# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2024

####################################################################### 
# 
# 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_mu016_op
_database_code_depnum_ccdc_archive 'CCDC 2346026'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Li([12]crown-4)2][1,2,3-P3C2tBu2].(C4H8O)'
_chemical_formula_moiety         
'C10 H18 P3, C16 H32 Li O8, 0.5(C4 H8 O), 0.5[C4H8O]'
_chemical_formula_sum            'C30 H58 Li O9 P3'
_chemical_formula_weight         662.61
_chemical_melting_point          ?
_chemical_oxdiff_formula         C30H48LiO9P3
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'
Li Li 0.0008 0.0003 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      orthorhombic
_space_group_IT_number           61
_space_group_name_H-M_alt        'P b c a'
_space_group_name_Hall           '-P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'
'-x, -y, -z'
'x-1/2, y, -z-1/2'
'x, -y-1/2, z-1/2'
'-x-1/2, y-1/2, z'

_cell_length_a                   37.25924(16)
_cell_length_b                   12.33778(5)
_cell_length_c                   31.13083(16)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     14310.72(11)
_cell_formula_units_Z            16
_cell_measurement_reflns_used    103390
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      71.5230
_cell_measurement_theta_min      2.3540
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    1.914
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.91a (Rigaku Oxford Diffraction, 2020)
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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.230
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             5728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-20 3 -10 0.0493
21 0 10 0.0884
11 7 3 0.1393
-5 -8 1 0.1466
8 -7 6 0.1405
-4 8 0 0.1372
15 0 -16 0.0808
8 6 -11 0.1356
-5 -7 9 0.1487
0 -8 4 0.1457
7 -8 -4 0.1552
-15 1 16 0.0840
20 0 -11 0.0953
7 0 -19 0.0829

_exptl_crystal_size_max          0.322
_exptl_crystal_size_mid          0.181
_exptl_crystal_size_min          0.167
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
-19.5972 2.5048 -10.0070 0.3076 -0.8594 -0.4083
21.0898 -0.1401 9.8702 -0.3334 0.9354 0.1176
11.4507 6.9615 2.8832 -0.1875 0.5369 -0.8226
-4.5143 -7.8660 0.6651 0.0786 -0.2328 0.9694
7.8692 -7.1684 6.1863 -0.1179 0.3197 0.9402
-3.5531 7.9242 0.1559 -0.1732 -0.0897 -0.9808
14.6887 0.0503 -16.0527 0.8729 0.4762 -0.1065
7.9360 6.0429 -11.4980 0.5003 0.2766 -0.8205
-5.4714 -6.8983 9.2102 -0.3580 -0.1995 0.9122
-0.2256 -7.8583 3.9366 -0.0509 -0.0326 0.9982
6.9089 -7.5102 -4.0124 0.3746 0.1998 0.9054
-14.8582 1.0451 15.7232 -0.8777 -0.4782 -0.0313
19.9087 0.0681 -11.4662 0.6858 0.7246 -0.0679
6.8300 0.0747 -19.3860 0.9809 0.1301 -0.1443

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0188
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.989
_diffrn_reflns_limit_h_max       45
_diffrn_reflns_limit_h_min       -45
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       38
_diffrn_reflns_limit_l_min       -38
_diffrn_reflns_number            263626
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.989
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         71.946
_diffrn_reflns_theta_min         2.372
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_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     67.00 110.00   0.50    0.35    --   60.44  30.00   0.00   86
  2  ω     78.00 124.00   0.50    0.35    --   74.67  30.00-120.00   92
  3  ω     80.00 124.00   0.50    0.35    --   74.67  30.00   0.00   88
  4  ω     62.00 105.00   0.50    0.35    --   60.44  30.00  60.00   86
  5  ω     62.00  98.00   0.50    0.35    --   60.44  30.00  90.00   72
  6  ω     75.00 123.00   0.50    0.35    --   73.92  30.00 150.00   96
  7  ω   -111.00 -63.00   0.50    0.35    --  -61.80 -30.00-180.00   96
  8  ω   -120.00 -77.00   0.50    0.35    --  -75.44 -30.00-150.00   86
  9  ω   -108.00 -69.00   0.50    0.35    --  -61.80 -30.00 120.00   78
 10  ω   -124.00 -76.00   0.50    0.35    --  -75.44 -30.00 150.00   96
 11  ω   -101.00 -29.00   0.50    0.35    --  -74.27 116.00  35.00  144
 12  ω   -106.00 -33.00   0.50    0.35    --  -75.44 125.00 120.00  146
 13  ω    -90.00 -29.00   0.50    0.35    --  -74.27 125.00 -30.00  122
 14  ω   -109.00 -34.00   0.50    0.35    --  -61.80 166.00-177.00  150
 15  ω   -123.00 -39.00   0.50    0.35    --  -75.44 166.00-177.00  168
 16  ω    -92.00 -18.00   0.50    0.35    --  -61.80 125.00-180.00  148
 17  ω   -106.00 -30.00   0.50    0.35    --  -75.44 125.00 -60.00  152
 18  ω   -102.00 -30.00   0.50    0.35    --  -75.44 116.00  35.00  144
 19  ω    -88.00 -16.00   0.50    0.35    --  -61.80 116.00  35.00  144
 20  ω   -101.00 -30.00   0.50    0.35    --  -75.44 125.00  60.00  142
 21  ω    -76.00 -30.00   0.50    0.35    --  -75.44 125.00  90.00   92
 22  ω   -106.00 -80.00   0.50    0.35    --  -75.44 125.00  90.00   52
 23  ω   -120.00 -76.00   0.50    0.35    --  -74.27-125.00  90.00   88
 24  ω   -111.00 -48.00   0.50    0.35    --  -74.27-166.00 160.00  126
 25  ω    -98.00 -48.00   0.50    0.35    --  -61.80-166.00 160.00  100
 26  ω   -119.00 -75.00   0.50    0.35    --  -74.27-125.00 -30.00   88
 27  ω     35.00  85.00   0.50    0.35    --   74.67 -95.00-120.00  100
 28  ω     76.00 105.00   0.50    0.35    --   74.67-125.00-120.00   58
 29  ω     29.00  55.00   0.50    0.35    --   74.67-125.00-120.00   52
 30  ω     15.00  87.00   0.50    0.35    --   60.44-116.00 -52.00  144
 31  ω     28.00 100.00   0.50    0.35    --   73.92-116.00 -52.00  144
 32  ω     29.00 101.00   0.50    0.35    --   74.67-116.00 -52.00  144
 33  ω     34.00  62.00   0.50    0.35    --   73.92 -95.00 -30.00   56
 34  ω     39.00 122.00   0.50    0.35    --   74.67-166.00 160.00  166
 35  ω     39.00 108.00   0.50    0.35    --   60.44-166.00 160.00  138
 36  ω     35.00  77.00   0.50    0.35    --   73.92 -95.00  60.00   84
 37  ω     21.00  71.00   0.50    0.35    --   60.44 -95.00   0.00  100
 38  ω     21.00  71.00   0.50    0.35    --   60.44 -95.00-180.00  100
 39  ω     14.00  47.00   0.50    0.35    --   60.44 -30.00 -90.00   66
 40  ω     11.00  40.00   0.50    0.35    --   60.44 -30.00   0.00   58
 41  ω     52.00 111.00   0.50    0.35    --   73.92 166.00-177.00  118
 42  ω     57.00  82.00   0.50    0.35    --   74.67 166.00-177.00   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0066831000
_diffrn_orient_matrix_UB_12      -0.0179153000
_diffrn_orient_matrix_UB_13      -0.0483152000
_diffrn_orient_matrix_UB_21      0.0408008000
_diffrn_orient_matrix_UB_22      0.0068239000
_diffrn_orient_matrix_UB_23      0.0076892000
_diffrn_orient_matrix_UB_31      0.0012822000
_diffrn_orient_matrix_UB_32      -0.1233420000
_diffrn_orient_matrix_UB_33      0.0074191000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                12302
_reflns_number_total             13906
_reflns_odcompleteness_completeness 99.98
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 Structure factors included contributions from the .fab file.
 
