18) 1 calc R . P . .
H22B H 0.072565 -0.193371 0.767736 0.045 Uiso 0.660(18) 1 calc R . P . .
H22C H -0.104367 -0.188455 0.803108 0.045 Uiso 0.660(18) 1 calc R . P . .
H22D H -0.003873 -0.224739 0.800004 0.045 Uiso 0.340(18) 1 calc R . P . .
H22E H -0.128424 -0.120804 0.773944 0.045 Uiso 0.340(18) 1 calc R . P . .
H22F H 0.048508 -0.125720 0.738573 0.045 Uiso 0.340(18) 1 calc R . P . .
C23 C -0.10216(17) 0.26783(16) 0.82882(7) 0.0273(3) Uani 1 1 d . . . . .
C24 C -0.24042(18) 0.18728(17) 0.85713(8) 0.0312(3) Uani 1 1 d . . . . .
H24 H -0.227039 0.103073 0.880225 0.037 Uiso 1 1 calc R . . . .
C25 C -0.39714(19) 0.22887(18) 0.85192(9) 0.0353(3) Uani 1 1 d . . . . .
H25 H -0.490741 0.172822 0.871151 0.042 Uiso 1 1 calc R . . . .
C26 C -0.41762(18) 0.35186(18) 0.81876(9) 0.0357(3) Uani 1 1 d . . . . .
H26 H -0.525244 0.380215 0.815304 0.043 Uiso 1 1 calc R . . . .
C27 C -0.28212(19) 0.43344(19) 0.79069(9) 0.0369(3) Uani 1 1 d . . . . .
H27 H -0.296111 0.518577 0.768354 0.044 Uiso 1 1 calc R . . . .
C28 C -0.12489(18) 0.39087(18) 0.79512(9) 0.0334(3) Uani 1 1 d . . . . .
H28 H -0.032250 0.446132 0.775012 0.040 Uiso 1 1 calc R . . . .
C21 C 0.1638(2) -0.13306(18) 0.93793(9) 0.0351(3) Uani 1 1 d . . . . .
H21A H 0.221919 -0.103016 0.988562 0.042 Uiso 0.102(18) 1 calc R . P . .
H21B H 0.050631 -0.197190 0.938200 0.042 Uiso 0.102(18) 1 calc R . P . .
H21C H 0.228910 -0.196083 0.903503 0.042 Uiso 0.102(18) 1 calc R . P . .
H21D H 0.112387 -0.227843 0.898281 0.042 Uiso 0.898(18) 1 calc R . P . .
H21E H 0.283675 -0.133670 0.948644 0.042 Uiso 0.898(18) 1 calc R . P . .
H21F H 0.105397 -0.134776 0.983340 0.042 Uiso 0.898(18) 1 calc R . P . .


_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
P1 C1 1.7987(14) . ?
P1 C4 1.8058(15) . ?
P1 C9 1.8314(14) . ?
C1 C2 1.353(2) . ?
C1 C5 1.506(2) . ?
C2 C3 1.477(2) . ?
C2 C6 1.502(2) . ?
C3 C4 1.347(2) . ?
C3 C7 1.502(2) . ?
C4 C8 1.499(2) . ?
C9 C10 1.395(2) . ?
C9 C14 1.393(2) . ?
C10 C11 1.384(2) . ?
C11 C12 1.379(2) . ?
C12 C13 1.382(2) . ?
C13 C14 1.387(2) . ?
P2 C15 1.8097(15) . ?
P2 C18 1.8003(14) . ?
P2 C23 1.8303(14) . ?
C15 C16 1.352(2) . ?
C15 C19 1.497(2) . ?
C16 C17 1.473(2) . ?
C16 C20 1.5033(19) . ?
C17 C18 1.355(2) . ?
C17 C21 1.5029(19) . ?
C18 C22 1.501(2) . ?
C23 C24 1.394(2) . ?
C23 C28 1.394(2) . ?
C24 C25 1.385(2) . ?
C25 C26 1.383(2) . ?
C26 C27 1.379(2) . ?
C27 C28 1.391(2) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 P1 C4 91.68(7) . . ?
C1 P1 C9 106.06(6) . . ?
C4 P1 C9 103.36(6) . . ?
C2 C1 P1 109.13(11) . . ?
C2 C1 C5 127.14(14) . . ?
C5 C1 P1 123.42(11) . . ?
C1 C2 C3 114.45(13) . . ?
C1 C2 C6 125.02(14) . . ?
C3 C2 C6 120.52(14) . . ?
C2 C3 C7 120.16(14) . . ?
C4 C3 C2 114.03(13) . . ?
C4 C3 C7 125.80(15) . . ?
C3 C4 P1 109.39(11) . . ?
C3 C4 C8 128.53(15) . . ?
C8 C4 P1 122.01(12) . . ?
C10 C9 P1 118.04(11) . . ?
C14 C9 P1 123.29(11) . . ?
C14 C9 C10 118.67(13) . . ?
C11 C10 C9 120.48(14) . . ?
C12 C11 C10 120.40(14) . . ?
C11 C12 C13 119.68(14) . . ?
C12 C13 C14 120.36(14) . . ?
C13 C14 C9 120.39(13) . . ?
C15 P2 C23 104.71(6) . . ?
C18 P2 C15 91.53(6) . . ?
C18 P2 C23 105.76(6) . . ?
C16 C15 P2 109.25(11) . . ?
C16 C15 C19 127.95(14) . . ?
C19 C15 P2 122.55(11) . . ?
C15 C16 C17 114.23(12) . . ?
C15 C16 C20 125.03(14) . . ?
C17 C16 C20 120.74(13) . . ?
C16 C17 C21 121.18(12) . . ?
C18 C17 C16 114.35(12) . . ?
C18 C17 C21 124.46(13) . . ?
C17 C18 P2 109.34(11) . . ?
C17 C18 C22 127.47(13) . . ?
C22 C18 P2 122.95(11) . . ?
C24 C23 P2 122.74(11) . . ?
C24 C23 C28 118.67(13) . . ?
C28 C23 P2 118.60(11) . . ?
C25 C24 C23 120.60(13) . . ?
C26 C25 C24 120.11(14) . . ?
C27 C26 C25 120.13(14) . . ?
C26 C27 C28 119.91(14) . . ?
C27 C28 C23 120.57(14) . . ?

_olex2_date_sample_completion    2018-01-29
_olex2_date_sample_data_collection 2018-01-29
_olex2_date_sample_submission    2018-01-29
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id ldpm35
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 25.031
_oxdiff_exptl_absorpt_empirical_full_min 0.525
####################################################################### 
# 
# 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_7
_database_code_depnum_ccdc_archive 'CCDC 2017380'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-07-19 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         dq1025
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   10s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         6/4/19
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      6/4/19
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     6/5/19
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   6/5/19
_LANL_internal_validation_user   ?
_LANL_internal_validation_date   ?
_LANL_internal_archive_date      ?
_LANL_internal_LA-UR             ?

