# Electronic Supplementary Material (ESI) for Catalysis Science & Technology.
# This journal is © The Royal Society of Chemistry 2022

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

data_3
_database_code_depnum_ccdc_archive 'CCDC 2108180'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2021-09-07 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H54 Cl6 Cr2 N10 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C24 H58 Cl10 Cr2 N10 P4'
_chemical_formula_weight         1069.18

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   11.9522(3)
_cell_length_b                   13.5271(4)
_cell_length_c                   14.8191(5)
_cell_angle_alpha                90
_cell_angle_beta                 104.592(3)
_cell_angle_gamma                90
_cell_volume                     2318.65(12)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2781
_cell_measurement_theta_min      2.7130
_cell_measurement_theta_max      28.1530

_exptl_crystal_description       blocks
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.531
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.31
_exptl_crystal_size_min          0.26
_exptl_absorpt_coefficient_mu    1.215
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.724
_exptl_absorpt_correction_T_max  0.775
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            8072
_diffrn_reflns_av_unetI/netI     0.0486
_diffrn_reflns_av_R_equivalents  0.0281
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_theta_min         2.475
_diffrn_reflns_theta_max         28.186
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.817
_diffrn_measured_fraction_theta_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.817
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.817
_diffrn_reflns_point_group_measured_fraction_full 0.988
_reflns_number_total             4651
_reflns_number_gt                3858
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0378P)²+2.3883P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         4651
_refine_ls_number_parameters     258
_refine_ls_number_restraints     64
_refine_ls_R_factor_all          0.0534
_refine_ls_R_factor_gt           0.0410
_refine_ls_wR_factor_ref         0.1015
_refine_ls_wR_factor_gt          0.0929
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_restrained_S_all      1.085
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.15125(4) 0.52552(3) 0.02208(3) 0.01900(13) Uani 1 1 d . . . . .
Cl1 Cl 0.20279(7) 0.39152(6) -0.05612(6) 0.0370(2) Uani 1 1 d . . . . .
Cl2 Cl 0.24770(7) 0.63347(6) -0.04979(5) 0.0338(2) Uani 1 1 d . . . . .
Cl3 Cl 0.02938(6) 0.42166(5) 0.08371(5) 0.02576(17) Uani 1 1 d . . . . .
P1 P 0.15526(6) 0.64714(5) 0.15060(5) 0.02092(17) Uani 1 1 d . . . . .
N2 N 0.28866(19) 0.60577(17) 0.20952(16) 0.0220(5) Uani 1 1 d . . . . .
P3 P 0.32120(6) 0.50829(6) 0.15040(5) 0.02194(17) Uani 1 1 d . . . . .
N4 N 0.1522(2) 0.76846(18) 0.13600(18) 0.0315(6) Uani 1 1 d . . . . .
C5 C 0.1020(3) 0.8222(3) 0.2026(2) 0.0413(8) Uani 1 1 d . . . . .
H5A H 0.057626 0.880323 0.172500 0.050 Uiso 1 1 calc R U . . .
H5B H 0.163486 0.844975 0.256708 0.050 Uiso 1 1 calc R U . . .
C6 C 0.0241(3) 0.7495(3) 0.2328(2) 0.0416(9) Uani 1 1 d . . . . .
H6A H 0.017972 0.764408 0.296813 0.050 Uiso 1 1 calc R U . . .
H6B H -0.054289 0.751107 0.190075 0.050 Uiso 1 1 calc R U . . .
N7 N 0.0781(2) 0.65309(19) 0.22957(17) 0.0306(6) Uani 1 1 d . . . . .
C8 C 0.2278(3) 0.8245(2) 0.0929(3) 0.0475(9) Uani 1 1 d . . . . .
H8A H 0.286017 0.858748 0.141171 0.071 Uiso 1 1 calc R U . . .
H8B H 0.182249 0.873151 0.049877 0.071 Uiso 1 1 calc R U . . .
H8C H 0.266244 0.779612 0.058376 0.071 Uiso 1 1 calc R U . . .
C9 C 0.0310(3) 0.5698(3) 0.2686(2) 0.0424(9) Uani 1 1 d . . . . .
H9A H -0.049430 0.559231 0.233923 0.064 Uiso 1 1 calc R U . . .
H9B H 0.034002 0.583155 0.334210 0.064 Uiso 1 1 calc R U . . .
H9C H 0.076512 0.510533 0.264318 0.064 Uiso 1 1 calc R U . . .
C10 C 0.3629(3) 0.6483(2) 0.2958(2) 0.0303(7) Uani 1 1 d . . . . .
H10A H 0.339923 0.718039 0.300838 0.036 Uiso 1 1 calc R U . . .
H10B H 0.443893 0.648300 0.290669 0.036 Uiso 1 1 calc R U . . .
C11 C 0.3581(3) 0.5951(3) 0.3840(2) 0.0431(9) Uani 1 1 d . . . . .
H11A H 0.372284 0.523773 0.377018 0.052 Uiso 1 1 calc R U . . .
H11B H 0.279969 0.602603 0.394457 0.052 Uiso 1 1 calc R U . . .
C12 C 0.4478(4) 0.6355(3) 0.4683(3) 0.0583(12) Uani 1 1 d . . . . .
H12A H 0.525351 0.627645 0.458345 0.087 Uiso 1 1 calc R U . . .
H12B H 0.442922 0.599062 0.524313 0.087 Uiso 1 1 calc R U . . .
H12C H 0.432761 0.705777 0.476312 0.087 Uiso 1 1 calc R U . . .
N13 N 0.3491(2) 0.40634(19) 0.21523(18) 0.0335(6) Uani 1 1 d . . . . .
C14 C 0.4644(3) 0.3726(3) 0.2323(4) 0.0662(13) Uani 1 1 d . . . . .
H14A H 0.465398 0.302733 0.212550 0.079 Uiso 1 1 calc R U . . .
H14B H 0.502165 0.376482 0.299816 0.079 Uiso 1 1 calc R U . . .
C15 C 0.5276(3) 0.4341(3) 0.1800(3) 0.0547(11) Uani 1 1 d . . . . .
H15A H 0.601885 0.456220 0.221471 0.066 Uiso 1 1 calc R U . . .
H15B H 0.544376 0.395642 0.128103 0.066 Uiso 1 1 calc R U . . .
N16 N 0.4568(2) 0.5183(2) 0.14395(19) 0.0329(6) Uani 1 1 d . . . . .
C17 C 0.2697(3) 0.3578(2) 0.2599(2) 0.0404(8) Uani 1 1 d . . . . .
H17A H 0.293688 0.369837 0.327194 0.061 Uiso 1 1 calc R U . . .
H17B H 0.269932 0.286526 0.247969 0.061 Uiso 1 1 calc R U . . .
H17C H 0.191642 0.384027 0.234694 0.061 Uiso 1 1 calc R U . . .
C18 C 0.5058(3) 0.5996(3) 0.1039(3) 0.0513(10) Uani 1 1 d . . . . .
H18A H 0.521235 0.578592 0.044910 0.077 Uiso 1 1 calc R U . . .
H18B H 0.578192 0.620464 0.147175 0.077 Uiso 1 1 calc R U . . .
H18C H 0.451180 0.655003 0.092380 0.077 Uiso 1 1 calc R U . . .
C20 C 0.8068(10) 0.6674(6) 0.4347(7) 0.080(3) Uani 0.691(3) 1 d D U P A 1
H20A H 0.879033 0.688119 0.418988 0.096 Uiso 0.691(3) 1 calc R U P A 1
H20B H 0.768173 0.727335 0.450592 0.096 Uiso 0.691(3) 1 calc R U P A 1
Cl4 Cl 0.8391(3) 0.58944(17) 0.52874(15) 0.1146(11) Uani 0.691(3) 1 d D U P A 1
Cl5 Cl 0.7163(3) 0.60894(14) 0.33877(15) 0.0833(8) Uani 0.691(3) 1 d D U P A 1
C20' C 0.847(3) 0.6629(18) 0.4488(17) 0.061(7) Uiso 0.171(3) 1 d D U P B 2
H20C H 0.892917 0.722650 0.443833 0.073 Uiso 0.171(3) 1 calc R U P B 2
H20D H 0.790988 0.678302 0.485826 0.073 Uiso 0.171(3) 1 calc R U P B 2
Cl4' Cl 0.9330(8) 0.5659(7) 0.4942(5) 0.071(2) Uiso 0.171(3) 1 d D U P B 2
Cl5' Cl 0.7787(6) 0.6155(5) 0.3393(5) 0.0458(17) Uiso 0.171(3) 1 d D U P B 2
C20" C 0.821(2) 0.693(2) 0.441(4) 0.074(9) Uiso 0.138(3) 1 d D U P C 3
H20E H 0.812545 0.747734 0.483183 0.089 Uiso 0.138(3) 1 calc R U P C 3
H20F H 0.852861 0.717362 0.390357 0.089 Uiso 0.138(3) 1 calc R U P C 3
Cl4" Cl 0.9002(9) 0.5962(8) 0.5011(7) 0.059(3) Uiso 0.138(3) 1 d D U P C 3
Cl5" Cl 0.6940(11) 0.6290(12) 0.4008(12) 0.121(4) Uiso 0.138(3) 1 d D U P C 3