 _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 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.445
_refine_diff_density_min         -0.266
_refine_diff_density_rms         0.040
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.042
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     851
_refine_ls_number_reflns         13906
_refine_ls_number_restraints     352
_refine_ls_R_factor_all          0.0461
_refine_ls_R_factor_gt           0.0413
_refine_ls_restrained_S_all      1.141
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0594P)²+5.3410P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1178
_refine_special_details          SQUEEZE
_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
 H16A-H18A = H18A-H20C
 2.5 with sigma of 0.02
 H6C-H8C = H8C-H5A
 2.5 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O16A \\sim C52A \\sim C46A \\sim C51A \\sim C45A \\sim C52B \\sim C45B \\sim
O16B \\sim C46B \\sim C47B \\sim O14A \\sim O15A \\sim O13A \\sim C48A \\sim
C50A \\sim C49A \\sim C47A \\sim O14B \\sim O15B \\sim C50B \\sim C51B \\sim
O13B \\sim C48B \\sim C49B: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.01 within 1.7A
4. Others
 Sof(O14B)=Sof(O15B)=Sof(C50B)=Sof(H50C)=Sof(H50D)=Sof(C51B)=Sof(H51C)=
 Sof(H51D)=Sof(C52B)=Sof(H52C)=Sof(H52D)=Sof(C45B)=Sof(H45C)=Sof(H45D)=
 Sof(O16B)=Sof(C46B)=Sof(H46C)=Sof(H46D)=Sof(C47B)=Sof(H47C)=Sof(H47D)=
 Sof(O13B)=Sof(C48B)=Sof(H48C)=Sof(H48D)=Sof(C49B)=Sof(H49C)=Sof(H49D)=1-FVAR(1)
 Sof(O14A)=Sof(O16A)=Sof(O15A)=Sof(O13A)=Sof(C48A)=Sof(H48A)=Sof(H48B)=
 Sof(C50A)=Sof(H50A)=Sof(H50B)=Sof(C52A)=Sof(H52A)=Sof(H52B)=Sof(C49A)=
 Sof(H49A)=Sof(H49B)=Sof(C46A)=Sof(H46A)=Sof(H46B)=Sof(C47A)=Sof(H47A)=
 Sof(H47B)=Sof(C51A)=Sof(H51A)=Sof(H51B)=Sof(C45A)=Sof(H45A)=Sof(H45B)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C44(H44A,H44B), C43(H43A,H43B), C32(H32A,H32B), C42(H42A,H42B), C31(H31A,
 H31B), C33(H33A,H33B), C34(H34A,H34B), C35(H35A,H35B), C25(H25A,H25B),
 C38(H38A,H38B), C27(H27A,H27B), C37(H37A,H37B), C48A(H48A,H48B), C41(H41A,
 H41B), C29(H29A,H29B), C28(H28A,H28B), C26(H26A,H26B), C30(H30A,H30B),
 C23(H23A,H23B), C39(H39A,H39B), C36(H36A,H36B), C56(H56A,H56B), C50A(H50A,
 H50B), C53(H53A,H53B), C40(H40A,H40B), C24(H24A,H24B), C22(H22A,H22B),
 C55(H55A,H55B), C21(H21A,H21B), C52A(H52A,H52B), C54(H54A,H54B), C49A(H49A,
 H49B), C46A(H46A,H46B), C47A(H47A,H47B), C51A(H51A,H51B), C45A(H45A,H45B),
 C50B(H50C,H50D), C51B(H51C,H51D), C52B(H52C,H52D), C45B(H45C,H45D), C46B(H46C,
 H46D), C47B(H47C,H47D), C48B(H48C,H48D), C49B(H49C,H49D)
5.b Idealised Me refined as rotating group:
 C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C15(H15A,H15B,H15C), C8(H8A,H8B,H8C),
 C4(H4A,H4B,H4C), C10(H10A,H10B,H10C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C),
  C5(H5A,H5B,H5C), C14(H14A,H14B,H14C), C20(H20A,H20B,H20C), C19(H19A,H19B,H19C)
;
_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 0.63337(2) 0.28793(3) 0.34628(2) 0.03411(10) Uani 1 1 d . . . . .
P4 P 0.63405(2) 0.75122(3) 0.59453(2) 0.03377(10) Uani 1 1 d . . . . .
P3 P 0.63238(2) 0.25345(3) 0.44543(2) 0.03458(10) Uani 1 1 d . . . . .
P2 P 0.59607(2) 0.27162(3) 0.39535(2) 0.03491(10) Uani 1 1 d . . . . .
P5 P 0.59775(2) 0.76785(3) 0.64469(2) 0.03683(10) Uani 1 1 d . . . . .
P6 P 0.63502(2) 0.78202(3) 0.69382(2) 0.03747(10) Uani 1 1 d . . . . .
O6 O 0.35756(3) 0.32144(8) 0.65630(3) 0.0378(2) Uani 1 1 d . . . . .
O12 O 0.64017(3) 0.17285(8) 0.69838(3) 0.0375(2) Uani 1 1 d . . . . .
O11 O 0.56666(3) 0.17459(8) 0.69294(4) 0.0389(2) Uani 1 1 d . . . . .
O3 O 0.33740(3) 0.13206(9) 0.60100(4) 0.0444(3) Uani 1 1 d . . . . .
O7 O 0.35645(3) 0.35525(9) 0.56945(4) 0.0422(3) Uani 1 1 d . . . . .
O17 O 0.50183(3) 0.13321(9) 0.77735(4) 0.0485(3) Uani 1 1 d . . . . .
O5 O 0.43168(3) 0.31582(9) 0.65744(4) 0.0423(3) Uani 1 1 d . . . . .
O8 O 0.43025(3) 0.34739(9) 0.56905(4) 0.0463(3) Uani 1 1 d . . . . .
O9 O 0.64465(4) 0.14420(9) 0.61137(4) 0.0484(3) Uani 1 1 d . . . . .
O4 O 0.38866(3) 0.15117(10) 0.53968(4) 0.0482(3) Uani 1 1 d . . . . .
O2 O 0.38856(3) 0.09868(9) 0.66393(4) 0.0487(3) Uani 1 1 d . . . . .
O1 O 0.44054(3) 0.11694(9) 0.60051(4) 0.0509(3) Uani 1 1 d . . . . .
O10 O 0.57097(4) 0.14892(9) 0.60503(4) 0.0504(3) Uani 1 1 d . . . . .
O14A O 0.66021(4) 0.36691(12) 0.64411(5) 0.0406(4) Uani 0.815(2) 1 d . U P A 1
O16A O 0.55842(6) 0.37904(17) 0.64175(8) 0.0578(6) Uani 0.815(2) 1 d . U P A 1
O15A O 0.60830(5) 0.39518(16) 0.70630(7) 0.0522(5) Uani 0.815(2) 1 d . U P A 1
O13A O 0.61089(6) 0.34973(15) 0.58014(6) 0.0552(5) Uani 0.815(2) 1 d . U P A 1
C1 C 0.67513(4) 0.27988(11) 0.37391(5) 0.0291(3) Uani 1 1 d . . . . .
C11 C 0.67625(4) 0.75665(11) 0.62127(5) 0.0290(3) Uani 1 1 d . . . . .
C2 C 0.67465(4) 0.26044(11) 0.41881(5) 0.0291(3) Uani 1 1 d . . . . .
C12 C 0.67670(4) 0.77443(11) 0.66622(5) 0.0307(3) Uani 1 1 d . . . . .
C3 C 0.70769(4) 0.29042(13) 0.34219(5) 0.0380(3) Uani 1 1 d . . . . .
C13 C 0.70833(4) 0.74526(13) 0.58885(5) 0.0365(3) Uani 1 1 d . . . . .
C7 C 0.70667(4) 0.24855(13) 0.45119(5) 0.0362(3) Uani 1 1 d . . . . .
C17 C 0.70923(5) 0.78462(13) 0.69800(5) 0.0429(4) Uani 1 1 d . . . . .
C44 C 0.62037(5) 0.09802(13) 0.72388(5) 0.0405(4) Uani 1 1 d . . . . .
H44A H 0.633013 0.083989 0.751295 0.049 Uiso 1 1 calc R U . . .
H44B H 0.617500 0.028418 0.708432 0.049 Uiso 1 1 calc R U . . .
C43 C 0.58454(5) 0.14826(13) 0.73223(5) 0.0412(4) Uani 1 1 d . . . . .
H43A H 0.569547 0.097266 0.748980 0.049 Uiso 1 1 calc R U . . .
H43B H 0.587725 0.214922 0.749514 0.049 Uiso 1 1 calc R U . . .
C6 C 0.73848(4) 0.36418(14) 0.35769(6) 0.0461(4) Uani 1 1 d . . . . .
H6A H 0.729848 0.439021 0.359841 0.069 Uiso 1 1 calc R U . . .
H6B H 0.758377 0.360771 0.337146 0.069 Uiso 1 1 calc R U . . .
H6C H 0.746783 0.339647 0.385932 0.069 Uiso 1 1 calc DR U . . .
C32 C 0.37631(5) 0.39490(13) 0.68330(5) 0.0442(4) Uani 1 1 d . . . . .
H32A H 0.362165 0.410125 0.709538 0.053 Uiso 1 1 calc R U . . .
H32B H 0.380657 0.464106 0.668073 0.053 Uiso 1 1 calc R U . . .
C42 C 0.54935(5) 0.08494(13) 0.67365(6) 0.0448(4) Uani 1 1 d . . . . .
H42A H 0.527401 0.065584 0.689847 0.054 Uiso 1 1 calc R U . . .
H42B H 0.565531 0.021301 0.673162 0.054 Uiso 1 1 calc R U . . .
C9 C 0.72134(5) 0.36125(14) 0.46350(6) 0.0459(4) Uani 1 1 d . . . . .
H9A H 0.728347 0.400423 0.437426 0.069 Uiso 1 1 calc R U . . .
H9B H 0.742293 0.352728 0.482223 0.069 Uiso 1 1 calc R U . . .
H9C H 0.702701 0.402205 0.478657 0.069 Uiso 1 1 calc R U . . .
C31 C 0.41112(5) 0.34227(14) 0.69478(5) 0.0448(4) Uani 1 1 d . . . . .
H31A H 0.425185 0.391836 0.713271 0.054 Uiso 1 1 calc R U . . .
H31B H 0.406313 0.275334 0.711346 0.054 Uiso 1 1 calc R U . . .
C33 C 0.32712(4) 0.36902(14) 0.63566(6) 0.0435(4) Uani 1 1 d . . . . .
H33A H 0.314842 0.418500 0.655928 0.052 Uiso 1 1 calc R U . . .
H33B H 0.309969 0.311349 0.627432 0.052 Uiso 1 1 calc R U . . .
C15 C 0.72272(5) 0.85792(14) 0.57663(6) 0.0459(4) Uani 1 1 d . . . . .
H15A H 0.704078 0.898260 0.561207 0.069 Uiso 1 1 calc R U . . .
H15B H 0.743844 0.849852 0.558151 0.069 Uiso 1 1 calc R U . . .
H15C H 0.729395 0.897465 0.602733 0.069 Uiso 1 1 calc R U . . .
C8 C 0.73718(4) 0.17306(14) 0.43585(6) 0.0451(4) Uani 1 1 d . . . . .
H8A H 0.727036 0.103416 0.426806 0.068 Uiso 1 1 calc R U . . .
H8B H 0.754161 0.161200 0.459428 0.068 Uiso 1 1 calc R U . . .
H8C H 0.749704 0.206678 0.411581 0.068 Uiso 1 1 calc DR U . . .
C34 C 0.33828(5) 0.43115(14) 0.59623(6) 0.0461(4) Uani 1 1 d . . . . .
H34A H 0.317012 0.461089 0.581316 0.055 Uiso 1 1 calc R U . . .
H34B H 0.354440 0.491695 0.604070 0.055 Uiso 1 1 calc R U . . .
C35 C 0.37666(5) 0.40408(15) 0.53559(5) 0.0486(4) Uani 1 1 d . . . . .
H35A H 0.363366 0.467328 0.524203 0.058 Uiso 1 1 calc R U . . .
H35B H 0.379737 0.351309 0.511922 0.058 Uiso 1 1 calc R U . . .
C25 C 0.35225(5) 0.06169(15) 0.66864(5) 0.0454(4) Uani 1 1 d . . . . .
H25A H 0.337797 0.118615 0.682892 0.054 Uiso 1 1 calc R U . . .
H25B H 0.351837 -0.003679 0.687077 0.054 Uiso 1 1 calc R U . . .
C4 C 0.69624(5) 0.34325(15) 0.29910(5) 0.0498(4) Uani 1 1 d . . . . .
H4A H 0.679049 0.295961 0.284399 0.075 Uiso 1 1 calc R U . . .
H4B H 0.717426 0.353538 0.280891 0.075 Uiso 1 1 calc R U . . .
H4C H 0.685026 0.413649 0.304795 0.075 Uiso 1 1 calc R U . . .
C38 C 0.66185(5) 0.06707(14) 0.63875(6) 0.0514(4) Uani 1 1 d . . . . .
H38A H 0.683758 0.038119 0.624889 0.062 Uiso 1 1 calc R U . . .
H38B H 0.645479 0.005933 0.645096 0.062 Uiso 1 1 calc R U . . .
C10 C 0.69469(5) 0.19665(15) 0.49407(5) 0.0458(4) Uani 1 1 d . . . . .
H10A H 0.676828 0.243277 0.507940 0.069 Uiso 1 1 calc R U . . .
H10B H 0.715528 0.188489 0.513010 0.069 Uiso 1 1 calc R U . . .
H10C H 0.684133 0.125307 0.488439 0.069 Uiso 1 1 calc R U . . .
C16 C 0.73888(4) 0.66971(14) 0.60420(6) 0.0480(4) Uani 1 1 d . . . . .
H16A H 0.748646 0.696923 0.631366 0.072 Uiso 1 1 calc DR U . . .
H16B H 0.757931 0.667952 0.582506 0.072 Uiso 1 1 calc R U . . .
H16C H 0.729415 0.596378 0.608453 0.072 Uiso 1 1 calc R U . . .
C27 C 0.32892(5) 0.11648(15) 0.55655(5) 0.0463(4) Uani 1 1 d . . . . .
H27A H 0.320664 0.185916 0.544054 0.056 Uiso 1 1 calc R U . . .
H27B H 0.309126 0.063356 0.553955 0.056 Uiso 1 1 calc R U . . .
C37 C 0.67125(4) 0.12649(14) 0.67912(6) 0.0469(4) Uani 1 1 d . . . . .
H37A H 0.682681 0.075783 0.699623 0.056 Uiso 1 1 calc R U . . .
H37B H 0.688725 0.184553 0.672461 0.056 Uiso 1 1 calc R U . . .
C18 C 0.73984(5) 0.85939(15) 0.68257(6) 0.0516(4) Uani 1 1 d . . . . .
H18A H 0.749108 0.832905 0.655042 0.077 Uiso 1 1 calc DR U . . .
H18B H 0.759185 0.859481 0.703891 0.077 Uiso 1 1 calc R U . . .
H18C H 0.730649 0.933263 0.678970 0.077 Uiso 1 1 calc R U . . .
C48A C 0.67094(11) 0.3830(4) 0.60090(14) 0.0447(9) Uani 0.815(2) 1 d . U P A 1
H48A H 0.679615 0.313731 0.588692 0.054 Uiso 0.815(2) 1 calc R U P A 1
H48B H 0.690905 0.435900 0.599870 0.054 Uiso 0.815(2) 1 calc R U P A 1
C41 C 0.53998(5) 0.11889(15) 0.62882(7) 0.0528(5) Uani 1 1 d . . . . .
H41A H 0.527681 0.058354 0.614025 0.063 Uiso 1 1 calc R U . . .
H41B H 0.523190 0.181013 0.629960 0.063 Uiso 1 1 calc R U . . .
C5 C 0.72175(5) 0.17712(15) 0.32965(6) 0.0523(5) Uani 1 1 d . . . . .
H5A H 0.726116 0.134491 0.355698 0.078 Uiso 1 1 calc DR U . . .
H5B H 0.744194 0.184666 0.313519 0.078 Uiso 1 1 calc R U . . .
H5C H 0.703867 0.140236 0.311784 0.078 Uiso 1 1 calc R U . . .
C29 C 0.46080(5) 0.37377(16) 0.59460(6) 0.0521(4) Uani 1 1 d . . . . .
H29A H 0.474009 0.434420 0.581054 0.062 Uiso 1 1 calc R U . . .
H29B H 0.477081 0.310454 0.595901 0.062 Uiso 1 1 calc R U . . .
C14 C 0.69628(5) 0.69290(15) 0.54609(5) 0.0481(4) Uani 1 1 d . . . . .
H14A H 0.686253 0.620897 0.551799 0.072 Uiso 1 1 calc R U . . .
H14B H 0.716977 0.686107 0.526850 0.072 Uiso 1 1 calc R U . . .
H14C H 0.677974 0.738512 0.532520 0.072 Uiso 1 1 calc R U . . .
C28 C 0.36063(5) 0.07674(15) 0.53222(6) 0.0517(4) Uani 1 1 d . . . . .
H28A H 0.367587 0.003579 0.542282 0.062 Uiso 1 1 calc R U . . .
H28B H 0.355071 0.072783 0.501166 0.062 Uiso 1 1 calc R U . . .
C20 C 0.72361(6) 0.67127(15) 0.70978(7) 0.0583(5) Uani 1 1 d . . . . .
H20A H 0.704831 0.630189 0.724645 0.087 Uiso 1 1 calc R U . . .
H20B H 0.744519 0.678748 0.728641 0.087 Uiso 1 1 calc R U . . .