_audit_creation_date             2019-06-05
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C32 H48 Co2 P4'
_chemical_formula_sum            'C32 H48 Co2 P4'
_chemical_formula_weight         674.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         Co(PC8H12)2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Co Co 0.3494 0.9721 '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'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'C 1 2/c 1'
_space_group_name_Hall           '-C 2yc'
loop_
_space_group_symop_operation_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                   20.161(3)
_cell_length_b                   9.0620(4)
_cell_length_c                   20.214(3)
_cell_angle_alpha                90
_cell_angle_beta                 119.71(2)
_cell_angle_gamma                90
_cell_volume                     3207.7(9)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    2287
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.0460
_cell_measurement_theta_min      2.3680
_shelx_estimated_absorpt_T_max   0.885
_shelx_estimated_absorpt_T_min   0.634
_exptl_absorpt_coefficient_mu    1.254
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.86109
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.397
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       'rect. Prism'
_exptl_crystal_F_000             1416
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From n-hexane.'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0647
_diffrn_reflns_av_unetI/netI     0.0456
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            17531
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.342
_diffrn_reflns_theta_min         2.326
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.27 185.27   0.50   10.00    --   28.00  73.72 -25.73  366
  2  ω      2.27 185.27   0.50   10.00    --   28.80  73.72  64.27  366
  3  ω      2.27 185.27   0.50   10.00    --   28.00  73.72 154.27  366
  4  ω      2.27 126.77   0.50   10.00    --   28.00  73.72-115.73  249
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0189981000
_diffrn_orient_matrix_UB_12      -0.0029387000
_diffrn_orient_matrix_UB_13      0.0403178000
_diffrn_orient_matrix_UB_21      0.0357423500
_diffrn_orient_matrix_UB_22      -0.0015310500
_diffrn_orient_matrix_UB_23      0.0011699000
_diffrn_orient_matrix_UB_31      0.0014079000
_diffrn_orient_matrix_UB_32      0.0782694000
_diffrn_orient_matrix_UB_33      0.0015344000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                2325
_reflns_number_total             2935
_reflns_odcompleteness_completeness 99.29
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.504
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.094
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         2935
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0491
_refine_ls_R_factor_gt           0.0333
_refine_ls_restrained_S_all      1.009
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0439P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0775
_refine_ls_wR_factor_ref         0.0834
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.5 times of:
  All C(H,H,H) groups
2.a Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Co1 Co 0.57257(2) 0.24195(4) 0.30728(2) 0.01024(12) Uani 1 1 d . . . . .
P1 P 0.63293(4) 0.19292(8) 0.43554(4) 0.01549(18) Uani 1 1 d . . . . .
P2 P 0.47088(4) 0.31069(7) 0.31004(4) 0.01130(17) Uani 1 1 d . . . . .
C1 C 0.66887(14) 0.3348(3) 0.40038(15) 0.0150(6) Uani 1 1 d . . . . .
C2 C 0.68931(14) 0.2794(3) 0.34772(15) 0.0163(6) Uani 1 1 d . . . . .
C3 C 0.67430(14) 0.1229(3) 0.33396(15) 0.0157(6) Uani 1 1 d . . . . .
C4 C 0.64368(14) 0.0615(3) 0.37663(14) 0.0143(6) Uani 1 1 d . . . . .
C5 C 0.67811(16) 0.4932(3) 0.42651(16) 0.0247(7) Uani 1 1 d . . . . .
H5A H 0.665108 0.558860 0.383245 0.037 Uiso 1 1 calc GR . . . .
H5B H 0.731151 0.510453 0.466124 0.037 Uiso 1 1 calc GR . . . .
H5C H 0.644085 0.513147 0.447124 0.037 Uiso 1 1 calc GR . . . .
C6 C 0.72672(15) 0.3700(3) 0.31300(16) 0.0234(7) Uani 1 1 d . . . . .
H6A H 0.711225 0.332855 0.261837 0.035 Uiso 1 1 calc GR . . . .
H6B H 0.782345 0.363005 0.344837 0.035 Uiso 1 1 calc GR . . . .
H6C H 0.710986 0.473338 0.309692 0.035 Uiso 1 1 calc GR . . . .
C7 C 0.69693(16) 0.0338(3) 0.28573(16) 0.0236(7) Uani 1 1 d . . . . .
H7A H 0.663027 -0.051733 0.264864 0.035 Uiso 1 1 calc GR . . . .
H7B H 0.749761 -0.000009 0.316943 0.035 Uiso 1 1 calc GR . . . .
H7C H 0.692787 0.095029 0.243877 0.035 Uiso 1 1 calc GR . . . .
C8 C 0.62566(16) -0.1006(3) 0.37508(16) 0.0236(7) Uani 1 1 d . . . . .
H8A H 0.597780 -0.116741 0.402708 0.035 Uiso 1 1 calc GR . . . .
H8B H 0.673322 -0.157278 0.399364 0.035 Uiso 1 1 calc GR . . . .
H8C H 0.594191 -0.133034 0.322165 0.035 Uiso 1 1 calc GR . . . .
C9 C 0.44852(14) 0.4863(3) 0.33723(14) 0.0136(6) Uani 1 1 d . . . . .
C10 C 0.42380(14) 0.4648(3) 0.38721(14) 0.0149(6) Uani 1 1 d . . . . .
C11 C 0.42090(14) 0.3079(3) 0.40651(15) 0.0150(6) Uani 1 1 d . . . . .
C12 C 0.44460(14) 0.2126(3) 0.37162(14) 0.0131(6) Uani 1 1 d . . . . .
C13 C 0.45315(16) 0.6315(3) 0.30356(17) 0.0234(7) Uani 1 1 d . . . . .
H13A H 0.506379 0.664787 0.328571 0.035 Uiso 1 1 calc GR . . . .
H13B H 0.421973 0.704969 0.311285 0.035 Uiso 1 1 calc GR . . . .
H13C H 0.434130 0.619210 0.248893 0.035 Uiso 1 1 calc GR . . . .
C14 C 0.40278(15) 0.5852(3) 0.42539(15) 0.0207(6) Uani 1 1 d . . . . .
H14A H 0.351897 0.565594 0.418411 0.031 Uiso 1 1 calc GR . . . .
H14B H 0.402597 0.680755 0.402564 0.031 Uiso 1 1 calc GR . . . .
H14C H 0.440220 0.587352 0.479914 0.031 Uiso 1 1 calc GR . . . .
C15 C 0.39534(17) 0.2654(3) 0.46249(16) 0.0236(7) Uani 1 1 d . . . . .
H15A H 0.431185 0.305605 0.512786 0.035 Uiso 1 1 calc GR . . . .
H15B H 0.394013 0.157622 0.465608 0.035 Uiso 1 1 calc GR . . . .
H15C H 0.344220 0.305372 0.445465 0.035 Uiso 1 1 calc GR . . . .
C16 C 0.45533(15) 0.0483(3) 0.38501(15) 0.0187(6) Uani 1 1 d . . . . .
H16A H 0.462397 0.002780 0.344945 0.028 Uiso 1 1 calc GR . . . .
H16B H 0.410124 0.005938 0.384033 0.028 Uiso 1 1 calc GR . . . .
H16C H 0.500432 0.029435 0.434732 0.028 Uiso 1 1 calc GR . . . .


_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
Co1 Co1 2.6848(10) 2_655 ?
Co1 P1 2.2964(9) . ?
Co1 P2 2.1696(8) . ?
Co1 P2 2.1727(9) 2_655 ?
Co1 C1 2.097(3) . ?
Co1 C2 2.101(3) . ?
Co1 C3 2.137(2) . ?
Co1 C4 2.169(2) . ?
P1 C1 1.787(3) . ?
P1 C4 1.772(3) . ?
P2 C9 1.812(3) . ?
P2 C12 1.809(3) . ?
C1 C2 1.410(4) . ?
C1 C5 1.509(3) . ?
C2 C3 1.448(4) . ?
C2 C6 1.504(4) . ?
C3 C4 1.401(4) . ?
C3 C7 1.500(3) . ?
C4 C8 1.510(3) . ?
C9 C10 1.344(4) . ?
C9 C13 1.505(4) . ?
C10 C11 1.484(4) . ?
C10 C14 1.513(3) . ?
C11 C12 1.344(4) . ?
C11 C15 1.507(4) . ?
C12 C16 1.510(3) . ?

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
P1 Co1 Co1 135.65(3) . 2_655 ?
P2 Co1 Co1 51.86(2) . 2_655 ?
P2 Co1 Co1 51.76(3) 2_655 2_655 ?
P2 Co1 P1 90.30(3) . . ?
P2 Co1 P1 171.60(3) 2_655 . ?
P2 Co1 P2 94.06(3) . 2_655 ?
C1 Co1 Co1 154.51(7) . 2_655 ?
C1 Co1 P1 47.73(8) . . ?
C1 Co1 P2 123.90(8) . 2_655 ?
C1 Co1 P2 109.16(8) . . ?
C1 Co1 C2 39.26(10) . . ?
C1 Co1 C3 68.28(10) . . ?
C1 Co1 C4 72.59(10) . . ?
C2 Co1 Co1 150.15(8) . 2_655 ?
C2 Co1 P1 74.17(8) . . ?
C2 Co1 P2 146.52(8) . . ?
C2 Co1 P2 98.41(8) . 2_655 ?
C2 Co1 C3 39.95(10) . . ?
C2 Co1 C4 67.42(10) . . ?
C3 Co1 Co1 135.83(7) . 2_655 ?
C3 Co1 P1 73.26(8) . . ?
C3 Co1 P2 103.75(8) . 2_655 ?
C3 Co1 P2 159.97(8) . . ?
C3 Co1 C4 37.97(9) . . ?
C4 Co1 Co1 130.27(7) . 2_655 ?
C4 Co1 P1 46.65(7) . . ?
C4 Co1 P2 134.55(7) . 2_655 ?
C4 Co1 P2 122.02(7) . . ?
C1 P1 Co1 60.27(8) . . ?
C4 P1 Co1 62.88(8) . . ?
C4 P1 C1 90.42(12) . . ?
Co1 P2 Co1 76.38(3) . 2_655 ?
C9 P2 Co1 123.82(9) . 2_655 ?
C9 P2 Co1 129.81(9) . . ?
C12 P2 Co1 118.64(9) . . ?
C12 P2 Co1 120.86(9) . 2_655 ?
C12 P2 C9 91.21(12) . . ?
P1 C1 Co1 71.99(9) . . ?
C2 C1 Co1 70.54(15) . . ?
C2 C1 P1 111.84(19) . . ?
C2 C1 C5 124.8(2) . . ?
C5 C1 Co1 126.48(18) . . ?
C5 C1 P1 123.3(2) . . ?
C1 C2 Co1 70.20(15) . . ?
C1 C2 C3 112.5(2) . . ?
C1 C2 C6 124.0(2) . . ?
C3 C2 Co1 71.34(14) . . ?
C3 C2 C6 123.4(2) . . ?
C6 C2 Co1 129.11(19) . . ?
C2 C3 Co1 68.71(14) . . ?
C2 C3 C7 123.3(2) . . ?
C4 C3 Co1 72.25(14) . . ?
C4 C3 C2 112.6(2) . . ?
C4 C3 C7 123.7(2) . . ?
C7 C3 Co1 132.11(18) . . ?
P1 C4 Co1 70.47(9) . . ?
C3 C4 Co1 69.78(14) . . ?
C3 C4 P1 112.64(19) . . ?
C3 C4 C8 123.3(2) . . ?
C8 C4 Co1 130.17(18) . . ?
C8 C4 P1 124.0(2) . . ?
C10 C9 P2 109.97(19) . . ?
C10 C9 C13 126.6(2) . . ?
C13 C9 P2 123.36(19) . . ?
C9 C10 C11 114.5(2) . . ?
C9 C10 C14 125.5(2) . . ?
C11 C10 C14 120.0(2) . . ?
C10 C11 C15 121.0(2) . . ?
C12 C11 C10 114.0(2) . . ?
C12 C11 C15 124.9(2) . . ?
C11 C12 P2 110.3(2) . . ?
C11 C12 C16 126.6(2) . . ?
C16 C12 P2 122.89(19) . . ?