_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 Cl2 2.2835(8) . ?
Cr1 Cl1 2.3168(8) . ?
Cr1 Cl3 2.3664(8) . ?
Cr1 P3 2.4187(8) . ?
Cr1 Cl3 2.4339(8) 3_565 ?
Cr1 P1 2.5080(8) . ?
P1 N4 1.654(3) . ?
P1 N7 1.664(2) . ?
P1 N2 1.708(2) . ?
N2 C10 1.478(3) . ?
N2 P3 1.682(2) . ?
P3 N16 1.653(3) . ?
P3 N13 1.666(3) . ?
N4 C8 1.446(4) . ?
N4 C5 1.470(4) . ?
C5 C6 1.499(5) . ?
C6 N7 1.461(4) . ?
N7 C9 1.444(4) . ?
C10 C11 1.505(4) . ?
C11 C12 1.528(5) . ?
N13 C14 1.413(4) . ?
N13 C17 1.444(4) . ?
C14 C15 1.469(6) . ?
C15 N16 1.439(4) . ?
N16 C18 1.442(4) . ?
C20 Cl4 1.712(9) . ?
C20 Cl5 1.744(8) . ?
C20' Cl4' 1.697(16) . ?
C20' Cl5' 1.744(16) . ?
Cl4' Cl4' 2.37(2) 3_766 ?
C20" Cl5" 1.714(16) . ?
C20" Cl4" 1.719(16) . ?

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
Cl2 Cr1 Cl1 92.17(3) . . ?
Cl2 Cr1 Cl3 172.68(3) . . ?
Cl1 Cr1 Cl3 89.75(3) . . ?
Cl2 Cr1 P3 90.32(3) . . ?
Cl1 Cr1 P3 92.37(3) . . ?
Cl3 Cr1 P3 96.66(3) . . ?
Cl2 Cr1 Cl3 88.97(3) . 3_565 ?
Cl1 Cr1 Cl3 102.24(3) . 3_565 ?
Cl3 Cr1 Cl3 83.72(3) . 3_565 ?
P3 Cr1 Cl3 165.39(3) . 3_565 ?
Cl2 Cr1 P1 91.11(3) . . ?
Cl1 Cr1 P1 159.46(3) . . ?
Cl3 Cr1 P1 89.55(3) . . ?
P3 Cr1 P1 67.33(3) . . ?
Cl3 Cr1 P1 98.09(3) 3_565 . ?
Cr1 Cl3 Cr1 96.28(3) . 3_565 ?
N4 P1 N7 92.63(13) . . ?
N4 P1 N2 112.27(13) . . ?
N7 P1 N2 105.52(12) . . ?
N4 P1 Cr1 123.77(10) . . ?
N7 P1 Cr1 131.13(10) . . ?
N2 P1 Cr1 90.58(8) . . ?
C10 N2 P3 126.10(19) . . ?
C10 N2 P1 126.49(19) . . ?
P3 N2 P1 107.41(13) . . ?
N16 P3 N13 92.57(13) . . ?
N16 P3 N2 108.94(13) . . ?
N13 P3 N2 112.79(13) . . ?
N16 P3 Cr1 126.03(10) . . ?
N13 P3 Cr1 122.65(10) . . ?
N2 P3 Cr1 94.32(8) . . ?
C8 N4 C5 116.3(3) . . ?
C8 N4 P1 125.6(2) . . ?
C5 N4 P1 113.7(2) . . ?
N4 C5 C6 105.4(3) . . ?
N7 C6 C5 105.2(3) . . ?
C9 N7 C6 117.6(3) . . ?
C9 N7 P1 125.8(2) . . ?
C6 N7 P1 113.2(2) . . ?
N2 C10 C11 114.8(3) . . ?
C10 C11 C12 111.5(3) . . ?
C14 N13 C17 119.7(3) . . ?
C14 N13 P3 114.5(2) . . ?
C17 N13 P3 125.6(2) . . ?
N13 C14 C15 109.3(3) . . ?
N16 C15 C14 108.2(3) . . ?
C15 N16 C18 119.6(3) . . ?
C15 N16 P3 114.0(2) . . ?
C18 N16 P3 126.3(2) . . ?
Cl4 C20 Cl5 110.5(5) . . ?
Cl4' C20' Cl5' 100.4(11) . . ?
C20' Cl4' Cl4' 159.9(15) . 3_766 ?
Cl5" C20" Cl4" 97.2(12) . . ?