H20C H 0.730609 0.632820 0.683539 0.087 Uiso 1 1 calc DR U . . .
C26 C 0.33592(5) 0.03520(15) 0.62552(6) 0.0488(4) Uani 1 1 d . . . . .
H26A H 0.349675 -0.023151 0.611185 0.059 Uiso 1 1 calc R U . . .
H26B H 0.310759 0.010972 0.629001 0.059 Uiso 1 1 calc R U . . .
C30 C 0.44999(5) 0.40544(15) 0.63933(6) 0.0521(4) Uani 1 1 d . . . . .
H30A H 0.471465 0.423340 0.656662 0.062 Uiso 1 1 calc R U . . .
H30B H 0.434091 0.469705 0.638572 0.062 Uiso 1 1 calc R U . . .
C23 C 0.44695(5) 0.06325(15) 0.64088(7) 0.0569(5) Uani 1 1 d . . . . .
H23A H 0.456566 0.116300 0.661781 0.068 Uiso 1 1 calc R U . . .
H23B H 0.465243 0.005995 0.636764 0.068 Uiso 1 1 calc R U . . .
C39 C 0.62650(6) 0.09657(16) 0.57565(6) 0.0594(5) Uani 1 1 d . . . . .
H39A H 0.640667 0.034510 0.564758 0.071 Uiso 1 1 calc R U . . .
H39B H 0.624459 0.150565 0.552250 0.071 Uiso 1 1 calc R U . . .
C36 C 0.41287(5) 0.44009(15) 0.55131(6) 0.0530(5) Uani 1 1 d . . . . .
H36A H 0.427167 0.469833 0.527235 0.064 Uiso 1 1 calc R U . . .
H36B H 0.410191 0.497120 0.573448 0.064 Uiso 1 1 calc R U . . .
C56 C 0.48221(5) 0.21105(15) 0.75300(7) 0.0565(5) Uani 1 1 d . . . . .
H56A H 0.456852 0.188027 0.750398 0.068 Uiso 1 1 calc R U . . .
H56B H 0.492466 0.216809 0.723748 0.068 Uiso 1 1 calc R U . . .
C50A C 0.64355(12) 0.4365(4) 0.71196(18) 0.0475(9) Uani 0.815(2) 1 d . U P A 1
H50A H 0.658486 0.381917 0.726903 0.057 Uiso 0.815(2) 1 calc R U P A 1
H50B H 0.642635 0.502400 0.730081 0.057 Uiso 0.815(2) 1 calc R U P A 1
C53 C 0.51265(7) 0.18179(16) 0.81631(7) 0.0664(6) Uani 1 1 d . . . . .
H53A H 0.536712 0.155633 0.824944 0.080 Uiso 1 1 calc R U . . .
H53B H 0.495377 0.165055 0.839544 0.080 Uiso 1 1 calc R U . . .
C19 C 0.69787(6) 0.83619(16) 0.74125(6) 0.0593(5) Uani 1 1 d . . . . .
H19A H 0.686270 0.906169 0.735851 0.089 Uiso 1 1 calc R U . . .
H19B H 0.719129 0.847131 0.759271 0.089 Uiso 1 1 calc R U . . .
H19C H 0.681011 0.787920 0.756019 0.089 Uiso 1 1 calc R U . . .
C40 C 0.58977(6) 0.05835(15) 0.58812(6) 0.0604(5) Uani 1 1 d . . . . .
H40A H 0.577019 0.029123 0.562737 0.073 Uiso 1 1 calc R U . . .
H40B H 0.591506 0.000366 0.610005 0.073 Uiso 1 1 calc R U . . .
C24 C 0.41372(6) 0.01388(15) 0.65856(7) 0.0592(5) Uani 1 1 d . . . . .
H24A H 0.404222 -0.041433 0.638529 0.071 Uiso 1 1 calc R U . . .
H24B H 0.418770 -0.021367 0.686487 0.071 Uiso 1 1 calc R U . . .
C22 C 0.43920(5) 0.04812(17) 0.56404(8) 0.0651(6) Uani 1 1 d . . . . .
H22A H 0.424130 -0.016183 0.570102 0.078 Uiso 1 1 calc R U . . .
H22B H 0.463621 0.023181 0.556357 0.078 Uiso 1 1 calc R U . . .
C55 C 0.48422(6) 0.31814(16) 0.77500(7) 0.0634(5) Uani 1 1 d . . . . .
H55A H 0.461199 0.336077 0.789210 0.076 Uiso 1 1 calc R U . . .
H55B H 0.490377 0.376537 0.754472 0.076 Uiso 1 1 calc R U . . .
C21 C 0.42356(6) 0.11211(18) 0.52847(6) 0.0616(6) Uani 1 1 d . . . . .
H21A H 0.439444 0.174227 0.521854 0.074 Uiso 1 1 calc R U . . .
H21B H 0.421848 0.066310 0.502440 0.074 Uiso 1 1 calc R U . . .
C52A C 0.54956(10) 0.4271(4) 0.68263(18) 0.0621(12) Uani 0.815(2) 1 d . U P A 1
H52A H 0.540056 0.370712 0.702169 0.075 Uiso 0.815(2) 1 calc R U P A 1
H52B H 0.530664 0.482629 0.678564 0.075 Uiso 0.815(2) 1 calc R U P A 1
C54 C 0.51343(7) 0.30228(17) 0.80724(8) 0.0750(7) Uani 1 1 d . . . . .
H54A H 0.508625 0.344468 0.833676 0.090 Uiso 1 1 calc R U . . .
H54B H 0.536955 0.324452 0.795363 0.090 Uiso 1 1 calc R U . . .
C49A C 0.66039(6) 0.46394(17) 0.66901(7) 0.0454(5) Uani 0.815(2) 1 d . U P A 1
H49A H 0.646406 0.521323 0.654382 0.054 Uiso 0.815(2) 1 calc R U P A 1
H49B H 0.685276 0.490101 0.673085 0.054 Uiso 0.815(2) 1 calc R U P A 1
C46A C 0.57657(11) 0.3932(5) 0.57018(17) 0.0700(14) Uani 0.815(2) 1 d . U P A 1
H46A H 0.560142 0.333369 0.562242 0.084 Uiso 0.815(2) 1 calc R U P A 1
H46B H 0.578708 0.442149 0.545119 0.084 Uiso 0.815(2) 1 calc R U P A 1
C47A C 0.63968(7) 0.42482(19) 0.57440(7) 0.0511(6) Uani 0.815(2) 1 d . U P A 1
H47A H 0.632475 0.497905 0.584293 0.061 Uiso 0.815(2) 1 calc R U P A 1
H47B H 0.646449 0.429272 0.543695 0.061 Uiso 0.815(2) 1 calc R U P A 1
C51A C 0.58224(7) 0.47880(18) 0.70247(10) 0.0619(7) Uani 0.815(2) 1 d . U P A 1
H51A H 0.591337 0.537967 0.683953 0.074 Uiso 0.815(2) 1 calc R U P A 1
H51B H 0.576367 0.509159 0.731056 0.074 Uiso 0.815(2) 1 calc R U P A 1
C45A C 0.56073(7) 0.4557(2) 0.60798(11) 0.0684(8) Uani 0.815(2) 1 d . U P A 1
H45A H 0.576496 0.516913 0.616163 0.082 Uiso 0.815(2) 1 calc R U P A 1
H45B H 0.536680 0.484464 0.600689 0.082 Uiso 0.815(2) 1 calc R U P A 1
Li2 Li 0.39043(7) 0.22998(19) 0.60652(8) 0.0314(5) Uani 1 1 d . . . . .
Li1 Li 0.60838(7) 0.26606(19) 0.64789(8) 0.0318(5) Uani 1 1 d . . . . .
O14B O 0.65723(19) 0.3758(5) 0.6701(3) 0.0452(15) Uani 0.185(2) 1 d . U P A 2
O15B O 0.5898(2) 0.3936(7) 0.7032(3) 0.0544(18) Uani 0.185(2) 1 d . U P A 2
C50B C 0.6513(6) 0.420(2) 0.7093(9) 0.046(2) Uani 0.185(2) 1 d . U P A 2
H50C H 0.670452 0.473142 0.715506 0.055 Uiso 0.185(2) 1 calc R U P A 2
H50D H 0.652749 0.361971 0.731258 0.055 Uiso 0.185(2) 1 calc R U P A 2
C51B C 0.6153(3) 0.4755(9) 0.7131(4) 0.0528(19) Uani 0.185(2) 1 d . U P A 2
H51C H 0.611576 0.503575 0.742521 0.063 Uiso 0.185(2) 1 calc R U P A 2
H51D H 0.613505 0.536469 0.692507 0.063 Uiso 0.185(2) 1 calc R U P A 2
C52B C 0.5581(6) 0.438(2) 0.6911(8) 0.059(3) Uani 0.185(2) 1 d . U P A 2
H52C H 0.554680 0.505432 0.708043 0.071 Uiso 0.185(2) 1 calc R U P A 2
H52D H 0.538713 0.387687 0.699451 0.071 Uiso 0.185(2) 1 calc R U P A 2
C45B C 0.5532(3) 0.4642(9) 0.6485(4) 0.0582(19) Uani 0.185(2) 1 d . U P A 2
H45C H 0.569166 0.525529 0.641059 0.070 Uiso 0.185(2) 1 calc R U P A 2
H45D H 0.528122 0.488748 0.644322 0.070 Uiso 0.185(2) 1 calc R U P A 2
O16B O 0.5603(3) 0.3756(8) 0.6193(3) 0.0475(18) Uani 0.185(2) 1 d . U P A 2
C46B C 0.5665(6) 0.406(2) 0.5777(9) 0.056(3) Uani 0.185(2) 1 d . U P A 2
H46C H 0.551693 0.470022 0.570666 0.068 Uiso 0.185(2) 1 calc R U P A 2
H46D H 0.559399 0.346162 0.558185 0.068 Uiso 0.185(2) 1 calc R U P A 2
C47B C 0.6075(3) 0.4335(9) 0.5707(4) 0.060(2) Uani 0.185(2) 1 d . U P A 2
H47C H 0.612457 0.438781 0.539571 0.072 Uiso 0.185(2) 1 calc R U P A 2
H47D H 0.612798 0.504912 0.583810 0.072 Uiso 0.185(2) 1 calc R U P A 2
O13B O 0.6294(2) 0.3576(7) 0.5883(3) 0.0482(16) Uani 0.185(2) 1 d . U P A 2
C48B C 0.6633(6) 0.3960(19) 0.5938(7) 0.046(2) Uani 0.185(2) 1 d . U P A 2
H48C H 0.668529 0.449635 0.570968 0.055 Uiso 0.185(2) 1 calc R U P A 2
H48D H 0.680520 0.335449 0.590651 0.055 Uiso 0.185(2) 1 calc R U P A 2
C49B C 0.6689(3) 0.4503(8) 0.6384(3) 0.0483(18) Uani 0.185(2) 1 d . U P A 2
H49C H 0.694569 0.468047 0.642661 0.058 Uiso 0.185(2) 1 calc R U P A 2
H49D H 0.654825 0.518219 0.640223 0.058 Uiso 0.185(2) 1 calc R U 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 P2 2.0748(6) . ?
P1 C1 1.7807(14) . ?
P4 P5 2.0761(6) . ?
P4 C11 1.7802(14) . ?
P3 P2 2.0763(6) . ?
P3 C2 1.7819(14) . ?
P5 P6 2.0732(6) . ?
P6 C12 1.7772(15) . ?
O6 C32 1.4199(19) . ?
O6 C33 1.4297(19) . ?
O6 Li2 2.275(3) . ?
O12 C44 1.4238(19) . ?
O12 C37 1.4238(19) . ?
O12 Li1 2.280(3) . ?
O11 C43 1.4300(19) . ?
O11 C42 1.4142(19) . ?
O11 Li1 2.378(3) . ?
O3 C27 1.4321(19) . ?
O3 C26 1.419(2) . ?
O3 Li2 2.322(3) . ?
O7 C34 1.425(2) . ?
O7 C35 1.429(2) . ?
O7 Li2 2.307(3) . ?
O17 C56 1.425(2) . ?
O17 C53 1.412(2) . ?
O5 C31 1.430(2) . ?
O5 C30 1.416(2) . ?
O5 Li2 2.449(3) . ?
O8 C29 1.426(2) . ?
O8 C36 1.426(2) . ?
O8 Li2 2.379(3) . ?
O9 C38 1.429(2) . ?
O9 C39 1.428(2) . ?
O9 Li1 2.319(3) . ?
O4 C28 1.410(2) . ?
O4 C21 1.430(2) . ?
O4 Li2 2.298(3) . ?
O2 C25 1.435(2) . ?
O2 C24 1.415(2) . ?
O2 Li2 2.413(3) . ?
O1 C23 1.441(2) . ?
O1 C22 1.419(2) . ?
O1 Li2 2.338(3) . ?
O10 C41 1.421(2) . ?
O10 C40 1.420(2) . ?
O10 Li1 2.411(3) . ?
O14A C48A 1.417(5) . ?
O14A C49A 1.426(3) . ?
O14A Li1 2.300(3) . ?
O16A C52A 1.442(6) . ?
O16A C45A 1.417(3) . ?
O16A Li1 2.333(3) . ?
O15A C50A 1.420(6) . ?
O15A C51A 1.422(3) . ?
O15A Li1 2.417(3) . ?
O13A C46A 1.421(5) . ?
O13A C47A 1.428(3) . ?
O13A Li1 2.350(3) . ?
C1 C2 1.418(2) . ?
C1 C3 1.569(2) . ?
C11 C12 1.416(2) . ?
C11 C13 1.571(2) . ?
C2 C7 1.569(2) . ?
C12 C17 1.570(2) . ?
C3 C6 1.542(2) . ?
C3 C4 1.551(2) . ?
C3 C5 1.543(2) . ?
C13 C15 1.538(2) . ?
C13 C16 1.547(2) . ?
C13 C14 1.546(2) . ?
C7 C9 1.542(2) . ?
C7 C8 1.545(2) . ?
C7 C10 1.546(2) . ?
C17 C18 1.544(2) . ?
C17 C20 1.542(2) . ?
C17 C19 1.548(2) . ?
C44 H44A 0.9900 . ?
C44 H44B 0.9900 . ?
C44 C43 1.495(2) . ?
C43 H43A 0.9900 . ?
C43 H43B 0.9900 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C32 H32A 0.9900 . ?
C32 H32B 0.9900 . ?
C32 C31 1.494(2) . ?
C42 H42A 0.9900 . ?
C42 H42B 0.9900 . ?
C42 C41 1.498(3) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C33 H33A 0.9900 . ?
C33 H33B 0.9900 . ?
C33 C34 1.506(2) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C34 H34A 0.9900 . ?
C34 H34B 0.9900 . ?
C35 H35A 0.9900 . ?
C35 H35B 0.9900 . ?
C35 C36 1.502(3) . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C25 C26 1.509(2) . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C38 H38A 0.9900 . ?
C38 H38B 0.9900 . ?
C38 C37 1.497(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?
C27 C28 1.486(3) . ?
C37 H37A 0.9900 . ?
C37 H37B 0.9900 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C48A H48A 0.9900 . ?
C48A H48B 0.9900 . ?
C48A C47A 1.518(4) . ?
C41 H41A 0.9900 . ?
C41 H41B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C29 H29A 0.9900 . ?
C29 H29B 0.9900 . ?
C29 C30 1.501(3) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C28 H28A 0.9900 . ?
C28 H28B 0.9900 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C30 H30A 0.9900 . ?
C30 H30B 0.9900 . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C24 1.485(3) . ?
C39 H39A 0.9900 . ?
C39 H39B 0.9900 . ?
C39 C40 1.499(3) . ?
C36 H36A 0.9900 . ?
C36 H36B 0.9900 . ?
C56 H56A 0.9900 . ?
C56 H56B 0.9900 . ?
C56 C55 1.490(3) . ?
C50A H50A 0.9900 . ?
C50A H50B 0.9900 . ?
C50A C49A 1.515(6) . ?
C53 H53A 0.9900 . ?
C53 H53B 0.9900 . ?
C53 C54 1.513(3) . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C40 H40A 0.9900 . ?
C40 H40B 0.9900 . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.479(3) . ?
C55 H55A 0.9900 . ?
C55 H55B 0.9900 . ?
C55 C54 1.493(3) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C52A H52A 0.9900 . ?
C52A H52B 0.9900 . ?
C52A C51A 1.507(4) . ?
C54 H54A 0.9900 . ?
C54 H54B 0.9900 . ?
C49A H49A 0.9900 . ?
C49A H49B 0.9900 . ?
C46A H46A 0.9900 . ?
C46A H46B 0.9900 . ?
C46A C45A 1.526(6) . ?
C47A H47A 0.9900 . ?
C47A H47B 0.9900 . ?
C51A H51A 0.9900 . ?
C51A H51B 0.9900 . ?
C45A H45A 0.9900 . ?
C45A H45B 0.9900 . ?
Li1 O14B 2.372(7) . ?
Li1 O15B 2.433(10) . ?
Li1 O16B 2.414(9) . ?
Li1 O13B 2.308(8) . ?
O14B C50B 1.35(3) . ?
O14B C49B 1.418(13) . ?
O15B C51B 1.422(14) . ?
O15B C52B 1.36(2) . ?
C50B H50C 0.9900 . ?
C50B H50D 0.9900 . ?
C50B C51B 1.51(2) . ?
C51B H51C 0.9900 . ?
C51B H51D 0.9900 . ?
C52B H52C 0.9900 . ?
C52B H52D 0.9900 . ?
C52B C45B 1.38(3) . ?
C45B H45C 0.9900 . ?
C45B H45D 0.9900 . ?
C45B O16B 1.446(16) . ?
O16B C46B 1.37(3) . ?
C46B H46C 0.9900 . ?
C46B H46D 0.9900 . ?
C46B C47B 1.58(2) . ?
C47B H47C 0.9900 . ?
C47B H47D 0.9900 . ?
C47B O13B 1.357(15) . ?
O13B C48B 1.36(2) . ?
C48B H48C 0.9900 . ?
C48B H48D 0.9900 . ?
C48B C49B 1.56(3) . ?
C49B H49C 0.9900 . ?
C49B H49D 0.9900 . ?