_olex2_exptl_crystal_mounting_method 
'From paratone on a microscope slide, onto a cryoloop.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.168
_oxdiff_exptl_absorpt_empirical_full_min 0.897
_chemical_properties_physical    
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_2-Cr
_database_code_depnum_ccdc_archive 'CCDC 2003387'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_LANL_internal_coll_name         dq1027
_LANL_internal_coll_client       CAPG
_LANL_internal_coll_type         custom
_LANL_internal_coll_frame_time   30s
_LANL_internal_coll_frame_width  0.5
_LANL_internal_coll_frame_method '\w scans'
_LANL_internal_coll_user         CAPG
_LANL_internal_coll_date         7/7/19
_LANL_internal_process_user      CAPG
_LANL_internal_process_date      7/10/19
_LANL_internal_solution_user     CAPG
_LANL_internal_solution_date     7/11/19
_LANL_internal_refinement_user   CAPG
_LANL_internal_refinement_date   7/12/19
_LANL_internal_validation_user   CAPG
_LANL_internal_validation_date   10/1/2020
_LANL_internal_archive_date      10/1/2020
_LANL_internal_LA-UR             ?

_audit_creation_date             2019-06-12
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C16 H24 Cr P2, C18 H36 K N2 O6'
_chemical_formula_sum            'C34 H60 Cr K N2 O6 P2'
_chemical_formula_weight         745.88
_chemical_melting_point          ?
_chemical_oxdiff_formula         KO6N2C18H36Cr(C8H12P)2
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cr Cr 0.3209 0.6236 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
K K 0.2009 0.2494 '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 0.0060 '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'