_refine_diff_density_max         0.522
_refine_diff_density_min         -0.621
_refine_diff_density_rms         0.083

####################################################################### 
# 
# 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 2115885'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2021-10-15 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2017/1
_shelx_SHELXL_version_number     2017/1
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C32 H72 Cr2 Li4 O4'
_chemical_formula_sum            'C32 H72 Cr2 Li4 O4'
_chemical_formula_weight         652.65

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'
Li Li -0.0003 0.0001 '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'

_space_group_crystal_system      orthorhombic
_space_group_IT_number           56
_space_group_name_H-M_alt        'P c c n'
_space_group_name_Hall           '-P 2ab 2ac'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y+1/2, z'
'-x, y+1/2, -z+1/2'
'x+1/2, -y, -z+1/2'
'-x, -y, -z'
'x-1/2, y-1/2, -z'
'x, -y-1/2, z-1/2'
'-x-1/2, y, z-1/2'

_cell_length_a                   9.9307(3)
_cell_length_b                   17.6625(6)
_cell_length_c                   22.0161(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3861.7(3)
_cell_formula_units_Z            4
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    2171
_cell_measurement_theta_min      2.6080
_cell_measurement_theta_max      26.9890

_exptl_crystal_description       blocks
_exptl_crystal_colour            Brown
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_F_000             1424
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.496
_exptl_crystal_size_mid          0.354
_exptl_crystal_size_min          0.333
_exptl_absorpt_coefficient_mu    0.592
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.810
_exptl_absorpt_correction_T_max  0.843
_exptl_absorpt_process_details   
; 
CrysAlisPro 1.171.38.43 (Rigaku Oxford Diffraction, 2015) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            8880
_diffrn_reflns_av_unetI/netI     0.0441
_diffrn_reflns_av_R_equivalents  0.0269
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_theta_min         2.353
_diffrn_reflns_theta_max         28.227
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.827
_diffrn_measured_fraction_theta_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.827
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.827
_diffrn_reflns_point_group_measured_fraction_full 0.991
_reflns_number_total             3948
_reflns_number_gt                2610
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'CrysAlisPro, Rigaku OD'
_computing_cell_refinement       'CrysAlisPro, Rigaku OD'
_computing_data_reduction        'CrysAlisPro, Rigaku OD'
_computing_structure_solution    'SHELXS-2014 (Sheldrick, 2017)'
_computing_structure_refinement  'SHELXL-2017/1 (Sheldrick, 2017)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0726P)²+3.9936P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       .
_refine_ls_number_reflns         3948
_refine_ls_number_parameters     250
_refine_ls_number_restraints     205
_refine_ls_R_factor_all          0.0981
_refine_ls_R_factor_gt           0.0619
_refine_ls_wR_factor_ref         0.1775
_refine_ls_wR_factor_gt          0.1525
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.099
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.31212(5) 0.20755(3) 0.36521(2) 0.0382(2) Uani 1 1 d . . . . .
Li1 Li 0.3951(7) 0.3049(4) 0.4402(3) 0.0595(17) Uani 1 1 d . . . . .
Li2 Li 0.1247(7) 0.1804(4) 0.2900(3) 0.0607(17) Uani 1 1 d . . . . .
C1 C 0.5202(3) 0.2505(2) 0.36099(17) 0.0490(9) Uani 1 1 d D . . . .
H1A H 0.527487 0.296846 0.335868 0.059 Uiso 0.640(14) 1 calc R U P A 1
H1B H 0.558051 0.260151 0.401864 0.059 Uiso 0.640(14) 1 calc R U P A 1
H1C H 0.519931 0.306324 0.356619 0.059 Uiso 0.360(14) 1 calc R U P A 2
H1D H 0.569200 0.237358 0.398690 0.059 Uiso 0.360(14) 1 calc R U P A 2
C2 C 0.5844(6) 0.1826(4) 0.3306(4) 0.056(2) Uani 0.640(14) 1 d D U P A 1
H2A H 0.569156 0.136438 0.355135 0.067 Uiso 0.640(14) 1 calc R U P A 1
H2B H 0.682686 0.190454 0.326274 0.067 Uiso 0.640(14) 1 calc R U P A 1
C3 C 0.5181(7) 0.1746(6) 0.2679(3) 0.062(2) Uani 0.640(14) 1 d D U P A 1
H3A H 0.544540 0.125428 0.250001 0.074 Uiso 0.640(14) 1 calc R U P A 1
H3B H 0.552228 0.215195 0.240967 0.074 Uiso 0.640(14) 1 calc R U P A 1
C2' C 0.5899(12) 0.2133(8) 0.3051(6) 0.054(3) Uiso 0.360(14) 1 d D U P A 2
H2'A H 0.601168 0.251270 0.272412 0.065 Uiso 0.360(14) 1 calc R U P A 2
H2'B H 0.680172 0.194541 0.316777 0.065 Uiso 0.360(14) 1 calc R U P A 2
C3' C 0.5035(12) 0.1473(8) 0.2821(8) 0.059(4) Uiso 0.360(14) 1 d D U P A 2
H3'A H 0.541687 0.126288 0.244105 0.071 Uiso 0.360(14) 1 calc R U P A 2
H3'B H 0.499633 0.106453 0.312831 0.071 Uiso 0.360(14) 1 calc R U P A 2
C4 C 0.3637(4) 0.1792(2) 0.27060(17) 0.0517(9) Uani 1 1 d D . . . .
H4A H 0.323088 0.130151 0.258923 0.062 Uiso 0.640(14) 1 calc R U P A 1
H4B H 0.330058 0.218838 0.242614 0.062 Uiso 0.640(14) 1 calc R U P A 1
H4C H 0.301851 0.140993 0.253180 0.062 Uiso 0.360(14) 1 calc R U P A 2
H4D H 0.365925 0.224580 0.244182 0.062 Uiso 0.360(14) 1 calc R U P A 2
C5 C 0.3509(4) 0.1739(2) 0.46031(17) 0.0494(9) Uani 1 1 d D . . . .
H5A H 0.443430 0.188184 0.472535 0.059 Uiso 0.563(15) 1 calc R U P B 1
H5B H 0.286249 0.198890 0.488024 0.059 Uiso 0.563(15) 1 calc R U P B 1
H5C H 0.427793 0.201644 0.478306 0.059 Uiso 0.437(15) 1 calc R U P B 2
H5D H 0.270324 0.179619 0.486361 0.059 Uiso 0.437(15) 1 calc R U P B 2
C6 C 0.3329(13) 0.0854(4) 0.4625(4) 0.060(3) Uani 0.563(15) 1 d D U P B 1
H6A H 0.417017 0.062165 0.477776 0.072 Uiso 0.563(15) 1 calc R U P B 1
H6B H 0.259875 0.072796 0.491336 0.072 Uiso 0.563(15) 1 calc R U P B 1
C7 C 0.2999(9) 0.0520(3) 0.4014(4) 0.052(2) Uani 0.563(15) 1 d D U P B 1
H7A H 0.382720 0.048706 0.376504 0.062 Uiso 0.563(15) 1 calc R U P B 1
H7B H 0.263695 0.000226 0.406652 0.062 Uiso 0.563(15) 1 calc R U P B 1
C6' C 0.3842(11) 0.0915(6) 0.4477(6) 0.055(3) Uiso 0.437(15) 1 d D U P B 2