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 P2 102.96(5) . . ?
C11 P4 P5 102.71(5) . . ?
C2 P3 P2 102.79(5) . . ?
P1 P2 P3 97.29(2) . . ?
P6 P5 P4 97.28(2) . . ?
C12 P6 P5 102.96(5) . . ?
C32 O6 C33 113.23(12) . . ?
C32 O6 Li2 117.06(12) . . ?
C33 O6 Li2 108.94(11) . . ?
C44 O12 C37 113.30(12) . . ?
C44 O12 Li1 116.26(11) . . ?
C37 O12 Li1 109.58(11) . . ?
C43 O11 Li1 107.92(11) . . ?
C42 O11 C43 113.45(12) . . ?
C42 O11 Li1 114.76(11) . . ?
C27 O3 Li2 109.21(11) . . ?
C26 O3 C27 113.46(13) . . ?
C26 O3 Li2 115.54(12) . . ?
C34 O7 C35 113.89(13) . . ?
C34 O7 Li2 114.10(11) . . ?
C35 O7 Li2 111.24(12) . . ?
C53 O17 C56 108.51(14) . . ?
C31 O5 Li2 106.78(11) . . ?
C30 O5 C31 113.80(13) . . ?
C30 O5 Li2 112.48(11) . . ?
C29 O8 Li2 111.29(12) . . ?
C36 O8 C29 113.29(14) . . ?
C36 O8 Li2 113.28(12) . . ?
C38 O9 Li1 113.61(11) . . ?
C39 O9 C38 113.76(14) . . ?
C39 O9 Li1 111.87(13) . . ?
C28 O4 C21 114.45(14) . . ?
C28 O4 Li2 116.48(12) . . ?
C21 O4 Li2 109.72(12) . . ?
C25 O2 Li2 108.45(11) . . ?
C24 O2 C25 113.68(14) . . ?
C24 O2 Li2 112.95(13) . . ?
C23 O1 Li2 109.69(12) . . ?
C22 O1 C23 115.40(15) . . ?
C22 O1 Li2 113.14(13) . . ?
C41 O10 Li1 109.73(12) . . ?
C40 O10 C41 112.88(14) . . ?
C40 O10 Li1 113.07(13) . . ?
C48A O14A C49A 113.4(2) . . ?
C48A O14A Li1 111.2(2) . . ?
C49A O14A Li1 115.48(14) . . ?
C52A O16A Li1 110.9(2) . . ?
C45A O16A C52A 113.2(3) . . ?
C45A O16A Li1 114.28(19) . . ?
C50A O15A C51A 112.4(2) . . ?
C50A O15A Li1 109.2(2) . . ?
C51A O15A Li1 114.57(19) . . ?
C46A O13A C47A 113.8(3) . . ?
C46A O13A Li1 109.0(2) . . ?
C47A O13A Li1 115.29(16) . . ?
C2 C1 P1 118.32(10) . . ?
C2 C1 C3 130.09(13) . . ?
C3 C1 P1 111.51(10) . . ?
C12 C11 P4 118.57(10) . . ?
C12 C11 C13 129.76(13) . . ?
C13 C11 P4 111.61(10) . . ?
C1 C2 P3 118.54(10) . . ?
C1 C2 C7 129.75(12) . . ?
C7 C2 P3 111.64(10) . . ?
C11 C12 P6 118.38(11) . . ?
C11 C12 C17 130.11(13) . . ?
C17 C12 P6 111.45(11) . . ?
C6 C3 C1 115.27(13) . . ?
C6 C3 C4 103.12(13) . . ?
C6 C3 C5 111.17(14) . . ?
C4 C3 C1 111.50(13) . . ?
C5 C3 C1 110.28(13) . . ?
C5 C3 C4 104.80(14) . . ?
C15 C13 C11 110.08(12) . . ?
C15 C13 C16 111.40(13) . . ?
C15 C13 C14 105.42(14) . . ?
C16 C13 C11 114.54(13) . . ?
C14 C13 C11 111.68(12) . . ?
C14 C13 C16 103.17(13) . . ?
C9 C7 C2 110.17(12) . . ?
C9 C7 C8 111.06(13) . . ?
C9 C7 C10 105.14(13) . . ?
C8 C7 C2 114.66(13) . . ?
C8 C7 C10 103.27(13) . . ?
C10 C7 C2 111.97(12) . . ?
C18 C17 C12 114.97(14) . . ?
C18 C17 C19 103.13(14) . . ?
C20 C17 C12 110.22(13) . . ?
C20 C17 C18 111.06(15) . . ?
C20 C17 C19 105.13(15) . . ?
C19 C17 C12 111.72(14) . . ?
O12 C44 H44A 110.3 . . ?
O12 C44 H44B 110.3 . . ?
O12 C44 C43 106.90(12) . . ?
H44A C44 H44B 108.6 . . ?
C43 C44 H44A 110.3 . . ?
C43 C44 H44B 110.3 . . ?
O11 C43 C44 111.21(12) . . ?
O11 C43 H43A 109.4 . . ?
O11 C43 H43B 109.4 . . ?
C44 C43 H43A 109.4 . . ?
C44 C43 H43B 109.4 . . ?
H43A C43 H43B 108.0 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O6 C32 H32A 110.3 . . ?
O6 C32 H32B 110.3 . . ?
O6 C32 C31 106.94(13) . . ?
H32A C32 H32B 108.6 . . ?
C31 C32 H32A 110.3 . . ?
C31 C32 H32B 110.3 . . ?
O11 C42 H42A 110.4 . . ?
O11 C42 H42B 110.4 . . ?
O11 C42 C41 106.44(13) . . ?
H42A C42 H42B 108.6 . . ?
C41 C42 H42A 110.4 . . ?
C41 C42 H42B 110.4 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O5 C31 C32 111.71(13) . . ?
O5 C31 H31A 109.3 . . ?
O5 C31 H31B 109.3 . . ?
C32 C31 H31A 109.3 . . ?
C32 C31 H31B 109.3 . . ?
H31A C31 H31B 107.9 . . ?
O6 C33 H33A 109.5 . . ?
O6 C33 H33B 109.5 . . ?
O6 C33 C34 110.87(14) . . ?
H33A C33 H33B 108.1 . . ?
C34 C33 H33A 109.5 . . ?
C34 C33 H33B 109.5 . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O7 C34 C33 105.88(13) . . ?
O7 C34 H34A 110.6 . . ?
O7 C34 H34B 110.6 . . ?
C33 C34 H34A 110.6 . . ?
C33 C34 H34B 110.6 . . ?
H34A C34 H34B 108.7 . . ?
O7 C35 H35A 109.4 . . ?
O7 C35 H35B 109.4 . . ?
O7 C35 C36 110.96(14) . . ?
H35A C35 H35B 108.0 . . ?
C36 C35 H35A 109.4 . . ?
C36 C35 H35B 109.4 . . ?
O2 C25 H25A 109.4 . . ?
O2 C25 H25B 109.4 . . ?
O2 C25 C26 110.97(14) . . ?
H25A C25 H25B 108.0 . . ?
C26 C25 H25A 109.4 . . ?
C26 C25 H25B 109.4 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
O9 C38 H38A 110.5 . . ?
O9 C38 H38B 110.5 . . ?
O9 C38 C37 106.24(14) . . ?
H38A C38 H38B 108.7 . . ?
C37 C38 H38A 110.5 . . ?
C37 C38 H38B 110.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
O3 C27 H27A 109.4 . . ?
O3 C27 H27B 109.4 . . ?
O3 C27 C28 111.18(14) . . ?
H27A C27 H27B 108.0 . . ?
C28 C27 H27A 109.4 . . ?
C28 C27 H27B 109.4 . . ?
O12 C37 C38 111.10(14) . . ?
O12 C37 H37A 109.4 . . ?
O12 C37 H37B 109.4 . . ?
C38 C37 H37A 109.4 . . ?
C38 C37 H37B 109.4 . . ?
H37A C37 H37B 108.0 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
O14A C48A H48A 109.6 . . ?
O14A C48A H48B 109.6 . . ?
O14A C48A C47A 110.3(3) . . ?
H48A C48A H48B 108.1 . . ?
C47A C48A H48A 109.6 . . ?
C47A C48A H48B 109.6 . . ?
O10 C41 C42 111.66(14) . . ?
O10 C41 H41A 109.3 . . ?
O10 C41 H41B 109.3 . . ?
C42 C41 H41A 109.3 . . ?
C42 C41 H41B 109.3 . . ?
H41A C41 H41B 107.9 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O8 C29 H29A 109.4 . . ?
O8 C29 H29B 109.4 . . ?
O8 C29 C30 111.26(14) . . ?
H29A C29 H29B 108.0 . . ?
C30 C29 H29A 109.4 . . ?
C30 C29 H29B 109.4 . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
O4 C28 C27 106.86(14) . . ?
O4 C28 H28A 110.3 . . ?
O4 C28 H28B 110.3 . . ?
C27 C28 H28A 110.3 . . ?
C27 C28 H28B 110.3 . . ?
H28A C28 H28B 108.6 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
O3 C26 C25 106.29(14) . . ?
O3 C26 H26A 110.5 . . ?
O3 C26 H26B 110.5 . . ?
C25 C26 H26A 110.5 . . ?
C25 C26 H26B 110.5 . . ?
H26A C26 H26B 108.7 . . ?
O5 C30 C29 107.17(14) . . ?
O5 C30 H30A 110.3 . . ?
O5 C30 H30B 110.3 . . ?
C29 C30 H30A 110.3 . . ?
C29 C30 H30B 110.3 . . ?
H30A C30 H30B 108.5 . . ?
O1 C23 H23A 109.2 . . ?
O1 C23 H23B 109.2 . . ?
O1 C23 C24 111.94(16) . . ?
H23A C23 H23B 107.9 . . ?
C24 C23 H23A 109.2 . . ?
C24 C23 H23B 109.2 . . ?
O9 C39 H39A 109.4 . . ?
O9 C39 H39B 109.4 . . ?
O9 C39 C40 111.12(14) . . ?
H39A C39 H39B 108.0 . . ?
C40 C39 H39A 109.4 . . ?
C40 C39 H39B 109.4 . . ?
O8 C36 C35 107.26(14) . . ?
O8 C36 H36A 110.3 . . ?
O8 C36 H36B 110.3 . . ?
C35 C36 H36A 110.3 . . ?
C35 C36 H36B 110.3 . . ?
H36A C36 H36B 108.5 . . ?
O17 C56 H56A 109.9 . . ?
O17 C56 H56B 109.9 . . ?
O17 C56 C55 109.11(16) . . ?
H56A C56 H56B 108.3 . . ?
C55 C56 H56A 109.9 . . ?
C55 C56 H56B 109.9 . . ?
O15A C50A H50A 109.5 . . ?
O15A C50A H50B 109.5 . . ?
O15A C50A C49A 110.7(4) . . ?
H50A C50A H50B 108.1 . . ?
C49A C50A H50A 109.5 . . ?
C49A C50A H50B 109.5 . . ?
O17 C53 H53A 110.7 . . ?
O17 C53 H53B 110.7 . . ?
O17 C53 C54 105.20(17) . . ?
H53A C53 H53B 108.8 . . ?
C54 C53 H53A 110.7 . . ?
C54 C53 H53B 110.7 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
O10 C40 C39 107.38(15) . . ?
O10 C40 H40A 110.2 . . ?
O10 C40 H40B 110.2 . . ?
C39 C40 H40A 110.2 . . ?
C39 C40 H40B 110.2 . . ?
H40A C40 H40B 108.5 . . ?
O2 C24 C23 107.03(15) . . ?
O2 C24 H24A 110.3 . . ?
O2 C24 H24B 110.3 . . ?
C23 C24 H24A 110.3 . . ?
C23 C24 H24B 110.3 . . ?
H24A C24 H24B 108.6 . . ?
O1 C22 H22A 110.3 . . ?
O1 C22 H22B 110.3 . . ?
O1 C22 C21 107.07(16) . . ?
H22A C22 H22B 108.6 . . ?
C21 C22 H22A 110.3 . . ?
C21 C22 H22B 110.3 . . ?
C56 C55 H55A 111.1 . . ?
C56 C55 H55B 111.1 . . ?
C56 C55 C54 103.25(17) . . ?
H55A C55 H55B 109.1 . . ?
C54 C55 H55A 111.1 . . ?
C54 C55 H55B 111.1 . . ?
O4 C21 C22 110.82(15) . . ?
O4 C21 H21A 109.5 . . ?
O4 C21 H21B 109.5 . . ?
C22 C21 H21A 109.5 . . ?
C22 C21 H21B 109.5 . . ?
H21A C21 H21B 108.1 . . ?
O16A C52A H52A 109.5 . . ?
O16A C52A H52B 109.5 . . ?
O16A C52A C51A 110.5(3) . . ?
H52A C52A H52B 108.1 . . ?
C51A C52A H52A 109.5 . . ?
C51A C52A H52B 109.5 . . ?
C53 C54 H54A 111.0 . . ?
C53 C54 H54B 111.0 . . ?
C55 C54 C53 103.90(17) . . ?
C55 C54 H54A 111.0 . . ?
C55 C54 H54B 111.0 . . ?
H54A C54 H54B 109.0 . . ?
O14A C49A C50A 106.9(2) . . ?
O14A C49A H49A 110.3 . . ?
O14A C49A H49B 110.3 . . ?
C50A C49A H49A 110.3 . . ?
C50A C49A H49B 110.3 . . ?
H49A C49A H49B 108.6 . . ?
O13A C46A H46A 109.3 . . ?
O13A C46A H46B 109.3 . . ?
O13A C46A C45A 111.8(4) . . ?
H46A C46A H46B 107.9 . . ?
C45A C46A H46A 109.3 . . ?
C45A C46A H46B 109.3 . . ?
O13A C47A C48A 106.7(2) . . ?
O13A C47A H47A 110.4 . . ?
O13A C47A H47B 110.4 . . ?
C48A C47A H47A 110.4 . . ?
C48A C47A H47B 110.4 . . ?
H47A C47A H47B 108.6 . . ?
O15A C51A C52A 106.2(3) . . ?
O15A C51A H51A 110.5 . . ?
O15A C51A H51B 110.5 . . ?
C52A C51A H51A 110.5 . . ?
C52A C51A H51B 110.5 . . ?
H51A C51A H51B 108.7 . . ?
O16A C45A C46A 105.0(3) . . ?
O16A C45A H45A 110.8 . . ?
O16A C45A H45B 110.8 . . ?
C46A C45A H45A 110.8 . . ?
C46A C45A H45B 110.8 . . ?
H45A C45A H45B 108.8 . . ?
O6 Li2 O3 81.40(9) . . ?
O6 Li2 O7 73.32(8) . . ?
O6 Li2 O5 71.48(8) . . ?
O6 Li2 O8 111.58(10) . . ?
O6 Li2 O4 144.23(13) . . ?
O6 Li2 O2 79.22(8) . . ?
O6 Li2 O1 141.29(12) . . ?
O3 Li2 O5 143.80(12) . . ?
O3 Li2 O8 144.19(12) . . ?
O3 Li2 O2 71.40(8) . . ?
O3 Li2 O1 111.30(10) . . ?
O7 Li2 O3 81.06(9) . . ?
O7 Li2 O5 112.24(10) . . ?
O7 Li2 O8 71.88(8) . . ?
O7 Li2 O2 143.54(12) . . ?
O7 Li2 O1 142.92(12) . . ?
O8 Li2 O5 70.29(8) . . ?
O8 Li2 O2 142.18(12) . . ?
O4 Li2 O3 71.84(8) . . ?
O4 Li2 O7 79.32(9) . . ?
O4 Li2 O5 141.93(12) . . ?
O4 Li2 O8 80.30(9) . . ?
O4 Li2 O2 112.69(10) . . ?
O4 Li2 O1 72.43(8) . . ?
O2 Li2 O5 80.16(8) . . ?
O1 Li2 O5 78.97(9) . . ?
O1 Li2 O8 79.98(9) . . ?
O1 Li2 O2 71.45(8) . . ?
O12 Li1 O11 72.16(8) . . ?
O12 Li1 O9 73.03(8) . . ?
O12 Li1 O10 112.31(10) . . ?
O12 Li1 O14A 82.64(9) . . ?
O12 Li1 O16A 140.57(13) . . ?
O12 Li1 O15A 79.30(10) . . ?
O12 Li1 O13A 145.05(13) . . ?
O12 Li1 O14B 71.83(19) . . ?
O12 Li1 O15B 89.2(2) . . ?
O12 Li1 O16B 157.2(3) . . ?
O12 Li1 O13B 128.6(3) . . ?
O11 Li1 O10 70.37(8) . . ?
O11 Li1 O15A 82.43(9) . . ?
O11 Li1 O15B 72.7(2) . . ?
O11 Li1 O16B 89.9(2) . . ?
O9 Li1 O11 111.24(10) . . ?
O9 Li1 O10 71.15(8) . . ?
O9 Li1 O16A 144.29(14) . . ?
O9 Li1 O15A 142.80(13) . . ?
O9 Li1 O13A 79.72(10) . . ?
O9 Li1 O14B 93.8(2) . . ?
O9 Li1 O15B 158.8(3) . . ?
O9 Li1 O16B 127.9(3) . . ?
O10 Li1 O15A 144.17(13) . . ?
O10 Li1 O15B 127.9(3) . . ?
O10 Li1 O16B 72.7(2) . . ?
O14A Li1 O11 146.67(13) . . ?
O14A Li1 O9 80.58(9) . . ?
O14A Li1 O10 141.38(13) . . ?
O14A Li1 O16A 110.03(11) . . ?
O14A Li1 O15A 71.52(9) . . ?
O14A Li1 O13A 71.52(9) . . ?
O16A Li1 O11 79.07(10) . . ?
O16A Li1 O10 81.47(10) . . ?
O16A Li1 O15A 70.55(10) . . ?
O16A Li1 O13A 72.30(11) . . ?
O13A Li1 O11 139.79(13) . . ?
O13A Li1 O10 77.86(9) . . ?
O13A Li1 O15A 112.68(11) . . ?
O14B Li1 O11 126.9(2) . . ?
O14B Li1 O10 161.3(2) . . ?
O14B Li1 O15B 69.1(3) . . ?
O14B Li1 O16B 111.0(3) . . ?
O16B Li1 O15B 71.8(3) . . ?
O13B Li1 O11 158.1(3) . . ?
O13B Li1 O9 74.1(2) . . ?
O13B Li1 O10 92.6(2) . . ?
O13B Li1 O14B 72.2(3) . . ?
O13B Li1 O15B 110.4(3) . . ?
O13B Li1 O16B 71.5(3) . . ?
C50B O14B Li1 111.5(12) . . ?
C50B O14B C49B 114.7(14) . . ?
C49B O14B Li1 113.7(6) . . ?
C51B O15B Li1 114.9(7) . . ?
C52B O15B Li1 108.3(13) . . ?
C52B O15B C51B 110.7(14) . . ?
O14B C50B H50C 108.9 . . ?
O14B C50B H50D 108.9 . . ?
O14B C50B C51B 113.4(19) . . ?
H50C C50B H50D 107.7 . . ?
C51B C50B H50C 108.9 . . ?
C51B C50B H50D 108.9 . . ?
O15B C51B C50B 104.7(13) . . ?
O15B C51B H51C 110.8 . . ?
O15B C51B H51D 110.8 . . ?
C50B C51B H51C 110.8 . . ?
C50B C51B H51D 110.8 . . ?
H51C C51B H51D 108.9 . . ?
O15B C52B H52C 107.7 . . ?
O15B C52B H52D 107.7 . . ?
O15B C52B C45B 119(2) . . ?
H52C C52B H52D 107.1 . . ?
C45B C52B H52C 107.7 . . ?
C45B C52B H52D 107.7 . . ?
C52B C45B H45C 108.8 . . ?
C52B C45B H45D 108.8 . . ?
C52B C45B O16B 113.9(14) . . ?
H45C C45B H45D 107.7 . . ?
O16B C45B H45C 108.8 . . ?
O16B C45B H45D 108.8 . . ?
C45B O16B Li1 109.1(6) . . ?
C46B O16B Li1 112.1(11) . . ?
C46B O16B C45B 114.8(16) . . ?
O16B C46B H46C 109.5 . . ?
O16B C46B H46D 109.5 . . ?
O16B C46B C47B 110.6(18) . . ?
H46C C46B H46D 108.1 . . ?
C47B C46B H46C 109.5 . . ?
C47B C46B H46D 109.5 . . ?
C46B C47B H47C 109.2 . . ?
C46B C47B H47D 109.2 . . ?
H47C C47B H47D 107.9 . . ?
O13B C47B C46B 112.1(13) . . ?
O13B C47B H47C 109.2 . . ?
O13B C47B H47D 109.2 . . ?
C47B O13B Li1 117.3(7) . . ?
C47B O13B C48B 111.6(13) . . ?
C48B O13B Li1 112.7(11) . . ?
O13B C48B H48C 109.0 . . ?
O13B C48B H48D 109.0 . . ?
O13B C48B C49B 112.7(17) . . ?
H48C C48B H48D 107.8 . . ?
C49B C48B H48C 109.0 . . ?
C49B C48B H48D 109.0 . . ?
O14B C49B C48B 107.6(11) . . ?
O14B C49B H49C 110.2 . . ?
O14B C49B H49D 110.2 . . ?
C48B C49B H49C 110.2 . . ?
C48B C49B H49D 110.2 . . ?
H49C C49B H49D 108.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 C1 C2 P3 -3.76(16) . . . . ?
P1 C1 C2 C7 179.49(12) . . . . ?
P1 C1 C3 C6 136.66(12) . . . . ?
P1 C1 C3 C4 19.54(16) . . . . ?
P1 C1 C3 C5 -96.45(14) . . . . ?
P4 C11 C12 P6 3.79(16) . . . . ?
P4 C11 C12 C17 -179.09(12) . . . . ?
P4 C11 C13 C15 96.55(14) . . . . ?
P4 C11 C13 C16 -137.01(12) . . . . ?
P4 C11 C13 C14 -20.19(16) . . . . ?
P3 C2 C7 C9 -97.52(13) . . . . ?
P3 C2 C7 C8 136.33(12) . . . . ?
P3 C2 C7 C10 19.10(16) . . . . ?
P2 P1 C1 C2 2.88(12) . . . . ?
P2 P1 C1 C3 179.92(9) . . . . ?
P2 P3 C2 C1 2.58(12) . . . . ?
P2 P3 C2 C7 179.89(9) . . . . ?
P5 P4 C11 C12 -2.67(12) . . . . ?
P5 P4 C11 C13 179.92(9) . . . . ?
P5 P6 C12 C11 -2.83(12) . . . . ?
P5 P6 C12 C17 179.54(9) . . . . ?
P6 C12 C17 C18 -136.32(13) . . . . ?
P6 C12 C17 C20 97.24(15) . . . . ?
P6 C12 C17 C19 -19.25(17) . . . . ?
O6 C32 C31 O5 57.99(18) . . . . ?
O6 C33 C34 O7 57.62(18) . . . . ?
O12 C44 C43 O11 56.83(17) . . . . ?
O11 C42 C41 O10 59.11(19) . . . . ?
O3 C27 C28 O4 -54.79(19) . . . . ?
O7 C35 C36 O8 56.6(2) . . . . ?
O17 C56 C55 C54 13.4(2) . . . . ?
O17 C53 C54 C55 32.2(3) . . . . ?
O8 C29 C30 O5 59.81(19) . . . . ?
O9 C38 C37 O12 57.46(18) . . . . ?
O9 C39 C40 O10 56.9(2) . . . . ?
O2 C25 C26 O3 -59.15(19) . . . . ?
O1 C23 C24 O2 -59.0(2) . . . . ?
O1 C22 C21 O4 -58.3(2) . . . . ?
O14A C48A C47A O13A -54.5(4) . . . . ?
O16A C52A C51A O15A -57.8(4) . . . . ?
O15A C50A C49A O14A -57.9(3) . . . . ?
O13A C46A C45A O16A -59.6(4) . . . . ?
C1 C2 C7 C9 79.4(2) . . . . ?
C1 C2 C7 C8 -46.7(2) . . . . ?
C1 C2 C7 C10 -163.97(15) . . . . ?
C11 C12 C17 C18 46.4(2) . . . . ?
C11 C12 C17 C20 -80.0(2) . . . . ?
C11 C12 C17 C19 163.47(16) . . . . ?
C2 C1 C3 C6 -46.7(2) . . . . ?
C2 C1 C3 C4 -163.87(15) . . . . ?
C2 C1 C3 C5 80.1(2) . . . . ?
C12 C11 C13 C15 -80.49(19) . . . . ?
C12 C11 C13 C16 46.0(2) . . . . ?
C12 C11 C13 C14 162.77(15) . . . . ?
C3 C1 C2 P3 179.84(12) . . . . ?
C3 C1 C2 C7 3.1(3) . . . . ?
C13 C11 C12 P6 -179.34(12) . . . . ?
C13 C11 C12 C17 -2.2(3) . . . . ?
C44 O12 C37 C38 82.42(17) . . . . ?
C43 O11 C42 C41 -166.61(13) . . . . ?
C32 O6 C33 C34 82.04(17) . . . . ?
C42 O11 C43 C44 80.93(17) . . . . ?
C31 O5 C30 C29 -163.46(14) . . . . ?
C33 O6 C32 C31 -168.00(14) . . . . ?
C34 O7 C35 C36 83.07(18) . . . . ?
C35 O7 C34 C33 -165.37(14) . . . . ?
C25 O2 C24 C23 162.73(16) . . . . ?
C38 O9 C39 C40 83.3(2) . . . . ?
C27 O3 C26 C25 169.35(14) . . . . ?
C37 O12 C44 C43 -165.61(13) . . . . ?
C48A O14A C49A C50A 172.3(3) . . . . ?
C41 O10 C40 C39 -163.48(15) . . . . ?
C29 O8 C36 C35 -165.31(15) . . . . ?
C28 O4 C21 C22 -84.62(19) . . . . ?
C26 O3 C27 C28 -82.16(18) . . . . ?
C30 O5 C31 C32 78.76(18) . . . . ?
C23 O1 C22 C21 165.95(16) . . . . ?
C39 O9 C38 C37 -166.28(15) . . . . ?
C36 O8 C29 C30 82.31(18) . . . . ?
C56 O17 C53 C54 -24.2(2) . . . . ?
C56 C55 C54 C53 -27.1(2) . . . . ?
C50A O15A C51A C52A 161.9(4) . . . . ?
C53 O17 C56 C55 6.9(2) . . . . ?
C40 O10 C41 C42 81.05(19) . . . . ?
C24 O2 C25 C26 -80.47(19) . . . . ?
C22 O1 C23 C24 -80.5(2) . . . . ?
C21 O4 C28 C27 164.15(15) . . . . ?
C52A O16A C45A C46A 170.3(3) . . . . ?
C49A O14A C48A C47A -81.7(3) . . . . ?
C46A O13A C47A C48A 159.6(3) . . . . ?
C47A O13A C46A C45A -83.9(4) . . . . ?
C51A O15A C50A C49A -84.1(3) . . . . ?
C45A O16A C52A C51A -78.9(4) . . . . ?
Li2 O6 C32 C31 -39.99(17) . . . . ?
Li2 O6 C33 C34 -50.08(16) . . . . ?
Li2 O3 C27 C28 48.30(17) . . . . ?
Li2 O3 C26 C25 42.13(18) . . . . ?
Li2 O7 C34 C33 -36.16(17) . . . . ?
Li2 O7 C35 C36 -47.57(18) . . . . ?
Li2 O5 C31 C32 -45.95(16) . . . . ?
Li2 O5 C30 C29 -41.86(17) . . . . ?
Li2 O8 C29 C30 -46.72(18) . . . . ?
Li2 O8 C36 C35 -37.31(18) . . . . ?
Li2 O4 C28 C27 34.32(19) . . . . ?
Li2 O4 C21 C22 48.49(19) . . . . ?
Li2 O2 C25 C26 46.05(17) . . . . ?
Li2 O2 C24 C23 38.6(2) . . . . ?
Li2 O1 C23 C24 48.70(19) . . . . ?
Li2 O1 C22 C21 38.47(19) . . . . ?
Li1 O12 C44 C43 -37.34(16) . . . . ?
Li1 O12 C37 C38 -49.22(17) . . . . ?
Li1 O11 C43 C44 -47.38(15) . . . . ?
Li1 O11 C42 C41 -41.91(17) . . . . ?
Li1 O9 C38 C37 -36.75(17) . . . . ?
Li1 O9 C39 C40 -47.10(19) . . . . ?
Li1 O10 C41 C42 -46.05(17) . . . . ?
Li1 O10 C40 C39 -38.17(18) . . . . ?
Li1 O14A C48A C47A 50.3(4) . . . . ?
Li1 O14A C49A C50A 42.3(3) . . . . ?
Li1 O16A C52A C51A 51.0(4) . . . . ?
Li1 O16A C45A C46A 42.1(3) . . . . ?
Li1 O15A C50A C49A 44.2(3) . . . . ?
Li1 O15A C51A C52A 36.5(3) . . . . ?
Li1 O13A C46A C45A 46.4(4) . . . . ?
Li1 O13A C47A C48A 32.6(3) . . . . ?
Li1 O14B C50B C51B -50(2) . . . . ?
Li1 O14B C49B C48B -33.2(12) . . . . ?
Li1 O15B C51B C50B -36.1(15) . . . . ?
Li1 O15B C52B C45B -39(2) . . . . ?
Li1 O16B C46B C47B -39(2) . . . . ?
Li1 O13B C48B C49B -44.2(18) . . . . ?
O14B C50B C51B O15B 58(2) . . . . ?
O15B C52B C45B O16B 53(2) . . . . ?
C50B O14B C49B C48B -163.2(15) . . . . ?
C51B O15B C52B C45B 87(2) . . . . ?
C52B O15B C51B C50B -159.2(19) . . . . ?
C52B C45B O16B Li1 -34.0(15) . . . . ?
C52B C45B O16B C46B -160.8(17) . . . . ?
C45B O16B C46B C47B 86.7(19) . . . . ?
O16B C46B C47B O13B 46(2) . . . . ?
C46B C47B O13B Li1 -29.6(16) . . . . ?
C46B C47B O13B C48B -161.7(17) . . . . ?
C47B O13B C48B C49B 90.1(16) . . . . ?
O13B C48B C49B O14B 52.1(18) . . . . ?
C49B O14B C50B C51B 81(2) . . . . ?