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

_cell_length_a                   10.1994(4)
_cell_length_b                   14.2193(7)
_cell_length_c                   15.0882(6)
_cell_angle_alpha                62.328(4)
_cell_angle_beta                 86.597(3)
_cell_angle_gamma                87.156(3)
_cell_volume                     1933.91(16)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    5781
_cell_measurement_temperature    100.0(2)
_cell_measurement_theta_max      28.7850
_cell_measurement_theta_min      2.4850
_shelx_estimated_absorpt_T_max   0.857
_shelx_estimated_absorpt_T_min   0.857
_exptl_absorpt_coefficient_mu    0.529
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.90197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear black'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.281
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       cube
_exptl_crystal_F_000             798
_exptl_crystal_preparation       'By CAPG.'
_exptl_crystal_recrystallization_method 'From THF.'
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.3
_exptl_crystal_size_min          0.3
_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0332
_diffrn_reflns_av_unetI/netI     0.0338
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            23292
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.350
_diffrn_reflns_theta_min         1.618
_diffrn_ambient_temperature      100.0(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω      2.27 185.27   0.50   30.00    --   28.00  73.72 -25.73  366
  2  ω      2.27 185.27   0.50   30.00    --   28.80  73.72  64.27  366
  3  ω      2.27 185.27   0.50   30.00    --   28.00  73.72 154.27  366
  4  ω      2.27 185.27   0.50   30.00    --   28.00  73.72-115.73  366
;
_diffrn_measurement_device       'abstract diffractometer'
_diffrn_measurement_device_type  
'Saxi-CrysAlisPro-abstract goniometer imported SAXI images'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0095924000
_diffrn_orient_matrix_UB_12      -0.0461027000
_diffrn_orient_matrix_UB_13      -0.0054196000
_diffrn_orient_matrix_UB_21      -0.0599920000
_diffrn_orient_matrix_UB_22      -0.0087431000
_diffrn_orient_matrix_UB_23      0.0286659000
_diffrn_orient_matrix_UB_31      -0.0341375000
_diffrn_orient_matrix_UB_32      0.0311870000
_diffrn_orient_matrix_UB_33      -0.0443997000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5848
_reflns_number_total             7060
_reflns_odcompleteness_completeness 98.80
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.485
_refine_diff_density_min         -0.250
_refine_diff_density_rms         0.084
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.100
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     423
_refine_ls_number_reflns         7060
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0459
_refine_ls_R_factor_gt           0.0338
_refine_ls_restrained_S_all      1.100
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0481P)²+0.2396P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0816
_refine_ls_wR_factor_ref         0.0872
_refine_special_details          ?
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C17(H17A,H17B), C18(H18A,H18B), C19(H19A,H19B), C20(H20A,H20B), C21(H21A,
 H21B), C22(H22A,H22B), C23(H23A,H23B), C24(H24A,H24B), C25(H25A,H25B),
 C26(H26A,H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B),
  C31(H31A,H31B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B)
2.b Idealised Me refined as rotating group:
 C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C13(H13A,
 H13B,H13C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Cr1 Cr 0.81663(3) 0.16130(2) 0.72559(2) 0.01135(9) Uani 1 1 d . . . . .
P1 P 0.79790(5) 0.05761(4) 0.64229(4) 0.01685(12) Uani 1 1 d . . . . .
P2 P 0.78691(5) 0.31477(4) 0.74779(4) 0.01392(12) Uani 1 1 d . . . . .
C1 C 0.65432(19) 0.12422(15) 0.66376(14) 0.0178(4) Uani 1 1 d . . . . .
C2 C 0.62465(18) 0.09296(14) 0.76703(14) 0.0149(4) Uani 1 1 d . . . . .
C3 C 0.71958(18) 0.01815(14) 0.83018(13) 0.0129(4) Uani 1 1 d . . . . .
C4 C 0.82232(18) -0.00655(14) 0.77474(13) 0.0136(4) Uani 1 1 d . . . . .
C5 C 0.5728(2) 0.20373(16) 0.57973(16) 0.0284(5) Uani 1 1 d . . . . .
H5A H 0.546765 0.263451 0.592970 0.043 Uiso 1 1 calc GR . . . .
H5B H 0.494112 0.169573 0.575264 0.043 Uiso 1 1 calc GR . . . .
H5C H 0.624642 0.229808 0.516402 0.043 Uiso 1 1 calc GR . . . .
C6 C 0.50218(19) 0.12645(16) 0.80703(17) 0.0237(5) Uani 1 1 d . . . . .
H6A H 0.440277 0.068096 0.835049 0.035 Uiso 1 1 calc GR . . . .
H6B H 0.461488 0.188754 0.752547 0.035 Uiso 1 1 calc GR . . . .
H6C H 0.525121 0.144294 0.859500 0.035 Uiso 1 1 calc GR . . . .
C7 C 0.7085(2) -0.03451(16) 0.94306(14) 0.0205(4) Uani 1 1 d . . . . .
H7A H 0.796508 -0.052852 0.969923 0.031 Uiso 1 1 calc GR . . . .
H7B H 0.657641 -0.099218 0.967668 0.031 Uiso 1 1 calc GR . . . .
H7C H 0.664035 0.014335 0.964924 0.031 Uiso 1 1 calc GR . . . .
C8 C 0.9306(2) -0.08797(15) 0.82235(15) 0.0208(4) Uani 1 1 d . . . . .
H8A H 1.003635 -0.075459 0.773256 0.031 Uiso 1 1 calc GR . . . .
H8B H 0.897164 -0.159284 0.844916 0.031 Uiso 1 1 calc GR . . . .
H8C H 0.961446 -0.082121 0.879847 0.031 Uiso 1 1 calc GR . . . .
C9 C 0.86734(19) 0.32607(15) 0.63381(14) 0.0168(4) Uani 1 1 d . . . . .
C10 C 0.98377(19) 0.26092(15) 0.65106(15) 0.0173(4) Uani 1 1 d . . . . .
C11 C 1.00688(18) 0.19731(14) 0.75447(14) 0.0153(4) Uani 1 1 d . . . . .
C12 C 0.90597(18) 0.21298(14) 0.81776(14) 0.0136(4) Uani 1 1 d . . . . .
C13 C 0.8192(2) 0.40082(16) 0.53125(14) 0.0252(5) Uani 1 1 d . . . . .
H13A H 0.833005 0.367463 0.487243 0.038 Uiso 1 1 calc GR . . . .
H13B H 0.868043 0.466823 0.503310 0.038 Uiso 1 1 calc GR . . . .
H13C H 0.725359 0.416738 0.536564 0.038 Uiso 1 1 calc GR . . . .
C14 C 1.0772(2) 0.26501(17) 0.56798(16) 0.0270(5) Uani 1 1 d . . . . .
H14A H 1.111045 0.193205 0.584843 0.040 Uiso 1 1 calc GR . . . .
H14B H 1.150552 0.310741 0.559843 0.040 Uiso 1 1 calc GR . . . .
H14C H 1.030751 0.293744 0.505336 0.040 Uiso 1 1 calc GR . . . .
C15 C 1.12519(19) 0.12488(16) 0.79389(17) 0.0245(5) Uani 1 1 d . . . . .
H15A H 1.100702 0.063130 0.857210 0.037 Uiso 1 1 calc GR . . . .
H15B H 1.194215 0.163263 0.805113 0.037 Uiso 1 1 calc GR . . . .
H15C H 1.157713 0.101057 0.745011 0.037 Uiso 1 1 calc GR . . . .
C16 C 0.9084(2) 0.16117(15) 0.93029(14) 0.0191(4) Uani 1 1 d . . . . .
H16A H 0.818301 0.154968 0.958534 0.029 Uiso 1 1 calc GR . . . .
H16B H 0.958671 0.204526 0.950490 0.029 Uiso 1 1 calc GR . . . .
H16C H 0.949792 0.090282 0.955088 0.029 Uiso 1 1 calc GR . . . .
K1 K 0.68259(4) 0.35590(3) 0.22045(3) 0.01436(10) Uani 1 1 d . . . . .
O1 O 0.60135(13) 0.31379(11) 0.06376(10) 0.0205(3) Uani 1 1 d . . . . .
O2 O 0.74616(14) 0.49841(11) 0.01309(10) 0.0249(3) Uani 1 1 d . . . . .
O3 O 0.52814(13) 0.49681(10) 0.27113(10) 0.0196(3) Uani 1 1 d . . . . .
O4 O 0.45634(12) 0.28586(10) 0.34744(10) 0.0169(3) Uani 1 1 d . . . . .
O5 O 0.84564(13) 0.17431(10) 0.31467(10) 0.0168(3) Uani 1 1 d . . . . .
O6 O 0.92353(12) 0.37288(10) 0.29196(10) 0.0180(3) Uani 1 1 d . . . . .
N1 N 0.57880(15) 0.14328(12) 0.27598(12) 0.0168(4) Uani 1 1 d . . . . .
N2 N 0.78223(16) 0.57224(13) 0.16215(13) 0.0212(4) Uani 1 1 d . . . . .
C17 C 0.5097(2) 0.15024(16) 0.18938(15) 0.0220(4) Uani 1 1 d . . . . .
H17A H 0.425423 0.189831 0.183781 0.026 Uiso 1 1 calc R . . . .
H17B H 0.489241 0.077593 0.202124 0.026 Uiso 1 1 calc R . . . .
C18 C 0.5870(2) 0.20379(16) 0.09148(15) 0.0243(5) Uani 1 1 d . . . . .
H18A H 0.674829 0.168793 0.097851 0.029 Uiso 1 1 calc R . . . .
H18B H 0.541211 0.197056 0.038742 0.029 Uiso 1 1 calc R . . . .
C19 C 0.6778(2) 0.36615(18) -0.02795(15) 0.0262(5) Uani 1 1 d . . . . .
H19A H 0.639534 0.354597 -0.080795 0.031 Uiso 1 1 calc R . . . .
H19B H 0.768753 0.336429 -0.018513 0.031 Uiso 1 1 calc R . . . .
C20 C 0.6791(2) 0.48193(18) -0.05881(15) 0.0271(5) Uani 1 1 d . . . . .
H20A H 0.723971 0.519803 -0.125559 0.033 Uiso 1 1 calc R . . . .
H20B H 0.587825 0.510544 -0.063402 0.033 Uiso 1 1 calc R . . . .
C21 C 0.7511(2) 0.60824(17) -0.01349(16) 0.0320(5) Uani 1 1 d . . . . .
H21A H 0.661249 0.636748 -0.010597 0.038 Uiso 1 1 calc R . . . .
H21B H 0.788046 0.648089 -0.082762 0.038 Uiso 1 1 calc R . . . .
C22 C 0.8357(2) 0.62173(17) 0.05822(16) 0.0301(5) Uani 1 1 d . . . . .
H22A H 0.924048 0.590330 0.056436 0.036 Uiso 1 1 calc R . . . .
H22B H 0.846015 0.698537 0.035383 0.036 Uiso 1 1 calc R . . . .
C23 C 0.6730(2) 0.63902(16) 0.17195(17) 0.0275(5) Uani 1 1 d . . . . .
H23A H 0.615555 0.660752 0.114637 0.033 Uiso 1 1 calc R . . . .
H23B H 0.709507 0.704284 0.167678 0.033 Uiso 1 1 calc R . . . .
C24 C 0.5904(2) 0.58636(16) 0.26751(17) 0.0275(5) Uani 1 1 d . . . . .
H24A H 0.646459 0.563058 0.325782 0.033 Uiso 1 1 calc R . . . .
H24B H 0.523023 0.637494 0.270482 0.033 Uiso 1 1 calc R . . . .
C25 C 0.4490(2) 0.44610(15) 0.36118(14) 0.0208(4) Uani 1 1 d . . . . .
H25A H 0.389605 0.499252 0.368970 0.025 Uiso 1 1 calc R . . . .
H25B H 0.505717 0.413395 0.419530 0.025 Uiso 1 1 calc R . . . .
C26 C 0.36998(19) 0.36271(15) 0.35714(15) 0.0200(4) Uani 1 1 d . . . . .
H26A H 0.313842 0.327955 0.419035 0.024 Uiso 1 1 calc R . . . .
H26B H 0.312260 0.395517 0.299361 0.024 Uiso 1 1 calc R . . . .
C27 C 0.38788(19) 0.19698(16) 0.35627(16) 0.0227(5) Uani 1 1 d . . . . .
H27A H 0.333807 0.218366 0.297238 0.027 Uiso 1 1 calc R . . . .
H27B H 0.328796 0.169691 0.416976 0.027 Uiso 1 1 calc R . . . .
C28 C 0.4869(2) 0.11154(15) 0.36313(15) 0.0213(4) Uani 1 1 d . . . . .
H28A H 0.538043 0.089784 0.423679 0.026 Uiso 1 1 calc R . . . .
H28B H 0.439057 0.048800 0.371653 0.026 Uiso 1 1 calc R . . . .
C29 C 0.6877(2) 0.06390(15) 0.30166(15) 0.0204(4) Uani 1 1 d . . . . .
H29A H 0.733531 0.071758 0.238956 0.025 Uiso 1 1 calc R . . . .
H29B H 0.650763 -0.008045 0.336215 0.025 Uiso 1 1 calc R . . . .
C30 C 0.7863(2) 0.07304(15) 0.36730(15) 0.0207(4) Uani 1 1 d . . . . .
H30A H 0.742130 0.065769 0.430316 0.025 Uiso 1 1 calc R . . . .
H30B H 0.854297 0.015816 0.384354 0.025 Uiso 1 1 calc R . . . .
C31 C 0.95102(19) 0.18366(15) 0.36836(15) 0.0190(4) Uani 1 1 d . . . . .
H31A H 1.016272 0.124999 0.382618 0.023 Uiso 1 1 calc R . . . .
H31B H 0.916900 0.179418 0.432891 0.023 Uiso 1 1 calc R . . . .
C32 C 1.01441(18) 0.28840(15) 0.30564(15) 0.0190(4) Uani 1 1 d . . . . .
H32A H 1.092511 0.293529 0.338975 0.023 Uiso 1 1 calc R . . . .
H32B H 1.043739 0.293954 0.239687 0.023 Uiso 1 1 calc R . . . .
C33 C 0.9859(2) 0.47323(16) 0.24603(17) 0.0260(5) Uani 1 1 d . . . . .
H33A H 1.026887 0.486015 0.180376 0.031 Uiso 1 1 calc R . . . .
H33B H 1.055869 0.473085 0.288857 0.031 Uiso 1 1 calc R . . . .
C34 C 0.8859(2) 0.56009(16) 0.23172(17) 0.0253(5) Uani 1 1 d . . . . .
H34A H 0.843931 0.545039 0.297667 0.030 Uiso 1 1 calc R . . . .
H34B H 0.931755 0.628165 0.205872 0.030 Uiso 1 1 calc R . . . .