H6'A H 0.455619 0.087268 0.416456 0.066 Uiso 0.437(15) 1 calc R U P B 2
H6'B H 0.414905 0.065699 0.485118 0.066 Uiso 0.437(15) 1 calc R U P B 2
C7' C 0.2551(12) 0.0577(7) 0.4253(6) 0.060(3) Uiso 0.437(15) 1 d D U P B 2
H7'A H 0.187846 0.058742 0.458432 0.072 Uiso 0.437(15) 1 calc R U P B 2
H7'B H 0.270816 0.004107 0.414144 0.072 Uiso 0.437(15) 1 calc R U P B 2
C8 C 0.1975(4) 0.1005(2) 0.36931(18) 0.0513(9) Uani 1 1 d D . . . .
H8A H 0.113581 0.105857 0.393194 0.062 Uiso 0.563(15) 1 calc R U P B 1
H8B H 0.176006 0.080869 0.328322 0.062 Uiso 0.563(15) 1 calc R U P B 1
H8C H 0.100136 0.110587 0.374571 0.062 Uiso 0.437(15) 1 calc R U P B 2
H8D H 0.210677 0.070623 0.331731 0.062 Uiso 0.437(15) 1 calc R U P B 2
O10 O 0.5159(7) 0.3498(6) 0.5015(3) 0.0629(16) Uani 0.835(9) 1 d D U P C 1
C11 C 0.6256(10) 0.3968(6) 0.4847(6) 0.109(3) Uani 0.835(9) 1 d D U P C 1
H11A H 0.608973 0.414130 0.442613 0.131 Uiso 0.835(9) 1 calc R U P C 1
H11B H 0.622419 0.442242 0.510972 0.131 Uiso 0.835(9) 1 calc R U P C 1
C12 C 0.7532(8) 0.3697(5) 0.4868(5) 0.138(4) Uani 0.835(9) 1 d D U P C 1
H12A H 0.816044 0.409279 0.473779 0.206 Uiso 0.835(9) 1 calc R U P C 1
H12B H 0.774689 0.354224 0.528413 0.206 Uiso 0.835(9) 1 calc R U P C 1
H12C H 0.761160 0.325936 0.459627 0.206 Uiso 0.835(9) 1 calc R U P C 1
C13 C 0.4989(10) 0.3364(6) 0.5655(3) 0.100(2) Uani 0.835(9) 1 d D U P C 1
H13A H 0.430083 0.296316 0.570505 0.120 Uiso 0.835(9) 1 calc R U P C 1
H13B H 0.584769 0.315962 0.581483 0.120 Uiso 0.835(9) 1 calc R U P C 1
C14 C 0.4621(9) 0.3968(5) 0.6016(3) 0.120(3) Uani 0.835(9) 1 d D U P C 1
H14A H 0.454110 0.379930 0.643851 0.180 Uiso 0.835(9) 1 calc R U P C 1
H14B H 0.530677 0.436500 0.598781 0.180 Uiso 0.835(9) 1 calc R U P C 1
H14C H 0.375306 0.416767 0.587754 0.180 Uiso 0.835(9) 1 calc R U P C 1
O10' O 0.530(5) 0.343(4) 0.4965(16) 0.082(7) Uiso 0.165(9) 1 d D U P C 2
C11' C 0.605(6) 0.410(2) 0.482(3) 0.087(8) Uiso 0.165(9) 1 d D U P C 2
H11C H 0.541014 0.447658 0.465871 0.105 Uiso 0.165(9) 1 calc R U P C 2
H11D H 0.639979 0.430682 0.521124 0.105 Uiso 0.165(9) 1 calc R U P C 2
C12' C 0.711(4) 0.405(2) 0.4428(19) 0.107(7) Uiso 0.165(9) 1 d D U P C 2
H12D H 0.752264 0.454631 0.437603 0.160 Uiso 0.165(9) 1 calc R U P C 2
H12E H 0.777978 0.369223 0.458918 0.160 Uiso 0.165(9) 1 calc R U P C 2
H12F H 0.678516 0.386284 0.403388 0.160 Uiso 0.165(9) 1 calc R U P C 2
C13' C 0.537(4) 0.318(3) 0.558(2) 0.085(7) Uiso 0.165(9) 1 d D U P C 2
H13C H 0.548898 0.262598 0.558081 0.102 Uiso 0.165(9) 1 calc R U P C 2
H13D H 0.619864 0.340164 0.576268 0.102 Uiso 0.165(9) 1 calc R U P C 2
C14' C 0.432(4) 0.335(3) 0.5968(18) 0.118(7) Uiso 0.165(9) 1 d D U P C 2
H14D H 0.451796 0.314211 0.637217 0.177 Uiso 0.165(9) 1 calc R U P C 2
H14E H 0.420804 0.389593 0.599389 0.177 Uiso 0.165(9) 1 calc R U P C 2
H14F H 0.349460 0.311613 0.581104 0.177 Uiso 0.165(9) 1 calc R U P C 2
O20 O 0.0215(7) 0.1250(4) 0.2261(3) 0.0631(17) Uani 0.686(7) 1 d D U P D 1
C21 C -0.1091(8) 0.0983(6) 0.2270(4) 0.105(3) Uani 0.686(7) 1 d D U P D 1
H21A H -0.126526 0.070481 0.188790 0.125 Uiso 0.686(7) 1 calc R U P D 1
H21B H -0.171353 0.142060 0.228298 0.125 Uiso 0.686(7) 1 calc R U P D 1
C22 C -0.1410(9) 0.0459(4) 0.2807(4) 0.089(2) Uani 0.686(7) 1 d D U P D 1
H22A H -0.235087 0.029426 0.278263 0.134 Uiso 0.686(7) 1 calc R U P D 1
H22B H -0.081739 0.001609 0.279336 0.134 Uiso 0.686(7) 1 calc R U P D 1
H22C H -0.126636 0.073299 0.318906 0.134 Uiso 0.686(7) 1 calc R U P D 1
C23 C 0.0430(11) 0.1472(6) 0.1651(4) 0.124(4) Uani 0.686(7) 1 d D U P D 1
H23A H -0.043840 0.165545 0.148619 0.149 Uiso 0.686(7) 1 calc R U P D 1
H23B H 0.105594 0.190871 0.165325 0.149 Uiso 0.686(7) 1 calc R U P D 1
C24 C 0.0946(13) 0.0929(8) 0.1242(4) 0.144(4) Uani 0.686(7) 1 d D U P D 1
H24A H 0.104496 0.115814 0.083865 0.216 Uiso 0.686(7) 1 calc R U P D 1
H24B H 0.182654 0.075349 0.138518 0.216 Uiso 0.686(7) 1 calc R U P D 1
H24C H 0.032530 0.049906 0.121735 0.216 Uiso 0.686(7) 1 calc R U P D 1
O20' O 0.0489(16) 0.1110(10) 0.2319(7) 0.076(6) Uiso 0.314(7) 1 d D U P D 2
C21' C -0.0280(13) 0.0452(8) 0.2433(7) 0.069(4) Uiso 0.314(7) 1 d D U P D 2
H21C H -0.000918 0.023017 0.282776 0.082 Uiso 0.314(7) 1 calc R U P D 2
H21D H -0.010331 0.007232 0.211218 0.082 Uiso 0.314(7) 1 calc R U P D 2
C22' C -0.1738(15) 0.0633(15) 0.2447(15) 0.134(7) Uiso 0.314(7) 1 d D U P D 2
H22D H -0.225361 0.017097 0.252598 0.202 Uiso 0.314(7) 1 calc R U P D 2
H22E H -0.191449 0.100360 0.276841 0.202 Uiso 0.314(7) 1 calc R U P D 2
H22F H -0.200848 0.084598 0.205386 0.202 Uiso 0.314(7) 1 calc R U P D 2
C23' C 0.0875(19) 0.0981(13) 0.1717(8) 0.112(5) Uiso 0.314(7) 1 d D U P D 2
H23C H 0.106746 0.043617 0.165853 0.135 Uiso 0.314(7) 1 calc R U P D 2
H23D H 0.170707 0.126865 0.162733 0.135 Uiso 0.314(7) 1 calc R U P D 2
C24' C -0.023(3) 0.1224(18) 0.1289(10) 0.166(7) Uiso 0.314(7) 1 d D U P D 2
H24D H 0.005368 0.113128 0.086941 0.249 Uiso 0.314(7) 1 calc R U P D 2
H24E H -0.104847 0.093450 0.137567 0.249 Uiso 0.314(7) 1 calc R U P D 2
H24F H -0.040999 0.176551 0.134453 0.249 Uiso 0.314(7) 1 calc R U P D 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
Cr1 Cr1 1.9419(10) 2 ?
Cr1 C4 2.202(4) . ?
Cr1 C1 2.203(3) . ?
Cr1 C8 2.209(4) . ?
Cr1 C5 2.210(4) . ?
Cr1 Li1 2.521(7) . ?
Cr1 Li2 2.538(7) . ?
Cr1 Li1 2.647(7) 2 ?
Cr1 Li2 2.656(7) 2 ?
Li1 O10' 1.95(4) . ?
Li1 O10 1.973(9) . ?
Li1 Li2 3.323(10) 2 ?
Li1 Li1 3.473(13) 2 ?
Li2 O20' 1.924(17) . ?
Li2 O20 1.997(8) . ?
Li2 Li2 3.499(14) 2 ?
C1 C2 1.514(7) . ?
C1 C2' 1.558(10) . ?
C2 C3 1.536(9) . ?
C3 C4 1.537(7) . ?
C2' C3' 1.534(14) . ?
C3' C4 1.520(12) . ?
C5 C6' 1.519(10) . ?
C5 C6 1.574(8) . ?
C6 C7 1.505(10) . ?
C7 C8 1.505(7) . ?
C6' C7' 1.498(12) . ?
C7' C8 1.554(10) . ?
O10 C11 1.420(7) . ?
O10 C13 1.439(7) . ?
C11 C12 1.355(11) . ?
C13 C14 1.379(9) . ?
O10' C13' 1.431(16) . ?
O10' C11' 1.433(17) . ?
C11' C12' 1.372(18) . ?
C13' C14' 1.372(18) . ?
O20 C21 1.380(9) . ?
O20 C23 1.416(9) . ?
C21 C22 1.534(10) . ?
C23 C24 1.412(11) . ?
O20' C23' 1.398(15) . ?
O20' C21' 1.414(14) . ?
C21' C22' 1.483(14) . ?
C23' C24' 1.508(16) . ?