_smtbx_masks_special_details     
;
A THF molecule per asymmetric unit was found to be disordered over a symmetry element and could thus not be modeled.
This is consistend with the compound having beeing crystallized from THF and n-hexane.
A solvent mask was used to account for this THF molecule. This is consistend with the 320 electrons found in a volume of 1164Å³ in 1 void per unit cell which accounts for 0.5 molecules of THF per cell.
;
loop_
_smtbx_masks_void_nr
_smtbx_masks_void_average_x
_smtbx_masks_void_average_y
_smtbx_masks_void_average_z
_smtbx_masks_void_volume
_smtbx_masks_void_count_electrons
_smtbx_masks_void_content
1 0.000 -0.928 0.000 291.0 80.4 '2 THF'
2 0.000 0.160 0.500 291.0 80.4 '2 THF'
3 0.500 -0.683 1.000 291.0 80.4 '2 THF'
4 0.500 -0.377 0.500 291.0 80.4 '2 THF'

_smtbx_masks_void_probe_radius   1.5
_smtbx_masks_void_truncation_radius 1.5
_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 2.787
_oxdiff_exptl_absorpt_empirical_full_min 0.442
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane/THF'
####################################################################### 
# 
# 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_mu297_mp
_database_code_depnum_ccdc_archive 'CCDC 2346028'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Rb([18]crown-6)][1,2,3-P3C2tBu2]'
_chemical_formula_moiety         'C22 H42 O6 P3 Rb'
_chemical_formula_sum            'C22 H42 O6 P3 Rb'
_chemical_formula_weight         580.93
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C22 H42 O6 P3 Rb1 '
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'
O O 0.0492 0.0322 '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'
Rb Rb -0.4688 1.6079 '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                   10.31930(10)
_cell_length_b                   16.00110(10)
_cell_length_c                   17.6998(2)
_cell_angle_alpha                90
_cell_angle_beta                 106.4890(10)
_cell_angle_gamma                90
_cell_volume                     2802.40(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32419
_cell_measurement_temperature    123.05(10)
_cell_measurement_theta_max      66.7080
_cell_measurement_theta_min      4.4670
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.320
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.254
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 orangish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   orangish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.377
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1216
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 2 0.0901
-2 8 -5 0.1625
6 1 -9 0.0818
3 -8 4 0.1372
5 3 -9 0.0687
-6 -3 -3 0.1425
-2 -1 1 0.1011
2 1 1 0.1329
-1 -2 11 0.1993
4 8 2 0.0940
-4 -8 0 0.0923
-4 7 7 0.1187
1 -10 -1 0.1001

_exptl_crystal_size_max          0.405
_exptl_crystal_size_mid          0.235
_exptl_crystal_size_min          0.192
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
-1.9985 1.0076 1.9954 0.1206 -0.1905 0.2370
-1.5698 8.2621 -5.3873 0.5064 -0.7364 -0.4485
5.6369 0.8439 -8.6258 -0.1665 0.2419 -0.9559
2.6079 -8.2261 3.9083 -0.5435 0.7904 0.2826
4.9457 3.3357 -8.9357 -0.0739 -0.0058 -0.9972
-5.5627 -2.5878 -2.7844 0.9415 0.0744 0.3287
-2.0005 -0.9945 0.9964 0.2041 0.0055 0.2381
2.0002 0.9960 1.0031 -0.3392 -0.0327 -0.1200
-1.0099 -1.5366 11.2574 -0.6158 -0.0487 0.7864
3.7120 7.7284 2.3060 -0.7055 -0.6028 -0.3727
-4.3143 -7.6569 -0.1473 0.6384 0.5455 0.5431
-4.3385 6.6341 6.6966 0.0673 -0.8510 0.5208
1.4732 -10.1314 -0.5514 -0.0777 0.9839 0.1610

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0518
_diffrn_reflns_av_unetI/netI     0.0184
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            42970
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        66.781
_diffrn_reflns_theta_max         66.781
_diffrn_reflns_theta_min         4.488
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.05(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     75.00 112.00   1.00    1.72    --   43.43  66.00  78.00   37
  2  ω     47.00  72.00   1.00    1.72    --   43.43  66.00  78.00   25
  3  ω    -27.00  71.00   1.00    1.72    --   43.43 -66.00 -56.00   98
  4  ω     41.00  66.00   1.00    6.86    --   86.50 -66.00 -56.00   25
  5  ω     83.00 108.00   1.00    6.86    --   86.50  66.00  78.00   25
  6  ω   -103.00 -75.00   1.00    6.86    --  -90.00  66.00  78.00   28
  7  ω   -145.00-118.00   1.00    6.86    --  -90.00 -66.00 -56.00   27
  8  ω    -62.00 -35.00   1.00    6.86    --  -90.00  66.00  78.00   27
  9  ω    -41.00  27.00   1.00    1.72    --  -43.43  66.00  78.00   68
 10  ω   -100.00 -73.00   1.00    1.72    --  -43.43 -66.00 -56.00   27
 11  ω      9.00  84.00   1.00    1.72    --   43.43-125.00-180.00   75
 12  ω     85.00 129.00   1.00    6.86    --   86.50  77.00   0.00   44
 13  ω   -106.00 -27.00   1.00    6.86    --  -90.00 125.00 120.00   79
 14  ω   -111.00 -79.00   1.00    6.86    --  -90.00 125.00  60.00   32
 15  ω   -108.00 -74.00   1.00    6.86    --  -90.00 125.00-150.00   34
 16  ω   -172.00-147.00   1.00    6.86    --  -90.00 -94.00  90.00   25
 17  ω   -154.00-110.00   1.00    6.86    --  -90.00 -77.00   0.00   44
 18  ω   -133.00-104.00   1.00    6.86    --  -90.00 -94.00  90.00   29
 19  ω   -142.00 -97.00   1.00    6.86    --  -90.00-125.00 -90.00   45
 20  ω    -96.00 -27.00   1.00    6.86    --  -90.00 125.00 -90.00   69
 21  ω   -111.00 -86.00   1.00    6.86    --  -90.00  45.00  90.00   25
 22  ω    -73.00 -22.00   1.00    6.86    --  -90.00  45.00  90.00   51
 23  ω   -113.00 -46.00   1.00    6.86    --  -90.00  61.00-180.00   67
 24  ω   -144.00-117.00   1.00    6.86    --  -90.00 -77.00-150.00   27
 25  ω   -161.00-101.00   1.00    6.86    --  -90.00-125.00 120.00   60
 26  ω   -111.00 -86.00   1.00    6.86    --  -90.00 125.00 -30.00   25
 27  ω    -72.00 -27.00   1.00    6.86    --  -90.00 125.00 -30.00   45
 28  ω    -61.00 -27.00   1.00    6.86    --  -90.00  30.00 -90.00   34
 29  ω   -120.00 -85.00   1.00    6.86    --  -90.00  77.00  90.00   35
 30  ω    -50.00 -21.00   1.00    6.86    --  -90.00  77.00  90.00   29
 31  ω    -52.00 -27.00   1.00    6.86    --  -90.00 125.00 -60.00   25
 32  ω   -147.00-120.00   1.00    6.86    --  -90.00 -30.00 -60.00   27
 33  ω   -109.00 -63.00   1.00    6.86    --  -90.00 -30.00 -60.00   46
 34  ω   -112.00 -82.00   1.00    6.86    --  -90.00 125.00 -60.00   30
 35  ω    -98.00 -71.00   1.00    6.86    --  -90.00  77.00 -30.00   27
 36  ω    -41.00 -16.00   1.00    6.86    --  -90.00  77.00 -30.00   25
 37  ω    -95.00 -53.00   1.00    6.86    --  -90.00 125.00  90.00   42
 38  ω    -75.00 -27.00   1.00    6.86    --  -90.00 125.00 150.00   48
 39  ω   -109.00 -83.00   1.00    6.86    --  -90.00 125.00   0.00   26
 40  ω    -68.00 -36.00   1.00    6.86    --  -90.00 125.00  60.00   32
 41  ω   -126.00 -96.00   1.00    6.86    --  -90.00  15.00-150.00   30
 42  ω    -71.00 -12.00   1.00    6.86    --  -90.00  15.00-150.00   59
 43  ω    -99.00 -72.00   1.00    6.86    --  -90.00  45.00  60.00   27
 44  ω    -57.00 -28.00   1.00    6.86    --  -90.00  45.00  60.00   29
 45  ω   -105.00 -65.00   1.00    6.86    --  -90.00  77.00 120.00   40
 46  ω   -112.00 -47.00   1.00    6.86    --  -90.00 125.00-180.00   65
 47  ω   -117.00 -73.00   1.00    6.86    --  -90.00  30.00-120.00   44
 48  ω    -61.00 -18.00   1.00    6.86    --  -90.00  30.00-120.00   43
 49  ω   -100.00 -29.00   1.00    6.86    --  -90.00 125.00-120.00   71
 50  ω   -114.00 -61.00   1.00    6.86    --  -90.00  45.00   0.00   53
 51  ω   -160.00 -94.00   1.00    6.86    --  -90.00 -45.00 120.00   66
 52  ω   -119.00 -94.00   1.00    6.86    --  -90.00  77.00 -90.00   25
 53  ω    -69.00 -29.00   1.00    6.86    --  -90.00  77.00 -90.00   40
 54  ω   -157.00-130.00   1.00    6.86    --  -90.00-125.00  60.00   27
 55  ω    -54.00 -27.00   1.00    6.86    --  -90.00 125.00-150.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1317878000
_diffrn_orient_matrix_UB_12      -0.0078170000
_diffrn_orient_matrix_UB_13      -0.0675868000
_diffrn_orient_matrix_UB_21      0.0358275000
_diffrn_orient_matrix_UB_22      -0.0911653000
_diffrn_orient_matrix_UB_23      -0.0135527000
_diffrn_orient_matrix_UB_31      -0.0747072000
_diffrn_orient_matrix_UB_32      -0.0299698000
_diffrn_orient_matrix_UB_33      0.0590665000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4855
_reflns_number_total             4954
_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 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection       
'CrysAlisPro system (CCD 42.90a 64-bit (release 14-04-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.133
_refine_diff_density_min         -0.352
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.028
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         4954
_refine_ls_number_restraints     9
_refine_ls_R_factor_all          0.0450
_refine_ls_R_factor_gt           0.0445
_refine_ls_restrained_S_all      1.027
_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)+(0.0574P)²+7.0094P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1148
_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. Rigid body (RIGU) restrains
 C19, O5, C18
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
3.a Secondary CH2 refined with riding coordinates:
 C19(H19A,H19B), C17(H17A,H17B), C18(H18A,H18B), C13(H13A,H13B), C11(H11A,
 H11B), C22(H22A,H22B), C21(H21A,H21B), C16(H16A,H16B), C15(H15A,H15B),
 C12(H12A,H12B), C14(H14A,H14B), C20(H20A,H20B)
3.b Idealised Me refined as rotating group:
 C7(H7A,H7B,H7C), C8(H8A,H8B,H8C), C9(H9A,H9B,H9C), C6(H6A,H6B,H6C), C5(H5A,
 H5B,H5C), C10(H10A,H10B,H10C)
;
_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
Rb1 Rb 0.61636(3) 0.62902(2) 0.29394(2) 0.02666(12) Uani 1 1 d . . . . .
P1 P 0.38986(8) 0.80373(5) 0.20139(4) 0.02698(19) Uani 1 1 d . . . . .
P3 P 0.33529(8) 0.71717(6) 0.34699(5) 0.0305(2) Uani 1 1 d . . . . .
P2 P 0.27034(8) 0.70822(6) 0.22490(5) 0.0309(2) Uani 1 1 d . . . . .
O5 O 0.8523(3) 0.70913(16) 0.27025(17) 0.0434(6) Uani 1 1 d . . . . .
O2 O 0.4968(3) 0.45777(17) 0.30002(17) 0.0456(6) Uani 1 1 d . . . . .
O1 O 0.4669(3) 0.53956(17) 0.15576(15) 0.0436(6) Uani 1 1 d . . . . .
O4 O 0.8903(3) 0.62126(17) 0.41424(16) 0.0437(6) Uani 1 1 d . . . . .
O6 O 0.6725(3) 0.64417(17) 0.13397(16) 0.0440(6) Uani 1 1 d . . . . .
O3 O 0.6726(3) 0.53011(17) 0.43962(16) 0.0461(6) Uani 1 1 d . . . . .
C2 C 0.4565(3) 0.79989(19) 0.36367(17) 0.0228(6) Uani 1 1 d . . . . .
C1 C 0.4775(3) 0.84078(19) 0.29730(18) 0.0229(6) Uani 1 1 d . . . . .
C4 C 0.5167(3) 0.8160(2) 0.45485(18) 0.0270(6) Uani 1 1 d . . . . .
C3 C 0.5670(3) 0.91878(19) 0.29371(19) 0.0269(6) Uani 1 1 d . . . . .
C7 C 0.5376(4) 0.9919(2) 0.3429(3) 0.0432(9) Uani 1 1 d . . . . .
H7A H 0.445994 1.012859 0.318675 0.065 Uiso 1 1 calc R U . . .
H7B H 0.603010 1.036836 0.344836 0.065 Uiso 1 1 calc R U . . .
H7C H 0.545168 0.972540 0.396507 0.065 Uiso 1 1 calc R U . . .
C19 C 0.8623(4) 0.7274(2) 0.1932(2) 0.0437(9) Uani 1 1 d . . . . .
H19A H 0.922205 0.685984 0.178463 0.052 Uiso 1 1 calc R U . . .
H19B H 0.902681 0.783482 0.192938 0.052 Uiso 1 1 calc R U . . .
C8 C 0.5171(4) 0.7348(3) 0.5033(2) 0.0439(9) Uani 1 1 d . . . . .
H8A H 0.423821 0.717407 0.497796 0.066 Uiso 1 1 calc R U . . .
H8B H 0.563396 0.745388 0.558928 0.066 Uiso 1 1 calc R U . . .
H8C H 0.564370 0.690391 0.483573 0.066 Uiso 1 1 calc R U . . .
C17 C 0.9647(4) 0.6949(3) 0.4064(3) 0.0482(10) Uani 1 1 d . . . . .
H17A H 1.055113 0.693067 0.445285 0.058 Uiso 1 1 calc R U . . .
H17B H 0.916824 0.744903 0.417822 0.058 Uiso 1 1 calc R U . . .
C18 C 0.9801(4) 0.7017(2) 0.3262(3) 0.0481(10) Uani 1 1 d . . . . .
H18A H 1.035868 0.751193 0.323054 0.058 Uiso 1 1 calc R U . . .
H18B H 1.026917 0.651471 0.314411 0.058 Uiso 1 1 calc R U . . .
C9 C 0.6633(4) 0.8459(3) 0.4837(2) 0.0486(10) Uani 1 1 d . . . . .
H9A H 0.722169 0.805571 0.467979 0.073 Uiso 1 1 calc R U . . .
H9B H 0.690085 0.850784 0.541299 0.073 Uiso 1 1 calc R U . . .
H9C H 0.671415 0.900527 0.460468 0.073 Uiso 1 1 calc R U . . .
C13 C 0.4765(5) 0.4536(3) 0.3774(3) 0.0510(10) Uani 1 1 d . . . . .
H13A H 0.425537 0.402299 0.381944 0.061 Uiso 1 1 calc R U . . .
H13B H 0.423037 0.502433 0.385560 0.061 Uiso 1 1 calc R U . . .
C6 C 0.7183(4) 0.8968(2) 0.3173(3) 0.0421(9) Uani 1 1 d . . . . .
H6A H 0.745223 0.874601 0.371123 0.063 Uiso 1 1 calc R U . . .
H6B H 0.770970 0.947164 0.314848 0.063 Uiso 1 1 calc R U . . .
H6C H 0.734991 0.854662 0.281015 0.063 Uiso 1 1 calc R U . . .
C11 C 0.4058(4) 0.4609(3) 0.1623(3) 0.0553(11) Uani 1 1 d . . . . .
H11A H 0.467919 0.415054 0.158266 0.066 Uiso 1 1 calc R U . . .
H11B H 0.321517 0.454601 0.118705 0.066 Uiso 1 1 calc R U . . .
C22 C 0.4906(4) 0.5502(3) 0.0822(2) 0.0479(10) Uani 1 1 d . . . . .
H22A H 0.405350 0.542461 0.039677 0.058 Uiso 1 1 calc R U . . .
H22B H 0.556422 0.507976 0.075250 0.058 Uiso 1 1 calc R U . . .
C21 C 0.5444(4) 0.6352(3) 0.0774(2) 0.0471(10) Uani 1 1 d . . . . .
H21A H 0.553441 0.644837 0.023925 0.056 Uiso 1 1 calc R U . . .
H21B H 0.480854 0.677238 0.087432 0.056 Uiso 1 1 calc R U . . .
C16 C 0.8715(4) 0.6133(3) 0.4891(2) 0.0518(11) Uani 1 1 d . . . . .
H16A H 0.814274 0.659601 0.498327 0.062 Uiso 1 1 calc R U . . .
H16B H 0.959879 0.616259 0.529783 0.062 Uiso 1 1 calc R U . . .
C15 C 0.8060(4) 0.5325(3) 0.4946(2) 0.0479(10) Uani 1 1 d . . . . .
H15A H 0.861363 0.486449 0.482906 0.057 Uiso 1 1 calc R U . . .
H15B H 0.799375 0.524631 0.548886 0.057 Uiso 1 1 calc R U . . .
C5 C 0.5383(5) 0.9550(3) 0.2104(2) 0.0546(11) Uani 1 1 d . . . . .
H5A H 0.566413 0.914845 0.176309 0.082 Uiso 1 1 calc R U . . .
H5B H 0.588773 1.007240 0.212285 0.082 Uiso 1 1 calc R U . . .
H5C H 0.441325 0.966171 0.189251 0.082 Uiso 1 1 calc R U . . .
C12 C 0.3748(4) 0.4559(3) 0.2389(3) 0.0532(11) Uani 1 1 d . . . . .
H12A H 0.316995 0.503534 0.244359 0.064 Uiso 1 1 calc R U . . .
H12B H 0.325416 0.403465 0.241716 0.064 Uiso 1 1 calc R U . . .
C10 C 0.4240(4) 0.8764(2) 0.4825(2) 0.0444(9) Uani 1 1 d . . . . .
H10A H 0.417987 0.929351 0.453903 0.067 Uiso 1 1 calc R U . . .
H10B H 0.461070 0.886603 0.539144 0.067 Uiso 1 1 calc R U . . .
H10C H 0.333635 0.851797 0.472126 0.067 Uiso 1 1 calc R U . . .
C14 C 0.6088(5) 0.4530(3) 0.4381(3) 0.0555(11) Uani 1 1 d . . . . .
H14A H 0.595609 0.441368 0.490372 0.067 Uiso 1 1 calc R U . . .
H14B H 0.666256 0.408170 0.426247 0.067 Uiso 1 1 calc R U . . .
C20 C 0.7273(5) 0.7250(3) 0.1351(3) 0.0489(10) Uani 1 1 d . . . . .
H20A H 0.667171 0.766403 0.149576 0.059 Uiso 1 1 calc R U . . .
H20B H 0.735021 0.739379 0.082173 0.059 Uiso 1 1 calc R U . . .