_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
Cr1 P1 2.3596(6) . ?
Cr1 P2 2.3596(6) . ?
Cr1 C1 2.1485(19) . ?
Cr1 C2 2.1561(18) . ?
Cr1 C3 2.1551(18) . ?
Cr1 C4 2.1440(18) . ?
Cr1 C9 2.1671(19) . ?
Cr1 C10 2.1702(19) . ?
Cr1 C11 2.1503(19) . ?
Cr1 C12 2.1143(18) . ?
P1 C1 1.799(2) . ?
P1 C4 1.7975(19) . ?
P2 C9 1.8015(19) . ?
P2 C12 1.8007(18) . ?
C1 C2 1.425(3) . ?
C1 C5 1.509(3) . ?
C2 C3 1.429(3) . ?
C2 C6 1.507(3) . ?
C3 C4 1.433(2) . ?
C3 C7 1.508(3) . ?
C4 C8 1.507(3) . ?
C9 C10 1.428(3) . ?
C9 C13 1.509(3) . ?
C10 C11 1.421(3) . ?
C10 C14 1.510(3) . ?
C11 C12 1.442(3) . ?
C11 C15 1.505(3) . ?
C12 C16 1.506(3) . ?
K1 O1 2.8690(14) . ?
K1 O2 2.8838(14) . ?
K1 O3 2.8368(13) . ?
K1 O4 2.8140(13) . ?
K1 O5 2.8104(13) . ?
K1 O6 2.8066(13) . ?
K1 N1 2.9703(16) . ?
K1 N2 2.9934(16) . ?
O1 C18 1.432(2) . ?
O1 C19 1.432(2) . ?
O2 C20 1.428(2) . ?
O2 C21 1.423(3) . ?
O3 C24 1.428(2) . ?
O3 C25 1.427(2) . ?
O4 C26 1.425(2) . ?
O4 C27 1.422(2) . ?
O5 C30 1.428(2) . ?
O5 C31 1.431(2) . ?
O6 C32 1.424(2) . ?
O6 C33 1.428(2) . ?
N1 C17 1.482(2) . ?
N1 C28 1.468(2) . ?
N1 C29 1.476(2) . ?
N2 C22 1.471(3) . ?
N2 C23 1.474(3) . ?
N2 C34 1.482(3) . ?
C17 C18 1.503(3) . ?
C19 C20 1.489(3) . ?
C21 C22 1.508(3) . ?
C23 C24 1.505(3) . ?
C25 C26 1.492(3) . ?
C27 C28 1.510(3) . ?
C29 C30 1.503(3) . ?
C31 C32 1.499(3) . ?
C33 C34 1.505(3) . ?

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
P2 Cr1 P1 155.43(2) . . ?
C1 Cr1 P1 46.76(5) . . ?
C1 Cr1 P2 115.42(5) . . ?
C1 Cr1 C2 38.67(7) . . ?
C1 Cr1 C3 66.75(7) . . ?
C1 Cr1 C9 109.76(7) . . ?
C1 Cr1 C10 130.10(7) . . ?
C1 Cr1 C11 164.92(7) . . ?
C2 Cr1 P1 73.42(5) . . ?
C2 Cr1 P2 102.29(5) . . ?
C2 Cr1 C9 128.72(7) . . ?
C2 Cr1 C10 165.24(7) . . ?
C3 Cr1 P1 73.29(5) . . ?
C3 Cr1 P2 118.87(5) . . ?
C3 Cr1 C2 38.72(7) . . ?
C3 Cr1 C9 163.49(7) . . ?
C3 Cr1 C10 155.63(7) . . ?
C4 Cr1 P1 46.74(5) . . ?
C4 Cr1 P2 154.53(5) . . ?
C4 Cr1 C1 71.77(7) . . ?
C4 Cr1 C2 67.26(7) . . ?
C4 Cr1 C3 38.94(7) . . ?
C4 Cr1 C9 157.21(7) . . ?
C4 Cr1 C10 122.62(7) . . ?
C4 Cr1 C11 105.53(7) . . ?
C9 Cr1 P1 116.92(5) . . ?
C9 Cr1 P2 46.66(5) . . ?
C9 Cr1 C10 38.45(7) . . ?
C10 Cr1 P1 104.82(5) . . ?
C10 Cr1 P2 73.02(5) . . ?
C11 Cr1 P1 120.40(5) . . ?
C11 Cr1 P2 73.63(5) . . ?
C11 Cr1 C2 154.79(7) . . ?
C11 Cr1 C3 120.86(7) . . ?
C11 Cr1 C9 66.78(7) . . ?
C11 Cr1 C10 38.41(7) . . ?
C12 Cr1 P1 155.62(5) . . ?
C12 Cr1 P2 47.07(5) . . ?
C12 Cr1 C1 155.20(8) . . ?
C12 Cr1 C2 120.10(7) . . ?
C12 Cr1 C3 104.02(7) . . ?
C12 Cr1 C4 116.44(7) . . ?
C12 Cr1 C9 72.20(7) . . ?
C12 Cr1 C10 67.34(7) . . ?
C12 Cr1 C11 39.51(7) . . ?
C1 P1 Cr1 60.44(6) . . ?
C4 P1 Cr1 60.31(6) . . ?
C4 P1 C1 88.77(9) . . ?
C9 P2 Cr1 61.04(6) . . ?
C12 P2 Cr1 59.29(6) . . ?
C12 P2 C9 88.92(9) . . ?
P1 C1 Cr1 72.80(7) . . ?
C2 C1 Cr1 70.95(10) . . ?
C2 C1 P1 113.49(14) . . ?
C2 C1 C5 123.89(18) . . ?
C5 C1 Cr1 125.50(13) . . ?
C5 C1 P1 122.61(15) . . ?
C1 C2 Cr1 70.38(11) . . ?
C1 C2 C3 112.06(16) . . ?
C1 C2 C6 124.65(17) . . ?
C3 C2 Cr1 70.60(10) . . ?
C3 C2 C6 123.09(17) . . ?
C6 C2 Cr1 130.83(13) . . ?
C2 C3 Cr1 70.67(10) . . ?
C2 C3 C4 112.63(16) . . ?
C2 C3 C7 123.77(17) . . ?
C4 C3 Cr1 70.11(10) . . ?
C4 C3 C7 123.49(16) . . ?
C7 C3 Cr1 130.31(13) . . ?
P1 C4 Cr1 72.95(7) . . ?
C3 C4 Cr1 70.95(10) . . ?
C3 C4 P1 112.88(13) . . ?
C3 C4 C8 123.95(16) . . ?
C8 C4 Cr1 130.12(13) . . ?
C8 C4 P1 122.75(14) . . ?
P2 C9 Cr1 72.30(7) . . ?
C10 C9 Cr1 70.89(11) . . ?
C10 C9 P2 112.88(14) . . ?
C10 C9 C13 124.08(17) . . ?
C13 C9 Cr1 127.16(14) . . ?
C13 C9 P2 122.97(15) . . ?
C9 C10 Cr1 70.66(11) . . ?
C9 C10 C14 123.31(18) . . ?
C11 C10 Cr1 70.04(11) . . ?
C11 C10 C9 112.99(16) . . ?
C11 C10 C14 123.57(18) . . ?
C14 C10 Cr1 130.86(13) . . ?
C10 C11 Cr1 71.55(11) . . ?
C10 C11 C12 112.17(17) . . ?
C10 C11 C15 124.19(17) . . ?
C12 C11 Cr1 68.90(10) . . ?
C12 C11 C15 123.61(18) . . ?
C15 C11 Cr1 129.03(13) . . ?
P2 C12 Cr1 73.64(7) . . ?
C11 C12 Cr1 71.59(10) . . ?
C11 C12 P2 112.78(14) . . ?
C11 C12 C16 124.07(17) . . ?
C16 C12 Cr1 129.09(13) . . ?
C16 C12 P2 122.68(14) . . ?
O1 K1 O2 59.08(4) . . ?
O1 K1 N1 61.58(4) . . ?
O1 K1 N2 117.71(4) . . ?
O2 K1 N1 119.57(4) . . ?
O2 K1 N2 59.93(4) . . ?
O3 K1 O1 119.17(4) . . ?
O3 K1 O2 99.27(4) . . ?
O3 K1 N1 118.64(4) . . ?
O3 K1 N2 60.72(4) . . ?
O4 K1 O1 97.98(4) . . ?
O4 K1 O2 137.89(4) . . ?
O4 K1 O3 59.11(4) . . ?
O4 K1 N1 60.27(4) . . ?
O4 K1 N2 119.26(4) . . ?
O5 K1 O1 97.12(4) . . ?
O5 K1 O2 117.02(4) . . ?
O5 K1 O3 138.71(4) . . ?
O5 K1 O4 99.38(4) . . ?
O5 K1 N1 60.46(4) . . ?
O5 K1 N2 120.70(4) . . ?
O6 K1 O1 135.85(4) . . ?
O6 K1 O2 95.59(4) . . ?
O6 K1 O3 98.93(4) . . ?
O6 K1 O4 121.66(4) . . ?
O6 K1 O5 60.52(4) . . ?
O6 K1 N1 120.06(4) . . ?
O6 K1 N2 61.12(4) . . ?
N1 K1 N2 178.82(5) . . ?
C18 O1 K1 115.03(11) . . ?
C19 O1 K1 113.71(11) . . ?
C19 O1 C18 111.21(15) . . ?
C20 O2 K1 115.98(11) . . ?
C21 O2 K1 116.57(12) . . ?
C21 O2 C20 111.61(15) . . ?
C24 O3 K1 118.10(11) . . ?
C25 O3 K1 114.63(10) . . ?
C25 O3 C24 110.20(15) . . ?
C26 O4 K1 118.74(10) . . ?
C27 O4 K1 120.33(10) . . ?
C27 O4 C26 112.04(14) . . ?
C30 O5 K1 118.65(11) . . ?
C30 O5 C31 111.57(14) . . ?
C31 O5 K1 115.90(10) . . ?
C32 O6 K1 113.39(10) . . ?
C32 O6 C33 111.54(14) . . ?
C33 O6 K1 118.60(11) . . ?
C17 N1 K1 108.17(11) . . ?
C28 N1 K1 109.72(11) . . ?
C28 N1 C17 109.88(15) . . ?
C28 N1 C29 108.85(15) . . ?
C29 N1 K1 110.02(11) . . ?
C29 N1 C17 110.20(15) . . ?
C22 N2 K1 110.84(12) . . ?
C22 N2 C23 109.38(16) . . ?
C22 N2 C34 110.24(16) . . ?
C23 N2 K1 108.87(11) . . ?
C23 N2 C34 109.74(16) . . ?
C34 N2 K1 107.74(11) . . ?
N1 C17 C18 113.78(16) . . ?
O1 C18 C17 110.02(16) . . ?
O1 C19 C20 109.24(16) . . ?
O2 C20 C19 109.39(16) . . ?
O2 C21 C22 109.26(17) . . ?
N2 C22 C21 113.57(17) . . ?
N2 C23 C24 114.62(17) . . ?
O3 C24 C23 109.44(17) . . ?
O3 C25 C26 109.46(15) . . ?
O4 C26 C25 109.30(16) . . ?
O4 C27 C28 108.74(15) . . ?
N1 C28 C27 114.49(16) . . ?
N1 C29 C30 113.86(15) . . ?
O5 C30 C29 108.69(15) . . ?
O5 C31 C32 108.57(15) . . ?
O6 C32 C31 109.97(15) . . ?
O6 C33 C34 109.66(16) . . ?
N2 C34 C33 113.87(17) . . ?