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
Cr1 Cr1 C4 108.84(11) 2 . ?
Cr1 Cr1 C1 109.26(11) 2 . ?
C4 Cr1 C1 79.66(14) . . ?
Cr1 Cr1 C8 109.48(11) 2 . ?
C4 Cr1 C8 87.94(15) . . ?
C1 Cr1 C8 141.26(14) . . ?
Cr1 Cr1 C5 108.57(10) 2 . ?
C4 Cr1 C5 142.58(15) . . ?
C1 Cr1 C5 88.23(14) . . ?
C8 Cr1 C5 79.68(14) . . ?
Cr1 Cr1 Li1 71.40(16) 2 . ?
C4 Cr1 Li1 134.3(2) . . ?
C1 Cr1 Li1 59.1(2) . . ?
C8 Cr1 Li1 136.5(2) . . ?
C5 Cr1 Li1 60.43(18) . . ?
Cr1 Cr1 Li2 71.32(16) 2 . ?
C4 Cr1 Li2 60.67(19) . . ?
C1 Cr1 Li2 136.5(2) . . ?
C8 Cr1 Li2 59.1(2) . . ?
C5 Cr1 Li2 134.1(2) . . ?
Li1 Cr1 Li2 142.7(2) . . ?
Cr1 Cr1 Li1 64.54(15) 2 2 ?
C4 Cr1 Li1 138.72(19) . 2 ?
C1 Cr1 Li1 141.62(19) . 2 ?
C8 Cr1 Li1 60.19(17) . 2 ?
C5 Cr1 Li1 61.5(2) . 2 ?
Li1 Cr1 Li1 84.4(3) . 2 ?
Li2 Cr1 Li1 79.7(2) . 2 ?
Cr1 Cr1 Li2 64.84(16) 2 2 ?
C4 Cr1 Li2 61.60(18) . 2 ?
C1 Cr1 Li2 59.68(19) . 2 ?
C8 Cr1 Li2 141.73(19) . 2 ?
C5 Cr1 Li2 138.59(19) . 2 ?
Li1 Cr1 Li2 79.8(2) . 2 ?
Li2 Cr1 Li2 84.7(3) . 2 ?
Li1 Cr1 Li2 129.4(2) 2 2 ?
O10' Li1 Cr1 151(2) . . ?
O10 Li1 Cr1 157.0(5) . . ?
O10' Li1 Cr1 164(2) . 2 ?
O10 Li1 Cr1 158.9(5) . 2 ?
Cr1 Li1 Cr1 44.06(12) . 2 ?
O10 Li1 Li2 133.3(4) . 2 ?
Cr1 Li1 Li2 51.88(18) . 2 ?
Cr1 Li1 Li2 48.71(17) 2 2 ?
O10 Li1 Li1 136.8(3) . 2 ?
Cr1 Li1 Li1 49.33(16) . 2 ?
Cr1 Li1 Li1 46.27(17) 2 2 ?
Li2 Li1 Li1 89.70(17) 2 2 ?
O20' Li2 Cr1 147.2(7) . . ?
O20 Li2 Cr1 158.3(5) . . ?
O20' Li2 Cr1 168.9(7) . 2 ?
O20 Li2 Cr1 157.8(4) . 2 ?
Cr1 Li2 Cr1 43.84(11) . 2 ?
O20 Li2 Li1 135.2(4) . 2 ?
Cr1 Li2 Li1 51.60(17) . 2 ?
Cr1 Li2 Li1 48.32(15) 2 2 ?
O20 Li2 Li2 135.2(3) . 2 ?
Cr1 Li2 Li2 49.10(18) . 2 ?
Cr1 Li2 Li2 46.24(17) 2 2 ?
Li1 Li2 Li2 89.26(16) 2 2 ?
C2 C1 Cr1 98.1(3) . . ?
C2' C1 Cr1 107.7(5) . . ?
C1 C2 C3 106.8(6) . . ?
C2 C3 C4 112.9(5) . . ?
C3' C2' C1 109.5(10) . . ?
C4 C3' C2' 106.5(10) . . ?
C3' C4 Cr1 98.0(7) . . ?
C3 C4 Cr1 106.3(3) . . ?
C6' C5 Cr1 97.0(5) . . ?
C6 C5 Cr1 106.0(3) . . ?
C7 C6 C5 112.8(6) . . ?
C8 C7 C6 110.1(6) . . ?
C7' C6' C5 104.8(9) . . ?
C6' C7' C8 112.5(9) . . ?
C7 C8 Cr1 99.1(3) . . ?
C7' C8 Cr1 105.0(4) . . ?
C11 O10 C13 116.2(5) . . ?
C11 O10 Li1 121.5(6) . . ?
C13 O10 Li1 122.2(5) . . ?
C12 C11 O10 120.2(9) . . ?
C14 C13 O10 117.9(7) . . ?
C13' O10' C11' 115(2) . . ?
C13' O10' Li1 122(3) . . ?
C11' O10' Li1 120(4) . . ?
C12' C11' O10' 119(2) . . ?
C14' C13' O10' 119(2) . . ?
C21 O20 C23 104.6(7) . . ?
C21 O20 Li2 129.7(6) . . ?
C23 O20 Li2 117.0(5) . . ?
O20 C21 C22 114.3(8) . . ?
C24 C23 O20 118.1(9) . . ?
C23' O20' C21' 100.5(13) . . ?
C23' O20' Li2 128.7(13) . . ?
C21' O20' Li2 128.1(11) . . ?
O20' C21' C22' 110.7(13) . . ?
O20' C23' C24' 110.3(14) . . ?