_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
Rb1 P1 3.7133(9) . ?
Rb1 P3 3.5819(9) . ?
Rb1 P2 3.6568(9) . ?
Rb1 O5 2.886(3) . ?
Rb1 O2 3.019(3) . ?
Rb1 O1 2.875(3) . ?
Rb1 O4 3.021(3) . ?
Rb1 O6 3.057(3) . ?
Rb1 O3 2.940(3) . ?
Rb1 C2 3.588(3) . ?
Rb1 C1 3.686(3) . ?
P1 P2 2.0789(12) . ?
P1 C1 1.783(3) . ?
P3 P2 2.0779(12) . ?
P3 C2 1.787(3) . ?
O5 C19 1.427(5) . ?
O5 C18 1.411(5) . ?
O2 C13 1.446(5) . ?
O2 C12 1.408(5) . ?
O1 C11 1.427(5) . ?
O1 C22 1.402(5) . ?
O4 C17 1.435(5) . ?
O4 C16 1.398(5) . ?
O6 C21 1.421(5) . ?
O6 C20 1.409(5) . ?
O3 C15 1.444(5) . ?
O3 C14 1.396(5) . ?
C2 C1 1.414(4) . ?
C2 C4 1.577(4) . ?
C1 C3 1.565(4) . ?
C4 C8 1.556(5) . ?
C4 C9 1.529(5) . ?
C4 C10 1.534(5) . ?
C3 C7 1.539(5) . ?
C3 C6 1.537(5) . ?
C3 C5 1.534(5) . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.479(6) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C18 1.477(6) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C13 C14 1.478(7) . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.481(7) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.480(6) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C16 C15 1.475(7) . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?

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
P3 Rb1 P1 50.510(19) . . ?
P3 Rb1 P2 33.343(19) . . ?
P3 Rb1 C2 28.86(5) . . ?
P3 Rb1 C1 44.47(5) . . ?
P2 Rb1 P1 32.756(19) . . ?
P2 Rb1 C1 48.67(5) . . ?
O5 Rb1 P1 93.03(6) . . ?
O5 Rb1 P3 129.99(5) . . ?
O5 Rb1 P2 125.57(6) . . ?
O5 Rb1 O2 141.11(7) . . ?
O5 Rb1 O4 57.39(8) . . ?
O5 Rb1 O6 55.98(8) . . ?
O5 Rb1 O3 113.71(8) . . ?
O5 Rb1 C2 101.59(7) . . ?
O5 Rb1 C1 86.67(7) . . ?
O2 Rb1 P1 119.12(6) . . ?
O2 Rb1 P3 88.77(5) . . ?
O2 Rb1 P2 87.50(5) . . ?
O2 Rb1 O4 104.34(8) . . ?
O2 Rb1 O6 106.96(8) . . ?
O2 Rb1 C2 116.54(7) . . ?
O2 Rb1 C1 132.00(7) . . ?
O1 Rb1 P1 83.17(5) . . ?
O1 Rb1 P3 98.07(5) . . ?
O1 Rb1 P2 69.59(5) . . ?
O1 Rb1 O5 111.62(8) . . ?
O1 Rb1 O2 56.82(8) . . ?
O1 Rb1 O4 138.40(7) . . ?
O1 Rb1 O6 56.52(8) . . ?
O1 Rb1 O3 113.75(8) . . ?
O1 Rb1 C2 118.94(7) . . ?
O1 Rb1 C1 110.75(7) . . ?
O4 Rb1 P1 133.47(5) . . ?
O4 Rb1 P3 119.80(5) . . ?
O4 Rb1 P2 151.59(5) . . ?
O4 Rb1 O6 105.70(8) . . ?
O4 Rb1 C2 102.63(7) . . ?
O4 Rb1 C1 108.47(7) . . ?
O6 Rb1 P1 78.04(5) . . ?
O6 Rb1 P3 126.31(5) . . ?
O6 Rb1 P2 94.98(5) . . ?
O6 Rb1 C2 118.99(7) . . ?
O6 Rb1 C1 96.82(7) . . ?
O3 Rb1 P1 137.31(5) . . ?
O3 Rb1 P3 87.41(6) . . ?
O3 Rb1 P2 114.24(6) . . ?
O3 Rb1 O2 57.38(8) . . ?
O3 Rb1 O4 56.46(8) . . ?
O3 Rb1 O6 144.41(7) . . ?
O3 Rb1 C2 95.97(7) . . ?
O3 Rb1 C1 117.49(7) . . ?
C2 Rb1 P1 44.34(5) . . ?
C2 Rb1 P2 49.47(5) . . ?
C2 Rb1 C1 22.37(7) . . ?
C1 Rb1 P1 27.89(5) . . ?
P2 P1 Rb1 72.13(3) . . ?
C1 P1 Rb1 75.20(10) . . ?
C1 P1 P2 102.90(11) . . ?
P2 P3 Rb1 75.31(3) . . ?
C2 P3 Rb1 75.77(10) . . ?
C2 P3 P2 103.11(11) . . ?
P1 P2 Rb1 75.12(3) . . ?
P3 P2 Rb1 71.35(3) . . ?
P3 P2 P1 97.06(5) . . ?
C19 O5 Rb1 121.5(2) . . ?
C18 O5 Rb1 121.3(2) . . ?
C18 O5 C19 112.4(3) . . ?
C13 O2 Rb1 104.3(2) . . ?
C12 O2 Rb1 106.1(2) . . ?
C12 O2 C13 112.9(3) . . ?
C11 O1 Rb1 120.9(2) . . ?
C22 O1 Rb1 122.5(2) . . ?
C22 O1 C11 112.3(3) . . ?
C17 O4 Rb1 108.5(2) . . ?
C16 O4 Rb1 108.5(2) . . ?
C16 O4 C17 112.8(3) . . ?
C21 O6 Rb1 105.1(2) . . ?
C20 O6 Rb1 103.9(2) . . ?
C20 O6 C21 113.1(3) . . ?
C15 O3 Rb1 119.3(2) . . ?
C14 O3 Rb1 119.0(2) . . ?
C14 O3 C15 113.0(3) . . ?
P3 C2 Rb1 75.37(10) . . ?
C1 C2 Rb1 82.69(17) . . ?
C1 C2 P3 118.1(2) . . ?
C1 C2 C4 131.7(3) . . ?
C4 C2 Rb1 112.98(17) . . ?
C4 C2 P3 110.1(2) . . ?
P1 C1 Rb1 76.91(10) . . ?
C2 C1 Rb1 74.94(17) . . ?
C2 C1 P1 118.8(2) . . ?
C2 C1 C3 129.4(3) . . ?
C3 C1 Rb1 119.74(18) . . ?
C3 C1 P1 111.9(2) . . ?
C8 C4 C2 111.4(3) . . ?
C9 C4 C2 117.3(3) . . ?
C9 C4 C8 103.3(3) . . ?
C9 C4 C10 110.1(3) . . ?
C10 C4 C2 109.2(3) . . ?
C10 C4 C8 104.8(3) . . ?
C7 C3 C1 111.7(3) . . ?
C6 C3 C1 111.8(3) . . ?
C6 C3 C7 111.6(3) . . ?
C5 C3 C1 112.7(3) . . ?
C5 C3 C7 104.0(3) . . ?
C5 C3 C6 104.6(3) . . ?
C3 C7 H7A 109.5 . . ?
C3 C7 H7B 109.5 . . ?
C3 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
O5 C19 H19A 109.6 . . ?
O5 C19 H19B 109.6 . . ?
O5 C19 C20 110.5(3) . . ?
H19A C19 H19B 108.1 . . ?
C20 C19 H19A 109.6 . . ?
C20 C19 H19B 109.6 . . ?
C4 C8 H8A 109.5 . . ?
C4 C8 H8B 109.5 . . ?
C4 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
O4 C17 H17A 109.4 . . ?
O4 C17 H17B 109.4 . . ?
O4 C17 C18 111.0(3) . . ?
H17A C17 H17B 108.0 . . ?
C18 C17 H17A 109.4 . . ?
C18 C17 H17B 109.4 . . ?
O5 C18 C17 110.3(3) . . ?
O5 C18 H18A 109.6 . . ?
O5 C18 H18B 109.6 . . ?
C17 C18 H18A 109.6 . . ?
C17 C18 H18B 109.6 . . ?
H18A C18 H18B 108.1 . . ?
C4 C9 H9A 109.5 . . ?
C4 C9 H9B 109.5 . . ?
C4 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
O2 C13 H13A 109.7 . . ?
O2 C13 H13B 109.7 . . ?
O2 C13 C14 109.6(3) . . ?
H13A C13 H13B 108.2 . . ?
C14 C13 H13A 109.7 . . ?
C14 C13 H13B 109.7 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O1 C11 H11A 109.7 . . ?
O1 C11 H11B 109.7 . . ?
O1 C11 C12 109.7(3) . . ?
H11A C11 H11B 108.2 . . ?
C12 C11 H11A 109.7 . . ?
C12 C11 H11B 109.7 . . ?
O1 C22 H22A 109.8 . . ?
O1 C22 H22B 109.8 . . ?
O1 C22 C21 109.4(3) . . ?
H22A C22 H22B 108.3 . . ?
C21 C22 H22A 109.8 . . ?
C21 C22 H22B 109.8 . . ?
O6 C21 C22 110.0(3) . . ?
O6 C21 H21A 109.7 . . ?
O6 C21 H21B 109.7 . . ?
C22 C21 H21A 109.7 . . ?
C22 C21 H21B 109.7 . . ?
H21A C21 H21B 108.2 . . ?
O4 C16 H16A 109.8 . . ?
O4 C16 H16B 109.8 . . ?
O4 C16 C15 109.4(3) . . ?
H16A C16 H16B 108.2 . . ?
C15 C16 H16A 109.8 . . ?
C15 C16 H16B 109.8 . . ?
O3 C15 C16 110.2(3) . . ?
O3 C15 H15A 109.6 . . ?
O3 C15 H15B 109.6 . . ?
C16 C15 H15A 109.6 . . ?
C16 C15 H15B 109.6 . . ?
H15A C15 H15B 108.1 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C12 C11 108.9(3) . . ?
O2 C12 H12A 109.9 . . ?
O2 C12 H12B 109.9 . . ?
C11 C12 H12A 109.9 . . ?
C11 C12 H12B 109.9 . . ?
H12A C12 H12B 108.3 . . ?
C4 C10 H10A 109.5 . . ?
C4 C10 H10B 109.5 . . ?
C4 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O3 C14 C13 109.9(4) . . ?
O3 C14 H14A 109.7 . . ?
O3 C14 H14B 109.7 . . ?
C13 C14 H14A 109.7 . . ?
C13 C14 H14B 109.7 . . ?
H14A C14 H14B 108.2 . . ?
O6 C20 C19 109.2(3) . . ?
O6 C20 H20A 109.8 . . ?
O6 C20 H20B 109.8 . . ?
C19 C20 H20A 109.8 . . ?
C19 C20 H20B 109.8 . . ?
H20A C20 H20B 108.3 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rb1 P1 C1 C2 -64.4(2) . . . . ?
Rb1 P1 C1 C3 117.1(2) . . . . ?
Rb1 P3 C2 C1 73.2(2) . . . . ?
Rb1 P3 C2 C4 -109.5(2) . . . . ?
Rb1 O5 C19 C20 17.7(4) . . . . ?
Rb1 O5 C18 C17 -32.3(4) . . . . ?
Rb1 O2 C13 C14 -67.2(3) . . . . ?
Rb1 O2 C12 C11 66.1(3) . . . . ?
Rb1 O1 C11 C12 26.7(4) . . . . ?
Rb1 O1 C22 C21 -27.5(4) . . . . ?
Rb1 O4 C17 C18 -58.7(3) . . . . ?
Rb1 O4 C16 C15 65.0(3) . . . . ?
Rb1 O6 C21 C22 -64.7(3) . . . . ?
Rb1 O6 C20 C19 68.8(3) . . . . ?
Rb1 O3 C15 C16 28.3(4) . . . . ?
Rb1 O3 C14 C13 -29.2(4) . . . . ?
Rb1 C2 C1 P1 65.48(18) . . . . ?
Rb1 C2 C1 C3 -116.3(3) . . . . ?
Rb1 C2 C4 C8 -52.7(3) . . . . ?
Rb1 C2 C4 C9 66.0(3) . . . . ?
Rb1 C2 C4 C10 -168.0(2) . . . . ?
Rb1 C1 C3 C7 -145.4(2) . . . . ?
Rb1 C1 C3 C6 -19.5(3) . . . . ?
Rb1 C1 C3 C5 98.0(3) . . . . ?
P1 C1 C3 C7 127.5(3) . . . . ?
P1 C1 C3 C6 -106.6(3) . . . . ?
P1 C1 C3 C5 10.9(4) . . . . ?
P3 C2 C1 Rb1 -69.08(18) . . . . ?
P3 C2 C1 P1 -3.6(3) . . . . ?
P3 C2 C1 C3 174.6(2) . . . . ?
P3 C2 C4 C8 29.4(3) . . . . ?
P3 C2 C4 C9 148.1(3) . . . . ?
P3 C2 C4 C10 -85.8(3) . . . . ?
P2 P1 C1 Rb1 67.28(5) . . . . ?
P2 P1 C1 C2 2.9(2) . . . . ?
P2 P1 C1 C3 -175.62(18) . . . . ?
P2 P3 C2 Rb1 -70.87(5) . . . . ?
P2 P3 C2 C1 2.4(2) . . . . ?
P2 P3 C2 C4 179.62(18) . . . . ?
O5 C19 C20 O6 -61.2(4) . . . . ?
O2 C13 C14 O3 68.0(4) . . . . ?
O1 C11 C12 O2 -64.3(4) . . . . ?
O1 C22 C21 O6 64.5(4) . . . . ?
O4 C17 C18 O5 62.3(4) . . . . ?
O4 C16 C15 O3 -63.9(4) . . . . ?
C2 C1 C3 C7 -50.7(4) . . . . ?
C2 C1 C3 C6 75.1(4) . . . . ?
C2 C1 C3 C5 -167.4(3) . . . . ?
C1 C2 C4 C8 -153.8(3) . . . . ?
C1 C2 C4 C9 -35.1(5) . . . . ?
C1 C2 C4 C10 90.9(4) . . . . ?
C4 C2 C1 Rb1 114.4(3) . . . . ?
C4 C2 C1 P1 179.9(2) . . . . ?
C4 C2 C1 C3 -2.0(5) . . . . ?
C19 O5 C18 C17 171.9(3) . . . . ?
C17 O4 C16 C15 -174.7(3) . . . . ?
C18 O5 C19 C20 173.5(3) . . . . ?
C13 O2 C12 C11 179.7(3) . . . . ?
C11 O1 C22 C21 175.8(3) . . . . ?
C22 O1 C11 C12 -176.1(3) . . . . ?
C21 O6 C20 C19 -177.8(3) . . . . ?
C16 O4 C17 C18 -179.0(3) . . . . ?
C15 O3 C14 C13 -176.8(3) . . . . ?
C12 O2 C13 C14 178.1(3) . . . . ?
C14 O3 C15 C16 175.8(3) . . . . ?
C20 O6 C21 C22 -177.4(3) . . . . ?