_olex2_exptl_crystal_mounting_method 
'From paratone on a microscope slide, onto a cryoloop.'
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.116
_oxdiff_exptl_absorpt_empirical_full_min 0.918
_chemical_properties_physical    Air-sensitive,Moisture-sensitive
####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_5
_database_code_depnum_ccdc_archive 'CCDC 2003389'
loop_
_audit_author_name
_audit_author_address
'Conrad Goodwin'
;Los Alamos National Laboratory
United States of America
;
_audit_update_record             
;
2020-05-11 deposited with the CCDC.	2020-11-30 downloaded from the CCDC.
;

_manchester_internal_coll_name   adpm457
_manchester_internal_coll_client CAPG
_manchester_internal_coll_type   custom
_manchester_internal_coll_frame_time 30s
_manchester_internal_coll_frame_width 0.8
_manchester_internal_coll_frame_method '\w scans'
_manchester_internal_coll_user   CAPG
_manchester_internal_coll_date   9/12/17
_manchester_internal_process_user CAPG
_manchester_internal_process_date 9/12/17
_manchester_internal_solution_user CAPG
_manchester_internal_solution_date 9/12/17
_manchester_internal_refinement_user CAPG
_manchester_internal_refinement_date 10/12/17
_manchester_internal_validation_user CAPG
_manchester_internal_validation_date 10/1/2020
_manchester_internal_archive_date 10/1/2020

_refine_special_details          
;
Rotational disorder was identified about the Zr-Cp axis, which manifested as a 
very clear second C5 ring. The ring was split into two parts, with both 
restrained to be idealied pentagons (AFIX 55), and then refined competetively 
against each other, converging at a ratio of 0.49(2):0.51(2). 

Global rigid bond restraints (RIGU) were applied.
;

_audit_creation_date             2017-12-10
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_shelx_SHELXL_version_number     2018/3
loop_
_audit_author_email
cgoodwin@lanl.gov
_chemical_name_common            ?
_chemical_name_systematic        ?
_chemical_formula_moiety         'C18 H22 Zr'
_chemical_formula_sum            'C18 H22 Zr'
_chemical_formula_weight         329.57
_chemical_melting_point          ?
_chemical_oxdiff_formula         Zr(C5H5)2(C4(CH3)4)
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Zr Zr -2.9673 0.5597 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_H-M_alt        'I 1 2/a 1'
_space_group_name_Hall           '-I 2ya'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x, -y+1/2, z+1/2'

_cell_length_a                   14.1554(8)
_cell_length_b                   9.6976(4)
_cell_length_c                   12.0182(6)
_cell_angle_alpha                90
_cell_angle_beta                 112.336(6)
_cell_angle_gamma                90
_cell_volume                     1525.99(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    1782
_cell_measurement_temperature    150.0(3)
_cell_measurement_theta_max      26.2880
_cell_measurement_theta_min      3.6050
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    0.705
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.775
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.30c (Rigaku Oxford Diffraction, 2017)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   ?
_exptl_crystal_colour            'clear brown'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_primary    brown
_exptl_crystal_density_diffrn    1.435
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             680
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-19 3 2 0.0672
1 13 4 0.0244
-2 -13 -4 0.0664
14 8 2 0.0288
8 -13 -5 0.0700
6 12 4 0.0188
-19 1 2 0.0728
0 2 16 0.0083
0 -2 -16 0.0297

_exptl_crystal_recrystallization_method 'From hexane.'
_exptl_crystal_size_max          0.167
_exptl_crystal_size_mid          0.118
_exptl_crystal_size_min          0.038
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
-19.0000 3.0000 2.0000 -0.1122 -0.3979 0.9238
1.0000 13.0000 4.0000 0.1820 0.8464 0.4823
-2.0000 -13.0000 -4.0000 -0.1935 -0.8779 -0.4397
14.0000 8.0000 2.0000 0.2373 0.9369 -0.2705
8.0000 -13.0000 -5.0000 -0.1409 -0.5741 -0.8596
6.0000 12.0000 4.0000 0.2457 0.9443 0.2271
-19.0000 1.0000 2.0000 -0.0999 -0.5167 0.8394
-0.0000 2.0000 16.0000 0.9898 0.2915 -0.0110
0.0000 -2.0000 -16.0000 -0.9898 -0.2915 0.0110

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0278
_diffrn_reflns_av_unetI/netI     0.0446
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -7
_diffrn_reflns_number            2872
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.386
_diffrn_reflns_theta_min         2.787
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.0(3)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.0714
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -84.00 -48.00   0.80   30.00    --  -20.40-178.00-150.00   45
  2  ω    -62.00  -2.80   0.80   30.00    --  -20.40 -37.00-180.00   74
  3  ω    -37.00  93.40   0.80   30.00    --   21.65  19.00-150.00  163
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Single source at offset/far, Eos'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0115250000
_diffrn_orient_matrix_UB_12      -0.0061626000
_diffrn_orient_matrix_UB_13      0.0626350000
_diffrn_orient_matrix_UB_21      0.0314546000
_diffrn_orient_matrix_UB_22      0.0593654000
_diffrn_orient_matrix_UB_23      0.0108000000
_diffrn_orient_matrix_UB_31      -0.0425861000
_diffrn_orient_matrix_UB_32      0.0422089000
_diffrn_orient_matrix_UB_33      -0.0059666000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_diffrn_special_details          ?
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                1401
_reflns_number_total             1558
_reflns_odcompleteness_completeness 99.88
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_collection       'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_data_reduction        'CrysAlisPro 1.171.39.30c (Rigaku OD, 2017)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXS (Sheldrick, 2008)'
_refine_diff_density_max         0.455
_refine_diff_density_min         -0.535
_refine_diff_density_rms         0.078
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.068
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     117
_refine_ls_number_reflns         1558
_refine_ls_number_restraints     144
_refine_ls_R_factor_all          0.0383
_refine_ls_R_factor_gt           0.0330
_refine_ls_restrained_S_all      1.027
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0370P)²+1.0274P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0771
_refine_ls_wR_factor_ref         0.0805