_refine_diff_density_max         0.557
_refine_diff_density_min         -0.311
_refine_diff_density_rms         0.072

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

data_4
_database_code_depnum_ccdc_archive 'CCDC 2108181'
loop_
_audit_author_name
_audit_author_address
'Andrew White'
;Imperial College London
United Kingdom
;
_audit_update_record             
;
2021-09-07 deposited with the CCDC.	2022-05-31 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-2018/3
_shelx_SHELXL_version_number     2018/3
_chemical_name_systematic        ?
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C22 H54 Cl6 Cr2 N10 P4, 2(C H2 Cl2)'
_chemical_formula_sum            'C24 H58 Cl10 Cr2 N10 P4'
_chemical_formula_weight         1069.18

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'
Cl Cl 0.1484 0.1585 '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'
N N 0.0061 0.0033 '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'

_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 21/c'
_space_group_name_Hall           '-P 2ybc'

_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. 
;

loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, y+1/2, -z+1/2'
'-x, -y, -z'
'x, -y-1/2, z-1/2'

_cell_length_a                   9.3625(3)
_cell_length_b                   12.7925(3)
_cell_length_c                   19.2108(5)
_cell_angle_alpha                90
_cell_angle_beta                 96.406(3)
_cell_angle_gamma                90
_cell_volume                     2286.52(11)
_cell_formula_units_Z            2
_cell_measurement_temperature    173(2)
_cell_measurement_reflns_used    3347
_cell_measurement_theta_min      2.9630
_cell_measurement_theta_max      28.0330

_exptl_crystal_description       blocks
_exptl_crystal_colour            'Dark blue'
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_density_diffrn    1.553
_exptl_crystal_F_000             1100
_exptl_transmission_factor_min   ?
_exptl_transmission_factor_max   ?
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.09
_exptl_absorpt_coefficient_mu    1.232
_shelx_estimated_absorpt_T_min   ?
_shelx_estimated_absorpt_T_max   ?
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_T_max  0.902
_exptl_absorpt_process_details   
; 
CrysAlisPro, Agilent Technologies, 
Version 1.171.37.35 (release 13-08-2014 CrysAlis171 .NET) 
(compiled Aug 13 2014,18:06:01) 
Analytical numeric absorption correction using a multifaceted crystal 
model based on expressions derived by R.C. Clark & J.S. Reid. 
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_absorpt_special_details   ?
_diffrn_ambient_temperature      173(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_source                   'Enhance (Mo) X-ray Source'
_diffrn_measurement_device_type  'Agilent Xcalibur 3 E'
_diffrn_measurement_method       'omega scans'
_diffrn_detector_area_resol_mean 16.0382
_diffrn_reflns_number            8211
_diffrn_reflns_av_unetI/netI     0.0413
_diffrn_reflns_av_R_equivalents  0.0214
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_theta_min         2.662
_diffrn_reflns_theta_max         28.310
_diffrn_reflns_theta_full        25.242
_diffrn_measured_fraction_theta_max 0.810
_diffrn_measured_fraction_theta_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.810
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.810
_diffrn_reflns_point_group_measured_fraction_full 0.990
_reflns_number_total             4609
_reflns_number_gt                3857
_reflns_threshold_expression     'I > 2σ(I)'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_max     .
_reflns_Friedel_fraction_full    .

_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. 
;

_computing_data_collection       'CrysAlisPro, Agilent Technologies'
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies'
_computing_structure_solution    'SHELXS-2013 (Sheldrick, 2013)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'CIFTAB-2014 (Sheldrick, 2017)'
_refine_special_details          ?
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0359P)²+4.4395P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_extinction_coef       0.0021(4)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_number_reflns         4609
_refine_ls_number_parameters     284
_refine_ls_number_restraints     194
_refine_ls_R_factor_all          0.0583
_refine_ls_R_factor_gt           0.0467
_refine_ls_wR_factor_ref         0.1121
_refine_ls_wR_factor_gt          0.1067
_refine_ls_goodness_of_fit_ref   1.115
_refine_ls_restrained_S_all      1.130
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