_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 1.706
_oxdiff_exptl_absorpt_empirical_full_min 0.714
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane/THF'
####################################################################### 
# 
# 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_mu117_mp
_database_code_depnum_ccdc_archive 'CCDC 2346031'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-05
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Cp*Ru(?5-1,2,3-P3C2tBu2)]'
_chemical_formula_moiety         'C20 H33 P3 Ru'
_chemical_formula_sum            'C20 H33 P3 Ru'
_chemical_formula_weight         467.44
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H33 P3 Ru'
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'
Ru Ru 0.0552 3.2960 '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/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.2485(5)
_cell_length_b                   13.0851(5)
_cell_length_c                   16.3300(9)
_cell_angle_alpha                90
_cell_angle_beta                 107.637(5)
_cell_angle_gamma                90
_cell_volume                     2086.96(18)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    13391
_cell_measurement_temperature    123.0(1)
_cell_measurement_theta_max      67.2810
_cell_measurement_theta_min      4.3940
_shelx_estimated_absorpt_T_max   0.438
_shelx_estimated_absorpt_T_min   0.253
_exptl_absorpt_coefficient_mu    8.234
_exptl_absorpt_correction_T_max  0.479
_exptl_absorpt_correction_T_min  0.274
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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   ?
_exptl_crystal_colour            'clear yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   .
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.488
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 6 -1 0.1013
-4 -6 2 0.0886
5 -6 0 0.0614
1 -1 -10 0.0631
-5 6 -1 0.0426
0 0 10 0.1333
0 4 9 0.1291
5 5 -6 0.0786
-5 -5 6 0.1087

_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.12
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
4.2665 6.4119 -0.7911 0.2300 0.9582 -0.1702
-4.4942 -6.2424 1.9074 -0.2325 -0.9705 0.0640
4.7203 -5.7330 -0.2963 -0.9587 0.2298 0.1677
0.8330 -1.3643 -10.3172 0.1597 -0.0358 0.9865
-4.5858 5.5266 -0.9646 0.9715 -0.2326 -0.0462
0.1586 0.1526 10.0427 -0.3543 0.0825 -0.9315
0.1425 4.2881 8.6634 0.0803 0.3420 -0.9363
4.8497 4.6576 -6.4814 0.2134 0.8892 0.4047
-4.8516 -4.6791 6.4421 -0.2139 -0.8910 -0.4004

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0526
_diffrn_reflns_av_unetI/netI     0.0265
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.987
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            17208
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.987
_diffrn_reflns_theta_full        67.067
_diffrn_reflns_theta_max         67.067
_diffrn_reflns_theta_min         4.415
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.0(1)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.987
_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     16.00 113.00   1.00   22.00    --   89.50 -29.00  90.00   97
  2  ω     12.00  86.00   1.00   22.00    --   89.50-103.00 -15.00   74
  3  ω   -166.00-101.00   1.00   22.00    --  -90.00-107.00-108.00   65
  4  ω     32.00  86.00   1.00    6.00    --    0.00-178.00   0.00   54
  5  ω     35.00  88.00   1.00    6.00    --    0.00 178.00 -90.00   53
  6  ω    -18.00  43.00   1.00    6.00    --    0.00-107.00-108.00   61
  7  ω   -120.00 -18.00   1.00   22.00    --  -90.00  77.00  90.00  102
  8  ω   -162.00 -94.00   1.00   22.00    --  -90.00-125.00   0.00   68
  9  ω   -171.00-101.00   1.00   22.00    --  -90.00 -95.00 120.00   70
 10  ω   -113.00 -21.00   1.00   22.00    --  -90.00  45.00  30.00   92
 11  ω   -115.00 -21.00   1.00   22.00    --  -90.00  61.00-120.00   94
 12  ω    -72.00  30.00   1.00    6.00    --    0.00 -77.00  60.00  102
 13  ω    -69.00  24.00   1.00    6.00    --    0.00 -57.00 150.00   93
 14  ω     67.00 158.00   1.00   22.00    --   89.50  45.00-120.00   91
 15  ω     67.00 158.00   1.00   22.00    --   89.50  45.00  30.00   91
 16  ω     64.00 112.00   1.00   22.00    --   89.50  61.00 -60.00   48
 17  ω     67.00 158.00   1.00   22.00    --   89.50  45.00 150.00   91
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, TitanS2, Gemini ultra'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0923752000
_diffrn_orient_matrix_UB_12      0.0929839000
_diffrn_orient_matrix_UB_13      -0.0352303000
_diffrn_orient_matrix_UB_21      0.1279194000
_diffrn_orient_matrix_UB_22      0.0649650000
_diffrn_orient_matrix_UB_23      0.0052108000
_diffrn_orient_matrix_UB_31      -0.0090138000
_diffrn_orient_matrix_UB_32      -0.0319159000
_diffrn_orient_matrix_UB_33      -0.0921262000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance Ultra (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3599
_reflns_number_total             3671
_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 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection       
'CrysAlisPro system (CCD 41.104a 64-bit (release 16-03-2021))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_refine_diff_density_max         0.656
_refine_diff_density_min         -0.426
_refine_diff_density_rms         0.098
_refine_ls_extinction_coef       0.00085(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.055
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3671
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0264
_refine_ls_R_factor_gt           0.0259
_refine_ls_restrained_S_all      1.055
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0474P)²+0.6989P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0685
_refine_ls_wR_factor_ref         0.0690
_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:
 C16(H16A,H16B,H16C), C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C17(H17A,H17B,
 H17C), C10(H10A,H10B,H10C), C14(H14A,H14B,H14C), C19(H19A,H19B,H19C), C12(H12A,
 H12B,H12C), C20(H20A,H20B,H20C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C)
;
_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
Ru1 Ru 0.65919(2) 0.73304(2) 0.36341(2) 0.01108(9) Uani 1 1 d . . . . .
P1 P 0.78374(5) 0.68508(4) 0.50808(3) 0.01846(14) Uani 1 1 d . . . . .
P3 P 0.64528(5) 0.55180(4) 0.34057(4) 0.01883(14) Uani 1 1 d . . . . .
P2 P 0.60607(6) 0.59635(4) 0.45501(4) 0.02188(14) Uani 1 1 d . . . . .
C4 C 0.5184(2) 0.85053(15) 0.37772(14) 0.0156(4) Uani 1 1 d . . . . .
C6 C 0.5294(2) 0.80578(15) 0.24271(13) 0.0161(4) Uani 1 1 d . . . . .
C1 C 0.8713(2) 0.67158(16) 0.42775(13) 0.0139(4) Uani 1 1 d . . . . .
C7 C 0.6403(2) 0.87373(15) 0.28061(13) 0.0153(4) Uani 1 1 d . . . . .
C2 C 0.8088(2) 0.61269(15) 0.35181(13) 0.0146(4) Uani 1 1 d . . . . .
C3 C 0.6340(2) 0.90135(16) 0.36390(13) 0.0152(4) Uani 1 1 d . . . . .
C5 C 0.4538(2) 0.79129(17) 0.30244(14) 0.0163(4) Uani 1 1 d . . . . .
C16 C 0.9648(2) 0.64323(18) 0.24864(15) 0.0258(5) Uani 1 1 d . . . . .
H16A H 0.920015 0.708268 0.227122 0.039 Uiso 1 1 calc R U . . .
H16B H 0.991492 0.608873 0.202857 0.039 Uiso 1 1 calc R U . . .
H16C H 1.046368 0.656149 0.297504 0.039 Uiso 1 1 calc R U . . .
C11 C 0.4685(2) 0.86288(18) 0.45421(15) 0.0236(5) Uani 1 1 d . . . . .
H11A H 0.421448 0.800338 0.462565 0.035 Uiso 1 1 calc R U . . .
H11B H 0.404777 0.920641 0.444836 0.035 Uiso 1 1 calc R U . . .
H11C H 0.546473 0.875743 0.505359 0.035 Uiso 1 1 calc R U . . .
C18 C 1.1270(2) 0.64452(18) 0.46610(15) 0.0243(5) Uani 1 1 d . . . . .
H18A H 1.116600 0.591638 0.506161 0.036 Uiso 1 1 calc R U . . .
H18B H 1.217075 0.676809 0.488728 0.036 Uiso 1 1 calc R U . . .
H18C H 1.119049 0.613413 0.410204 0.036 Uiso 1 1 calc R U . . .
C17 C 0.9325(2) 0.47025(17) 0.30667(16) 0.0256(5) Uani 1 1 d . . . . .
H17A H 1.009803 0.478943 0.358991 0.038 Uiso 1 1 calc R U . . .
H17B H 0.965333 0.441278 0.261172 0.038 Uiso 1 1 calc R U . . .
H17C H 0.865051 0.424016 0.318362 0.038 Uiso 1 1 calc R U . . .
C8 C 0.8653(2) 0.57504(16) 0.27749(14) 0.0177(4) Uani 1 1 d . . . . .
C10 C 0.7221(2) 0.97849(16) 0.42337(15) 0.0233(5) Uani 1 1 d . . . . .
H10A H 0.740513 0.955503 0.482912 0.035 Uiso 1 1 calc R U . . .
H10B H 0.674621 1.044443 0.415869 0.035 Uiso 1 1 calc R U . . .
H10C H 0.808766 0.985968 0.410207 0.035 Uiso 1 1 calc R U . . .
C14 C 0.7318(2) 0.91920(17) 0.23429(15) 0.0216(5) Uani 1 1 d . . . . .
H14A H 0.808614 0.954039 0.275563 0.032 Uiso 1 1 calc R U . . .
H14B H 0.679860 0.968476 0.191581 0.032 Uiso 1 1 calc R U . . .
H14C H 0.766869 0.864900 0.205344 0.032 Uiso 1 1 calc R U . . .
C19 C 1.0248(2) 0.81354(17) 0.39472(16) 0.0234(5) Uani 1 1 d . . . . .
H19A H 0.978590 0.793580 0.335123 0.035 Uiso 1 1 calc R U . . .
H19B H 1.121465 0.827730 0.401700 0.035 Uiso 1 1 calc R U . . .
H19C H 0.981241 0.875006 0.408732 0.035 Uiso 1 1 calc R U . . .
C9 C 1.0140(2) 0.72601(15) 0.45540(16) 0.0177(5) Uani 1 1 d . . . . .
C12 C 0.3239(2) 0.73082(17) 0.28650(18) 0.0245(6) Uani 1 1 d . . . . .
H12A H 0.324292 0.674181 0.247300 0.037 Uiso 1 1 calc R U . . .
H12B H 0.245191 0.775228 0.260717 0.037 Uiso 1 1 calc R U . . .
H12C H 0.317604 0.703591 0.341068 0.037 Uiso 1 1 calc R U . . .
C20 C 1.0467(3) 0.77701(18) 0.54472(16) 0.0273(6) Uani 1 1 d . . . . .
H20A H 0.978329 0.829873 0.543315 0.041 Uiso 1 1 calc R U . . .
H20B H 1.137890 0.808158 0.559724 0.041 Uiso 1 1 calc R U . . .
H20C H 1.044698 0.725349 0.587769 0.041 Uiso 1 1 calc R U . . .
C13 C 0.4888(3) 0.76896(17) 0.15172(16) 0.0241(5) Uani 1 1 d . . . . .
H13A H 0.569155 0.768524 0.131098 0.036 Uiso 1 1 calc R U . . .
H13B H 0.418977 0.814628 0.115640 0.036 Uiso 1 1 calc R U . . .
H13C H 0.451556 0.699595 0.148817 0.036 Uiso 1 1 calc R U . . .
C15 C 0.7475(2) 0.5558(2) 0.19363(15) 0.0303(6) Uani 1 1 d . . . . .
H15A H 0.686298 0.503050 0.203704 0.045 Uiso 1 1 calc R U . . .
H15B H 0.785682 0.533028 0.148482 0.045 Uiso 1 1 calc R U . . .
H15C H 0.695991 0.619273 0.175591 0.045 Uiso 1 1 calc R U . . .