_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Sof(C6B)=Sof(H6B)=Sof(C5B)=Sof(H5B)=Sof(C9B)=Sof(H9B)=Sof(C8B)=Sof(H8B)=
 Sof(C7B)=Sof(H7B)=1-FVAR(1)
 Sof(C7A)=Sof(H7A)=Sof(C6A)=Sof(H6A)=Sof(C5A)=Sof(H5A)=Sof(C9A)=Sof(H9A)=
 Sof(C8A)=Sof(H8A)=FVAR(1)
4.a Aromatic/amide H refined with riding coordinates:
 C7A(H7A), C6A(H6A), C5A(H5A), C9A(H9A), C8A(H8A), C6B(H6B), C5B(H5B),
 C9B(H9B), C8B(H8B), C7B(H7B)
4.b Fitted pentagon refined as free rotating group:
 C7A(C6A,C5A,C9A,C8A), C6B(C5B,C9B,C8B,C7B)
4.c Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C4(H4A,H4B,H4C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
Zr1 Zr 0.250000 0.55308(4) 0.500000 0.02119(14) Uani 1 2 d S TU P . .
C1 C 0.4660(2) 0.7245(3) 0.5230(3) 0.0372(7) Uani 1 1 d . U . . .
H1A H 0.507876 0.750343 0.603918 0.056 Uiso 1 1 calc GR . . . .
H1B H 0.476997 0.788046 0.467794 0.056 Uiso 1 1 calc GR . . . .
H1C H 0.483841 0.633090 0.507265 0.056 Uiso 1 1 calc GR . . . .
C2 C 0.3548(2) 0.7278(3) 0.5072(2) 0.0255(6) Uani 1 1 d . U . . .
C3 C 0.3054(2) 0.8472(3) 0.5081(2) 0.0239(6) Uani 1 1 d . U . . .
C4 C 0.3583(2) 0.9861(3) 0.5285(3) 0.0326(7) Uani 1 1 d . U . . .
H4A H 0.330842 1.040147 0.456339 0.049 Uiso 1 1 calc GR . . . .
H4B H 0.430209 0.972906 0.549311 0.049 Uiso 1 1 calc GR . . . .
H4C H 0.347363 1.033303 0.592810 0.049 Uiso 1 1 calc GR . . . .
C7A C 0.3538(8) 0.3791(10) 0.6528(12) 0.036(3) Uani 0.492(17) 1 d . U . A 1
H7A H 0.391259 0.314127 0.629835 0.043 Uiso 0.492(17) 1 calc R . . A 1
C6A C 0.3889(6) 0.5110(12) 0.7026(11) 0.040(3) Uani 0.492(17) 1 d G U . A 1
H6A H 0.453327 0.547719 0.717888 0.048 Uiso 0.492(17) 1 calc R . . A 1
C5A C 0.3083(10) 0.5772(6) 0.7248(7) 0.035(3) Uani 0.492(17) 1 d G U . A 1
H5A H 0.310657 0.664783 0.757227 0.042 Uiso 0.492(17) 1 calc R . . A 1
C9A C 0.2234(6) 0.4861(12) 0.6888(8) 0.034(2) Uani 0.492(17) 1 d G U . A 1
H9A H 0.160414 0.503541 0.693487 0.041 Uiso 0.492(17) 1 calc R . . A 1
C8A C 0.2515(7) 0.3636(8) 0.6443(9) 0.032(2) Uani 0.492(17) 1 d G U . A 1
H8A H 0.210229 0.286823 0.614754 0.039 Uiso 0.492(17) 1 calc R . . A 1
C6B C 0.3545(8) 0.5764(6) 0.7255(7) 0.034(2) Uani 0.508(17) 1 d . U . A 2
H6B H 0.386935 0.659512 0.755539 0.040 Uiso 0.508(17) 1 calc R . . A 2
C5B C 0.2533(7) 0.5403(11) 0.7111(7) 0.034(2) Uani 0.508(17) 1 d G U . A 2
H5B H 0.207823 0.595549 0.730057 0.041 Uiso 0.508(17) 1 calc R . . A 2
C9B C 0.2337(5) 0.4049(12) 0.6626(9) 0.034(3) Uani 0.508(17) 1 d G U . A 2
H9B H 0.173127 0.355962 0.644317 0.041 Uiso 0.508(17) 1 calc R . . A 2
C8B C 0.3228(9) 0.3574(7) 0.6471(11) 0.038(3) Uani 0.508(17) 1 d G U . A 2
H8B H 0.330796 0.271853 0.616810 0.045 Uiso 0.508(17) 1 calc R . . A 2
C7B C 0.3974(5) 0.4634(11) 0.6859(11) 0.036(2) Uani 0.508(17) 1 d G U . A 2
H7B H 0.462936 0.459457 0.685548 0.044 Uiso 0.508(17) 1 calc R . . A 2


_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
Zr1 C2 2.233(3) 2_556 ?
Zr1 C2 2.233(3) . ?
Zr1 C7A 2.516(12) 2_556 ?
Zr1 C7A 2.516(12) . ?
Zr1 C6A 2.514(10) . ?
Zr1 C6A 2.514(11) 2_556 ?
Zr1 C5A 2.518(9) 2_556 ?
Zr1 C5A 2.518(7) . ?
Zr1 C9A 2.522(10) 2_556 ?
Zr1 C9A 2.522(7) . ?
Zr1 C8A 2.52(2) 2_556 ?
Zr1 C8A 2.521(10) . ?
Zr1 C6B 2.557(8) 2_556 ?
Zr1 C6B 2.557(8) . ?
Zr1 C5B 2.523(7) . ?
Zr1 C5B 2.523(6) 2_556 ?
Zr1 C9B 2.51(2) 2_556 ?
Zr1 C9B 2.506(9) . ?
Zr1 C8B 2.53(3) 2_556 ?
Zr1 C8B 2.531(12) . ?
Zr1 C7B 2.561(11) . ?
Zr1 C7B 2.561(17) 2_556 ?
C1 C2 1.513(4) . ?
C2 C3 1.355(4) . ?
C3 C3 1.506(5) 2_556 ?
C3 C4 1.515(4) . ?
C7A C6A 1.4200 . ?
C7A C8A 1.4200 . ?
C6A C5A 1.4200 . ?
C5A C9A 1.4200 . ?
C9A C8A 1.4200 . ?
C6B C5B 1.4200 . ?
C6B C7B 1.4200 . ?
C5B C9B 1.4200 . ?
C9B C8B 1.4200 . ?
C8B C7B 1.4200 . ?