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 0.08768(5) 0.48384(4) 0.58803(3) 0.01805(15) Uani 1 1 d . . . . .
Cl1 Cl -0.09501(10) 0.39755(8) 0.63634(5) 0.0335(2) Uani 1 1 d . . . . .
Cl2 Cl 0.25506(9) 0.36250(7) 0.63115(5) 0.0304(2) Uani 1 1 d . . . . .
Cl3 Cl -0.08342(9) 0.59773(6) 0.52748(4) 0.0232(2) Uani 1 1 d . . . . .
P1 P 0.27959(9) 0.61802(7) 0.58020(5) 0.0240(2) Uani 1 1 d . . . . .
N2 N 0.2626(3) 0.6631(2) 0.66272(16) 0.0281(7) Uani 1 1 d D . . . .
P3 P 0.13282(10) 0.58898(7) 0.69246(5) 0.0243(2) Uani 1 1 d . . . . .
N4 N 0.4480(3) 0.5885(3) 0.56744(18) 0.0343(8) Uani 1 1 d . . . . .
C5 C 0.5165(4) 0.6696(4) 0.5282(2) 0.0467(11) Uani 1 1 d . . . . .
H5A H 0.581177 0.637570 0.496770 0.056 Uiso 1 1 calc R U . . .
H5B H 0.573177 0.718025 0.560616 0.056 Uiso 1 1 calc R U . . .
C6 C 0.3953(5) 0.7268(4) 0.4863(2) 0.0479(11) Uani 1 1 d . . . . .
H6A H 0.423217 0.799656 0.476955 0.057 Uiso 1 1 calc R U . . .
H6B H 0.367227 0.691188 0.441079 0.057 Uiso 1 1 calc R U . . .
N7 N 0.2787(3) 0.7245(3) 0.52996(17) 0.0350(8) Uani 1 1 d . . . . .
C8 C 0.5450(4) 0.5257(4) 0.6141(3) 0.0497(12) Uani 1 1 d . . . . .
H8A H 0.490100 0.472271 0.636225 0.075 Uiso 1 1 calc R U . . .
H8B H 0.595311 0.570445 0.650269 0.075 Uiso 1 1 calc R U . . .
H8C H 0.615210 0.491696 0.587344 0.075 Uiso 1 1 calc R U . . .
C9 C 0.1533(5) 0.7871(3) 0.5074(2) 0.0429(10) Uani 1 1 d . . . . .
H9A H 0.084336 0.781913 0.542086 0.064 Uiso 1 1 calc R U . . .
H9B H 0.108619 0.761626 0.462051 0.064 Uiso 1 1 calc R U . . .
H9C H 0.182071 0.860254 0.502931 0.064 Uiso 1 1 calc R U . . .
C10 C 0.3502(7) 0.7548(5) 0.6926(4) 0.0390(17) Uani 0.743(12) 1 d D U P A 1
H10A H 0.424579 0.769829 0.660402 0.047 Uiso 0.743(12) 1 calc R U P A 1
C11 C 0.4279(9) 0.7275(6) 0.7631(4) 0.069(3) Uani 0.743(12) 1 d D U P A 1
H11A H 0.484253 0.787775 0.781849 0.104 Uiso 0.743(12) 1 calc R U P A 1
H11B H 0.357731 0.708699 0.795268 0.104 Uiso 0.743(12) 1 calc R U P A 1
H11C H 0.492219 0.668148 0.758220 0.104 Uiso 0.743(12) 1 calc R U P A 1
C12 C 0.2577(15) 0.8521(7) 0.6951(11) 0.054(3) Uani 0.743(12) 1 d D U P A 1
H12A H 0.209469 0.866785 0.648171 0.081 Uiso 0.743(12) 1 calc R U P A 1
H12B H 0.185510 0.840654 0.727504 0.081 Uiso 0.743(12) 1 calc R U P A 1
H12C H 0.318519 0.911646 0.711178 0.081 Uiso 0.743(12) 1 calc R U P A 1
C10' C 0.3299(17) 0.7408(14) 0.7160(10) 0.039(5) Uiso 0.257(12) 1 d D U P A 2
H10B H 0.296446 0.724597 0.762454 0.047 Uiso 0.257(12) 1 calc R U P A 2
C11' C 0.4910(17) 0.7288(15) 0.7222(12) 0.052(5) Uiso 0.257(12) 1 d D U P A 2
H11D H 0.517025 0.657029 0.736277 0.077 Uiso 0.257(12) 1 calc R U P A 2
H11E H 0.525318 0.743944 0.676949 0.077 Uiso 0.257(12) 1 calc R U P A 2
H11F H 0.535417 0.777617 0.757578 0.077 Uiso 0.257(12) 1 calc R U P A 2
C12' C 0.280(4) 0.850(3) 0.694(4) 0.057(8) Uiso 0.257(12) 1 d D U P A 2
H12D H 0.175266 0.853016 0.691261 0.086 Uiso 0.257(12) 1 calc R U P A 2
H12E H 0.321892 0.900130 0.729440 0.086 Uiso 0.257(12) 1 calc R U P A 2
H12F H 0.311792 0.866457 0.648811 0.086 Uiso 0.257(12) 1 calc R U P A 2
N13 N 0.0134(4) 0.6672(3) 0.72414(17) 0.0356(8) Uani 1 1 d . . . . .
C14 C -0.0249(5) 0.6313(4) 0.7917(2) 0.0465(11) Uani 1 1 d . . . . .
H14A H -0.106581 0.581757 0.785167 0.056 Uiso 1 1 calc R U . . .
H14B H -0.051985 0.691002 0.820220 0.056 Uiso 1 1 calc R U . . .
C15 C 0.1075(6) 0.5779(4) 0.8265(2) 0.0522(12) Uani 1 1 d . . . . .
H15A H 0.169827 0.628629 0.854526 0.063 Uiso 1 1 calc R U . . .
H15B H 0.081003 0.521401 0.857817 0.063 Uiso 1 1 calc R U . . .
N16 N 0.1814(4) 0.5352(3) 0.76992(16) 0.0349(8) Uani 1 1 d . . . . .
C17 C -0.0898(5) 0.7316(4) 0.6824(2) 0.0524(13) Uani 1 1 d . . . . .
H17A H -0.177851 0.691398 0.669448 0.079 Uiso 1 1 calc R U . . .
H17B H -0.049452 0.753922 0.639836 0.079 Uiso 1 1 calc R U . . .
H17C H -0.112150 0.793254 0.709444 0.079 Uiso 1 1 calc R U . . .
C18 C 0.3152(5) 0.4802(4) 0.7892(2) 0.0437(11) Uani 1 1 d . . . . .
H18A H 0.377629 0.522581 0.822446 0.066 Uiso 1 1 calc R U . . .
H18B H 0.363219 0.467420 0.747220 0.066 Uiso 1 1 calc R U . . .
H18C H 0.295244 0.413262 0.811015 0.066 Uiso 1 1 calc R U . . .
C20 C 0.7879(10) 0.8731(7) 0.4524(4) 0.057(2) Uani 0.622(3) 1 d D U P B -1
H20A H 0.793087 0.796174 0.447942 0.069 Uiso 0.622(3) 1 calc R U P B -1
H20B H 0.876642 0.902486 0.436592 0.069 Uiso 0.622(3) 1 calc R U P B -1
Cl4 Cl 0.7860(4) 0.9025(3) 0.53705(14) 0.0664(9) Uani 0.622(3) 1 d D U P B -1
Cl5 Cl 0.6435(3) 0.9172(2) 0.39711(12) 0.0693(7) Uani 0.622(3) 1 d D U P B -1
C20' C 0.7074(14) 0.905(2) 0.4327(16) 0.051(4) Uiso 0.193(3) 1 d D U P C -2
H20C H 0.689632 0.833980 0.449755 0.061 Uiso 0.193(3) 1 calc R U P C -2
H20D H 0.698210 0.901771 0.380871 0.061 Uiso 0.193(3) 1 calc R U P C -2
Cl5' Cl 0.5716(7) 0.9845(5) 0.4557(5) 0.0514(17) Uiso 0.193(3) 1 d D U P C -2
Cl4' Cl 0.8805(8) 0.9364(7) 0.4606(5) 0.063(2) Uiso 0.193(3) 1 d D U P C -2
C20" C 0.706(2) 0.865(2) 0.475(3) 0.065(5) Uiso 0.108(3) 1 d D U P D -3
H20E H 0.697551 0.801870 0.503655 0.078 Uiso 0.108(3) 1 calc R U P D -3
H20F H 0.680837 0.845735 0.424885 0.078 Uiso 0.108(3) 1 calc R U P D -3
Cl4" Cl 0.8759(14) 0.9105(14) 0.4867(10) 0.076(4) Uiso 0.108(3) 1 d D U P D -3
Cl5" Cl 0.5925(12) 0.9604(10) 0.4980(8) 0.061(3) Uiso 0.108(3) 1 d D U P D -3
C20* C 0.724(7) 0.905(6) 0.4525(14) 0.062(5) Uiso 0.077(3) 1 d D U P E -4
H20G H 0.710640 0.831349 0.436661 0.074 Uiso 0.077(3) 1 calc R U P E -4
H20H H 0.813283 0.931771 0.435994 0.074 Uiso 0.077(3) 1 calc R U P E -4
Cl4* Cl 0.737(2) 0.910(2) 0.5421(12) 0.053(5) Uiso 0.077(3) 1 d D U P E -4
Cl5* Cl 0.580(2) 0.9788(16) 0.4187(11) 0.063(4) Uiso 0.077(3) 1 d D U P E -4


_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 Cl2 2.2939(10) . ?
Cr1 Cl1 2.3151(10) . ?
Cr1 Cl3 2.3719(9) . ?
Cr1 P3 2.4131(10) . ?
Cr1 Cl3 2.4484(9) 3_566 ?
Cr1 P1 2.5015(10) . ?
P1 N4 1.666(3) . ?
P1 N7 1.669(3) . ?
P1 N2 1.711(3) . ?
N2 C10 1.508(6) . ?
N2 C10' 1.514(15) . ?
N2 P3 1.690(3) . ?
P3 N16 1.656(3) . ?
P3 N13 1.666(3) . ?
N4 C8 1.446(5) . ?
N4 C5 1.471(5) . ?
C5 C6 1.505(6) . ?
C6 N7 1.449(5) . ?
N7 C9 1.447(5) . ?
C10 C11 1.507(8) . ?
C10 C12 1.520(9) . ?
C10' C11' 1.507(15) . ?
C10' C12' 1.510(16) . ?
N13 C17 1.443(6) . ?
N13 C14 1.459(5) . ?
C14 C15 1.505(7) . ?
C15 N16 1.458(5) . ?
N16 C18 1.448(5) . ?
C20 Cl4 1.670(7) . ?
C20 Cl5 1.719(8) . ?
C20' Cl4' 1.697(15) . ?
C20' Cl5' 1.721(14) . ?
C20" Cl4" 1.683(16) . ?
C20" Cl5" 1.712(16) . ?
C20* Cl4* 1.714(17) . ?
C20* Cl5* 1.715(17) . ?

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
Cl2 Cr1 Cl1 92.18(4) . . ?
Cl2 Cr1 Cl3 171.71(4) . . ?
Cl1 Cr1 Cl3 90.04(4) . . ?
Cl2 Cr1 P3 91.59(4) . . ?
Cl1 Cr1 P3 90.06(4) . . ?
Cl3 Cr1 P3 96.40(3) . . ?
Cl2 Cr1 Cl3 88.87(3) . 3_566 ?
Cl1 Cr1 Cl3 102.83(4) . 3_566 ?
Cl3 Cr1 Cl3 82.85(3) . 3_566 ?
P3 Cr1 Cl3 167.07(4) . 3_566 ?
Cl2 Cr1 P1 91.13(4) . . ?
Cl1 Cr1 P1 156.78(4) . . ?
Cl3 Cr1 P1 89.97(3) . . ?
P3 Cr1 P1 66.87(3) . . ?
Cl3 Cr1 P1 100.20(3) 3_566 . ?
Cr1 Cl3 Cr1 97.15(3) . 3_566 ?
N4 P1 N7 92.49(17) . . ?
N4 P1 N2 113.58(16) . . ?
N7 P1 N2 105.42(16) . . ?
N4 P1 Cr1 123.48(12) . . ?
N7 P1 Cr1 129.60(12) . . ?
N2 P1 Cr1 91.93(11) . . ?
C10 N2 P3 133.5(4) . . ?
C10' N2 P3 113.6(8) . . ?
C10 N2 P1 120.8(4) . . ?
C10' N2 P1 140.7(8) . . ?
P3 N2 P1 105.61(16) . . ?
N16 P3 N13 92.84(17) . . ?
N16 P3 N2 113.63(16) . . ?
N13 P3 N2 108.88(16) . . ?
N16 P3 Cr1 121.37(12) . . ?
N13 P3 Cr1 125.20(12) . . ?
N2 P3 Cr1 95.59(11) . . ?
C8 N4 C5 115.5(3) . . ?
C8 N4 P1 125.0(3) . . ?
C5 N4 P1 112.9(3) . . ?
N4 C5 C6 105.7(3) . . ?
N7 C6 C5 104.6(3) . . ?
C9 N7 C6 117.0(3) . . ?
C9 N7 P1 125.2(3) . . ?
C6 N7 P1 113.3(3) . . ?
C11 C10 N2 110.4(5) . . ?
C11 C10 C12 112.4(9) . . ?
N2 C10 C12 111.2(7) . . ?
C11' C10' C12' 113.0(18) . . ?
C11' C10' N2 108.9(14) . . ?
C12' C10' N2 109(3) . . ?
C17 N13 C14 117.3(3) . . ?
C17 N13 P3 125.1(3) . . ?
C14 N13 P3 112.2(3) . . ?
N13 C14 C15 105.4(3) . . ?
N16 C15 C14 105.9(3) . . ?
C18 N16 C15 117.4(3) . . ?
C18 N16 P3 125.1(3) . . ?
C15 N16 P3 114.1(3) . . ?
Cl4 C20 Cl5 115.8(5) . . ?
Cl4' C20' Cl5' 119.2(13) . . ?
Cl4" C20" Cl5" 108.8(14) . . ?
Cl4* C20* Cl5* 108.7(15) . . ?

_refine_diff_density_max         0.893
_refine_diff_density_min         -0.672
_refine_diff_density_rms         0.084