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
C2 Zr1 C2 81.23(14) 2_556 . ?
C2 Zr1 C7A 106.6(3) . . ?
C2 Zr1 C7A 137.12(19) . 2_556 ?
C2 Zr1 C7A 137.12(19) 2_556 . ?
C2 Zr1 C7A 106.6(3) 2_556 2_556 ?
C2 Zr1 C6A 115.1(3) 2_556 . ?
C2 Zr1 C6A 115.1(7) . 2_556 ?
C2 Zr1 C6A 79.74(18) . . ?
C2 Zr1 C6A 79.7(6) 2_556 2_556 ?
C2 Zr1 C5A 85.0(2) 2_556 . ?
C2 Zr1 C5A 86.9(3) . . ?
C2 Zr1 C5A 86.9(6) 2_556 2_556 ?
C2 Zr1 C5A 85.0(7) . 2_556 ?
C2 Zr1 C9A 84.6(7) . 2_556 ?
C2 Zr1 C9A 119.0(3) . . ?
C2 Zr1 C9A 84.61(18) 2_556 . ?
C2 Zr1 C9A 119.0(6) 2_556 2_556 ?
C2 Zr1 C8A 134.0(6) 2_556 2_556 ?
C2 Zr1 C8A 114.3(3) 2_556 . ?
C2 Zr1 C8A 114.3(6) . 2_556 ?
C2 Zr1 C8A 134.01(19) . . ?
C2 Zr1 C6B 94.7(2) . 2_556 ?
C2 Zr1 C6B 77.50(19) 2_556 2_556 ?
C2 Zr1 C6B 94.7(2) 2_556 . ?
C2 Zr1 C6B 77.50(19) . . ?
C2 Zr1 C5B 80.46(15) 2_556 . ?
C2 Zr1 C5B 103.9(3) . . ?
C2 Zr1 C5B 80.5(7) . 2_556 ?
C2 Zr1 C5B 103.9(7) 2_556 2_556 ?
C2 Zr1 C9B 102.0(3) 2_556 . ?
C2 Zr1 C9B 102.0(6) . 2_556 ?
C2 Zr1 C9B 131.4(5) 2_556 2_556 ?
C2 Zr1 C9B 131.44(19) . . ?
C2 Zr1 C8B 117.0(5) 2_556 2_556 ?
C2 Zr1 C8B 117.0(3) . . ?
C2 Zr1 C8B 133.2(2) 2_556 . ?
C2 Zr1 C8B 133.2(5) . 2_556 ?
C2 Zr1 C7B 126.9(2) 2_556 . ?
C2 Zr1 C7B 85.1(6) 2_556 2_556 ?
C2 Zr1 C7B 126.9(6) . 2_556 ?
C2 Zr1 C7B 85.1(2) . . ?
C7A Zr1 C7A 95.7(5) . 2_556 ?
C7A Zr1 C5A 135.1(7) . 2_556 ?
C7A Zr1 C5A 54.3(9) 2_556 2_556 ?
C7A Zr1 C5A 135.1(3) 2_556 . ?
C7A Zr1 C5A 54.32(16) . . ?
C7A Zr1 C9A 103.8(7) . 2_556 ?
C7A Zr1 C9A 54.3(8) 2_556 2_556 ?
C7A Zr1 C9A 103.8(3) 2_556 . ?
C7A Zr1 C9A 54.27(15) . . ?
C7A Zr1 C8A 32.8(6) 2_556 2_556 ?
C7A Zr1 C8A 82.1(3) 2_556 . ?
C7A Zr1 C8A 82.1(5) . 2_556 ?
C7A Zr1 C8A 32.75(13) . . ?
C7A Zr1 C6B 49.0(2) 2_556 2_556 ?
C7A Zr1 C6B 140.8(2) . 2_556 ?
C7A Zr1 C5B 118.9(8) . 2_556 ?
C7A Zr1 C5B 56.7(7) 2_556 2_556 ?
C7A Zr1 C8B 88.7(4) . 2_556 ?
C7A Zr1 C8B 10.6(5) 2_556 2_556 ?
C7A Zr1 C7B 117.7(7) . 2_556 ?
C7A Zr1 C7B 22.9(7) 2_556 2_556 ?
C6A Zr1 C7A 32.8(8) 2_556 2_556 ?
C6A Zr1 C7A 32.80(14) . . ?
C6A Zr1 C7A 128.5(6) 2_556 . ?
C6A Zr1 C7A 128.5(5) . 2_556 ?
C6A Zr1 C6A 161.3(7) . 2_556 ?
C6A Zr1 C5A 32.8(3) 2_556 2_556 ?
C6A Zr1 C5A 150.6(8) . 2_556 ?
C6A Zr1 C5A 32.78(10) . . ?
C6A Zr1 C5A 150.6(8) 2_556 . ?
C6A Zr1 C9A 120.0(9) . 2_556 ?
C6A Zr1 C9A 120.0(8) 2_556 . ?
C6A Zr1 C9A 54.3(2) 2_556 2_556 ?
C6A Zr1 C9A 54.29(13) . . ?
C6A Zr1 C8A 54.3(6) 2_556 2_556 ?
C6A Zr1 C8A 110.3(6) 2_556 . ?
C6A Zr1 C8A 110.3(8) . 2_556 ?
C6A Zr1 C8A 54.31(18) . . ?
C6A Zr1 C6B 164.9(2) . 2_556 ?
C6A Zr1 C6B 20.5(8) 2_556 2_556 ?
C6A Zr1 C5B 132.4(7) . 2_556 ?
C6A Zr1 C5B 46.3(12) 2_556 2_556 ?
C6A Zr1 C8B 40.6(9) 2_556 2_556 ?
C6A Zr1 C8B 121.1(5) . 2_556 ?
C6A Zr1 C7B 150.2(6) . 2_556 ?
C6A Zr1 C7B 12.1(11) 2_556 2_556 ?
C5A Zr1 C5A 169.3(7) 2_556 . ?
C5A Zr1 C9A 32.7(3) 2_556 2_556 ?
C5A Zr1 C9A 152.8(9) . 2_556 ?
C5A Zr1 C9A 32.73(8) . . ?
C5A Zr1 C9A 152.8(8) 2_556 . ?
C5A Zr1 C8A 54.26(13) . . ?
C5A Zr1 C8A 136.0(4) . 2_556 ?
C5A Zr1 C8A 136.0(6) 2_556 . ?
C5A Zr1 C8A 54.3(5) 2_556 2_556 ?
C5A Zr1 C6B 161.95(17) . 2_556 ?
C5A Zr1 C6B 14.7(8) 2_556 2_556 ?
C5A Zr1 C5B 18.6(11) 2_556 2_556 ?
C5A Zr1 C5B 163.1(8) . 2_556 ?
C5A Zr1 C8B 134.4(4) . 2_556 ?
C5A Zr1 C8B 55.9(9) 2_556 2_556 ?
C5A Zr1 C7B 43.1(12) 2_556 2_556 ?
C5A Zr1 C7B 142.5(8) . 2_556 ?
C9A Zr1 C9A 150.1(7) 2_556 . ?
C9A Zr1 C6B 45.0(8) 2_556 2_556 ?
C9A Zr1 C6B 138.79(19) . 2_556 ?
C9A Zr1 C5B 160.0(8) . 2_556 ?
C9A Zr1 C5B 15.1(10) 2_556 2_556 ?
C9A Zr1 C8B 48.6(10) 2_556 2_556 ?
C9A Zr1 C8B 106.0(7) . 2_556 ?
C9A Zr1 C7B 110.3(8) . 2_556 ?
C9A Zr1 C7B 58.6(10) 2_556 2_556 ?
C8A Zr1 C9A 117.8(5) 2_556 . ?
C8A Zr1 C9A 32.71(9) . . ?
C8A Zr1 C9A 117.8(6) . 2_556 ?
C8A Zr1 C9A 32.7(4) 2_556 2_556 ?
C8A Zr1 C8A 86.4(3) 2_556 . ?
C8A Zr1 C6B 130.1(2) . 2_556 ?
C8A Zr1 C6B 59.0(5) 2_556 2_556 ?
C8A Zr1 C5B 130.4(8) . 2_556 ?
C8A Zr1 C5B 44.0(9) 2_556 2_556 ?
C8A Zr1 C8B 80.1(4) . 2_556 ?
C8A Zr1 C8B 22.8(8) 2_556 2_556 ?
C8A Zr1 C7B 98.3(7) . 2_556 ?
C8A Zr1 C7B 50.3(9) 2_556 2_556 ?
C6B Zr1 C6B 169.8(3) 2_556 . ?
C6B Zr1 C7B 155.0(7) . 2_556 ?
C6B Zr1 C7B 32.22(11) . . ?
C6B Zr1 C7B 154.98(16) 2_556 . ?
C6B Zr1 C7B 32.2(7) 2_556 2_556 ?
C5B Zr1 C6B 148.5(8) 2_556 . ?
C5B Zr1 C6B 32.46(8) . . ?
C5B Zr1 C5B 174.4(7) 2_556 . ?
C5B Zr1 C8B 54.09(15) . . ?
C5B Zr1 C8B 120.8(6) 2_556 . ?
C5B Zr1 C7B 53.7(4) 2_556 2_556 ?
C5B Zr1 C7B 123.9(8) . 2_556 ?
C5B Zr1 C7B 123.9(8) 2_556 . ?
C5B Zr1 C7B 53.73(13) . . ?
C9B Zr1 C6B 133.6(7) 2_556 . ?
C9B Zr1 C6B 53.96(12) . . ?
C9B Zr1 C5B 32.80(9) . . ?
C9B Zr1 C5B 141.6(4) 2_556 . ?
C9B Zr1 C8B 32.74(13) . . ?
C9B Zr1 C8B 88.9(4) 2_556 . ?
C9B Zr1 C7B 101.5(7) 2_556 . ?
C9B Zr1 C7B 101.5(7) . 2_556 ?
C9B Zr1 C7B 53.91(18) . . ?
C9B Zr1 C7B 53.9(5) 2_556 2_556 ?
C8B Zr1 C6B 53.70(16) . . ?
C8B Zr1 C6B 136.5(3) 2_556 . ?
C8B Zr1 C8B 82.8(3) 2_556 . ?
C8B Zr1 C7B 32.4(5) 2_556 2_556 ?
C8B Zr1 C7B 109.6(5) 2_556 . ?
C8B Zr1 C7B 109.6(5) . 2_556 ?
C8B Zr1 C7B 32.38(14) . . ?
C7B Zr1 C7B 140.3(6) . 2_556 ?
C1 C2 Zr1 129.3(2) . . ?
C3 C2 Zr1 108.14(19) . . ?
C3 C2 C1 122.2(3) . . ?
C2 C3 C3 120.99(16) . 2_556 ?
C2 C3 C4 122.4(3) . . ?
C3 C3 C4 116.57(17) 2_556 . ?
C6A C7A Zr1 73.5(3) . . ?
C6A C7A C8A 108.0 . . ?
C8A C7A Zr1 73.8(3) . . ?
C7A C6A Zr1 73.7(3) . . ?
C5A C6A Zr1 73.8(3) . . ?
C5A C6A C7A 108.0 . . ?
C6A C5A Zr1 73.5(4) . . ?
C6A C5A C9A 108.0 . . ?
C9A C5A Zr1 73.8(3) . . ?
C5A C9A Zr1 73.5(3) . . ?
C8A C9A Zr1 73.6(4) . . ?
C8A C9A C5A 108.0 . . ?
C7A C8A Zr1 73.4(3) . . ?
C9A C8A Zr1 73.7(3) . . ?
C9A C8A C7A 108.0 . . ?
C5B C6B Zr1 72.5(3) . . ?
C7B C6B Zr1 74.1(4) . . ?
C7B C6B C5B 108.0 . . ?
C6B C5B Zr1 75.1(3) . . ?
C9B C5B Zr1 73.0(3) . . ?
C9B C5B C6B 108.0 . . ?
C5B C9B Zr1 74.2(3) . . ?
C5B C9B C8B 108.0 . . ?
C8B C9B Zr1 74.6(4) . . ?
C9B C8B Zr1 72.7(3) . . ?
C7B C8B Zr1 75.0(3) . . ?
C7B C8B C9B 108.0 . . ?
C6B C7B Zr1 73.7(3) . . ?
C8B C7B Zr1 72.6(3) . . ?
C8B C7B C6B 108.0 . . ?

_olex2_date_sample_completion    2017-12-09
_olex2_date_sample_data_collection 2017-12-09
_olex2_date_sample_submission    2017-12-09
_olex2_exptl_crystal_mounting_method 'From fomblin on a microscope slide.'
_olex2_submission_original_sample_id adpm457
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details 
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.780
_oxdiff_exptl_absorpt_empirical_full_min 0.658