_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
Ru1 P1 2.4035(6) . ?
Ru1 P3 2.3983(6) . ?
Ru1 P2 2.4953(6) . ?
Ru1 C4 2.169(2) . ?
Ru1 C6 2.230(2) . ?
Ru1 C1 2.256(2) . ?
Ru1 C7 2.258(2) . ?
Ru1 C2 2.246(2) . ?
Ru1 C3 2.218(2) . ?
Ru1 C5 2.176(2) . ?
P1 P2 2.1115(8) . ?
P1 C1 1.808(2) . ?
P3 P2 2.1093(8) . ?
P3 C2 1.814(2) . ?
C4 C3 1.435(3) . ?
C4 C5 1.434(3) . ?
C4 C11 1.495(3) . ?
C6 C7 1.428(3) . ?
C6 C5 1.430(3) . ?
C6 C13 1.496(3) . ?
C1 C2 1.435(3) . ?
C1 C9 1.565(3) . ?
C7 C3 1.428(3) . ?
C7 C14 1.495(3) . ?
C2 C8 1.573(3) . ?
C3 C10 1.499(3) . ?
C5 C12 1.502(3) . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C16 C8 1.532(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C18 C9 1.545(3) . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C17 C8 1.544(3) . ?
C8 C15 1.547(3) . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C19 C9 1.540(3) . ?
C9 C20 1.546(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?

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 Ru1 P2 51.02(2) . . ?
P3 Ru1 P1 83.31(2) . . ?
P3 Ru1 P2 51.02(2) . . ?
C4 Ru1 P1 104.58(6) . . ?
C4 Ru1 P3 135.04(6) . . ?
C4 Ru1 P2 99.81(6) . . ?
C4 Ru1 C6 63.54(8) . . ?
C4 Ru1 C1 141.34(8) . . ?
C4 Ru1 C7 63.10(8) . . ?
C4 Ru1 C2 178.52(8) . . ?
C4 Ru1 C3 38.16(8) . . ?
C4 Ru1 C5 38.56(8) . . ?
C6 Ru1 P1 167.75(6) . . ?
C6 Ru1 P3 107.05(6) . . ?
C6 Ru1 P2 130.97(6) . . ?
C6 Ru1 C1 142.79(8) . . ?
C6 Ru1 C7 37.12(8) . . ?
C6 Ru1 C2 117.68(8) . . ?
C1 Ru1 P1 45.53(5) . . ?
C1 Ru1 P3 73.95(5) . . ?
C1 Ru1 P2 79.61(5) . . ?
C1 Ru1 C7 117.72(7) . . ?
C7 Ru1 P1 136.49(5) . . ?
C7 Ru1 P3 136.30(6) . . ?
C7 Ru1 P2 161.61(5) . . ?
C2 Ru1 P1 74.16(5) . . ?
C2 Ru1 P3 45.84(5) . . ?
C2 Ru1 P2 80.01(5) . . ?
C2 Ru1 C1 37.18(8) . . ?
C2 Ru1 C7 117.26(7) . . ?
C3 Ru1 P1 106.47(5) . . ?
C3 Ru1 P3 168.84(6) . . ?
C3 Ru1 P2 131.52(6) . . ?
C3 Ru1 C6 62.63(7) . . ?
C3 Ru1 C1 116.68(8) . . ?
C3 Ru1 C7 37.20(8) . . ?
C3 Ru1 C2 141.25(8) . . ?
C5 Ru1 P1 133.89(6) . . ?
C5 Ru1 P3 105.75(6) . . ?
C5 Ru1 P2 99.72(6) . . ?
C5 Ru1 C6 37.86(8) . . ?
C5 Ru1 C1 179.32(8) . . ?
C5 Ru1 C7 62.93(8) . . ?
C5 Ru1 C2 142.92(8) . . ?
C5 Ru1 C3 63.65(8) . . ?
P2 P1 Ru1 66.74(2) . . ?
C1 P1 Ru1 62.93(7) . . ?
C1 P1 P2 101.78(7) . . ?
P2 P3 Ru1 66.87(2) . . ?
C2 P3 Ru1 62.64(6) . . ?
C2 P3 P2 101.95(7) . . ?
P1 P2 Ru1 62.24(2) . . ?
P3 P2 Ru1 62.11(2) . . ?
P3 P2 P1 98.25(3) . . ?
C3 C4 Ru1 72.77(12) . . ?
C3 C4 C11 126.1(2) . . ?
C5 C4 Ru1 70.98(11) . . ?
C5 C4 C3 107.73(18) . . ?
C5 C4 C11 126.0(2) . . ?
C11 C4 Ru1 125.02(14) . . ?
C7 C6 Ru1 72.50(11) . . ?
C7 C6 C5 108.17(18) . . ?
C7 C6 C13 125.2(2) . . ?
C5 C6 Ru1 69.02(11) . . ?
C5 C6 C13 126.1(2) . . ?
C13 C6 Ru1 130.71(15) . . ?
P1 C1 Ru1 71.54(7) . . ?
C2 C1 Ru1 71.01(11) . . ?
C2 C1 P1 119.33(15) . . ?
C2 C1 C9 128.80(19) . . ?
C9 C1 Ru1 131.01(14) . . ?
C9 C1 P1 111.83(15) . . ?
C6 C7 Ru1 70.39(11) . . ?
C6 C7 C3 108.07(18) . . ?
C6 C7 C14 124.58(19) . . ?
C3 C7 Ru1 69.89(12) . . ?
C3 C7 C14 126.7(2) . . ?
C14 C7 Ru1 132.43(14) . . ?
P3 C2 Ru1 71.52(7) . . ?
C1 C2 Ru1 71.81(11) . . ?
C1 C2 P3 118.66(15) . . ?
C1 C2 C8 131.49(18) . . ?
C8 C2 Ru1 134.80(14) . . ?
C8 C2 P3 109.19(14) . . ?
C4 C3 Ru1 69.07(11) . . ?
C4 C3 C10 125.06(19) . . ?
C7 C3 Ru1 72.92(12) . . ?
C7 C3 C4 108.09(18) . . ?
C7 C3 C10 126.5(2) . . ?
C10 C3 Ru1 128.56(15) . . ?
C4 C5 Ru1 70.46(11) . . ?
C4 C5 C12 126.0(2) . . ?
C6 C5 Ru1 73.13(11) . . ?
C6 C5 C4 107.94(18) . . ?
C6 C5 C12 125.9(2) . . ?
C12 C5 Ru1 125.35(15) . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C8 C16 H16A 109.5 . . ?
C8 C16 H16B 109.5 . . ?
C8 C16 H16C 109.5 . . ?
C4 C11 H11A 109.5 . . ?
C4 C11 H11B 109.5 . . ?
C4 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C9 C18 H18A 109.5 . . ?
C9 C18 H18B 109.5 . . ?
C9 C18 H18C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C8 C17 H17A 109.5 . . ?
C8 C17 H17B 109.5 . . ?
C8 C17 H17C 109.5 . . ?
C16 C8 C2 119.29(18) . . ?
C16 C8 C17 109.62(18) . . ?
C16 C8 C15 103.63(19) . . ?
C17 C8 C2 105.91(17) . . ?
C17 C8 C15 106.52(18) . . ?
C15 C8 C2 111.29(17) . . ?
C3 C10 H10A 109.5 . . ?
C3 C10 H10B 109.5 . . ?
C3 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C7 C14 H14A 109.5 . . ?
C7 C14 H14B 109.5 . . ?
C7 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C9 C19 H19A 109.5 . . ?
C9 C19 H19B 109.5 . . ?
C9 C19 H19C 109.5 . . ?
C18 C9 C1 108.76(16) . . ?
C18 C9 C20 104.50(19) . . ?
C19 C9 C1 113.32(18) . . ?
C19 C9 C18 112.9(2) . . ?
C19 C9 C20 104.40(18) . . ?
C20 C9 C1 112.7(2) . . ?
C5 C12 H12A 109.5 . . ?
C5 C12 H12B 109.5 . . ?
C5 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C9 C20 H20A 109.5 . . ?
C9 C20 H20B 109.5 . . ?
C9 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C6 C13 H13A 109.5 . . ?
C6 C13 H13B 109.5 . . ?
C6 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C8 C15 H15A 109.5 . . ?
C8 C15 H15B 109.5 . . ?
C8 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Ru1 P1 C1 C2 -54.48(14) . . . . ?
Ru1 P1 C1 C9 127.70(15) . . . . ?
Ru1 P3 C2 C1 56.09(14) . . . . ?
Ru1 P3 C2 C8 -132.09(14) . . . . ?
Ru1 C4 C3 C7 62.88(14) . . . . ?
Ru1 C4 C3 C10 -123.1(2) . . . . ?
Ru1 C4 C5 C6 -63.99(14) . . . . ?
Ru1 C4 C5 C12 120.1(2) . . . . ?
Ru1 C6 C7 C3 -59.98(14) . . . . ?
Ru1 C6 C7 C14 128.6(2) . . . . ?
Ru1 C6 C5 C4 62.26(14) . . . . ?
Ru1 C6 C5 C12 -121.8(2) . . . . ?
Ru1 C1 C2 P3 -55.95(12) . . . . ?
Ru1 C1 C2 C8 134.4(2) . . . . ?
Ru1 C1 C9 C18 -159.94(16) . . . . ?
Ru1 C1 C9 C19 -33.6(3) . . . . ?
Ru1 C1 C9 C20 84.7(2) . . . . ?
Ru1 C7 C3 C4 -60.43(14) . . . . ?
Ru1 C7 C3 C10 125.7(2) . . . . ?
Ru1 C2 C8 C16 71.9(3) . . . . ?
Ru1 C2 C8 C17 -164.02(16) . . . . ?
Ru1 C2 C8 C15 -48.7(3) . . . . ?
P1 C1 C2 Ru1 54.73(12) . . . . ?
P1 C1 C2 P3 -1.2(2) . . . . ?
P1 C1 C2 C8 -170.88(16) . . . . ?
P1 C1 C9 C18 116.02(18) . . . . ?
P1 C1 C9 C19 -117.61(18) . . . . ?
P1 C1 C9 C20 0.7(2) . . . . ?
P3 C2 C8 C16 154.59(16) . . . . ?
P3 C2 C8 C17 -81.34(17) . . . . ?
P3 C2 C8 C15 34.0(2) . . . . ?
P2 P1 C1 Ru1 55.97(5) . . . . ?
P2 P1 C1 C2 1.49(17) . . . . ?
P2 P1 C1 C9 -176.34(12) . . . . ?
P2 P3 C2 Ru1 -55.83(5) . . . . ?
P2 P3 C2 C1 0.26(17) . . . . ?
P2 P3 C2 C8 172.08(12) . . . . ?
C6 C7 C3 Ru1 60.30(14) . . . . ?
C6 C7 C3 C4 -0.1(2) . . . . ?
C6 C7 C3 C10 -174.0(2) . . . . ?
C1 C2 C8 C16 -35.0(3) . . . . ?
C1 C2 C8 C17 89.1(3) . . . . ?
C1 C2 C8 C15 -155.6(2) . . . . ?
C7 C6 C5 Ru1 -62.30(14) . . . . ?
C7 C6 C5 C4 0.0(2) . . . . ?
C7 C6 C5 C12 175.9(2) . . . . ?
C2 C1 C9 C18 -61.6(3) . . . . ?
C2 C1 C9 C19 64.8(3) . . . . ?
C2 C1 C9 C20 -176.9(2) . . . . ?
C3 C4 C5 Ru1 63.95(14) . . . . ?
C3 C4 C5 C6 0.0(2) . . . . ?
C3 C4 C5 C12 -176.0(2) . . . . ?
C5 C4 C3 Ru1 -62.78(14) . . . . ?
C5 C4 C3 C7 0.1(2) . . . . ?
C5 C4 C3 C10 174.07(19) . . . . ?
C5 C6 C7 Ru1 60.09(14) . . . . ?
C5 C6 C7 C3 0.1(2) . . . . ?
C5 C6 C7 C14 -171.28(19) . . . . ?
C11 C4 C3 Ru1 121.2(2) . . . . ?
C11 C4 C3 C7 -175.95(19) . . . . ?
C11 C4 C3 C10 -2.0(3) . . . . ?
C11 C4 C5 Ru1 -120.0(2) . . . . ?
C11 C4 C5 C6 176.02(19) . . . . ?
C11 C4 C5 C12 0.1(3) . . . . ?
C14 C7 C3 Ru1 -128.5(2) . . . . ?
C14 C7 C3 C4 171.02(19) . . . . ?
C14 C7 C3 C10 -2.8(3) . . . . ?
C9 C1 C2 Ru1 -127.9(2) . . . . ?
C9 C1 C2 P3 176.19(16) . . . . ?
C9 C1 C2 C8 6.5(4) . . . . ?
C13 C6 C7 Ru1 -127.9(2) . . . . ?
C13 C6 C7 C3 172.10(19) . . . . ?
C13 C6 C7 C14 0.7(3) . . . . ?
C13 C6 C5 Ru1 125.8(2) . . . . ?
C13 C6 C5 C4 -171.94(19) . . . . ?
C13 C6 C5 C12 4.0(3) . . . . ?

_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 1.565
_oxdiff_exptl_absorpt_empirical_full_min 0.754
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
####################################################################### 
# 
# 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_mu113_mc
_database_code_depnum_ccdc_archive 'CCDC 2346030'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-05
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Cp*Fe(?5-1,2,3-P3C2tBu2)]'
_chemical_formula_moiety         'C20 H33 Fe P3'
_chemical_formula_sum            'C20 H33 Fe P3'
_chemical_formula_weight         422.22
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H33 P3 Fe '
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'
Fe Fe -1.1336 3.1974 '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      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/c 1'
_space_group_name_Hall           '-P 2ybc'
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                   10.1779(2)
_cell_length_b                   12.7916(2)
_cell_length_c                   16.4260(2)
_cell_angle_alpha                90
_cell_angle_beta                 107.870(2)
_cell_angle_gamma                90
_cell_volume                     2035.35(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    8850
_cell_measurement_temperature    122.97(16)
_cell_measurement_theta_max      66.6000
_cell_measurement_theta_min      4.4480
_shelx_estimated_absorpt_T_max   0.417
_shelx_estimated_absorpt_T_min   0.279
_exptl_absorpt_coefficient_mu    8.148
_exptl_absorpt_correction_T_max  0.975
_exptl_absorpt_correction_T_min  0.639
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 brownish red'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.378
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             896
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-6 -2 1 0.0666
-3 3 -6 0.0977
2 5 -8 0.0859
6 2 -1 0.0731
-5 3 7 0.0552
-4 -1 10 0.0793
2 3 -10 0.1059
-4 6 -1 0.0954
5 -3 -7 0.0783
4 -6 0 0.0688
-5 2 8 0.0548
-6 -2 5 0.0544
-2 -7 6 0.0971
-4 -4 -4 0.0563
-4 -6 -1 0.0500
3 0 8 0.1021
1 5 7 0.0563
4 -7 -3 0.0639
6 -3 -3 0.0655
-3 6 6 0.0439

_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.13
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
-6.2947 -2.0549 1.3464 0.2834 0.9578 -0.0480
-3.1750 3.2633 -6.3860 0.1290 0.4366 -0.8904
2.2702 5.3500 -8.0586 -0.1171 -0.3953 -0.9111
6.2685 1.5539 -0.5315 -0.2806 -0.9485 0.1470
-5.4806 3.1968 6.8199 0.9221 0.3823 0.0598
-3.7549 -0.7983 10.1530 0.6699 0.2778 0.6885
1.6976 3.2167 -9.8275 -0.3393 -0.1408 -0.9301
-4.0606 5.9109 -1.4435 0.6380 0.2644 -0.7233
5.4591 -3.0524 -7.0348 -0.9202 -0.3815 -0.0881
4.4529 -5.7830 0.3012 -0.7085 -0.2936 0.6417
-5.2766 2.2645 8.0573 0.8982 0.3724 0.2337
-6.3844 -1.5283 4.9746 0.5116 0.8355 0.2007
-2.2424 -6.5567 6.2975 -0.0677 0.5120 0.8563
-3.8941 -4.4347 -4.2178 -0.3265 0.9212 -0.2114
-3.8169 -6.2187 -1.3924 -0.3307 0.9328 0.1431
2.9224 0.2668 7.6489 0.2276 -0.6426 0.7316
1.4513 5.4695 6.5817 0.6730 -0.7088 0.2114
3.9491 -6.5562 -3.3723 -0.9228 -0.0730 0.3784
6.1081 -3.1635 -2.8954 -0.7611 -0.5844 0.2814
-2.9810 6.3472 6.1505 0.9869 -0.1296 -0.0956

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0363
_diffrn_reflns_av_unetI/netI     0.0268
_diffrn_reflns_Laue_measured_fraction_full 0.971
_diffrn_reflns_Laue_measured_fraction_max 0.971
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            12907
_diffrn_reflns_point_group_measured_fraction_full 0.971
_diffrn_reflns_point_group_measured_fraction_max 0.971
_diffrn_reflns_theta_full        66.789
_diffrn_reflns_theta_max         66.789
_diffrn_reflns_theta_min         4.466
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      122.97(16)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.971
_diffrn_measured_fraction_theta_max 0.971
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -45.00 -20.00   1.00    4.00    --  -43.66  47.00-135.00   25
  2  ω     35.00 108.00   1.00    4.00    --   43.66  47.00-135.00   73
  3  ω     19.00  49.00   1.00    4.00    --   43.66 -47.00  75.00   30
  4  ω     85.00 110.00   1.00   14.00    --   86.50  47.00-135.00   25
  5  ω     39.00  64.00   1.00   14.00    --   86.50 -47.00  75.00   25
  6  ω    -80.00 -54.00   1.00   14.00    --  -90.00  47.00-135.00   26
  7  ω   -137.00-112.00   1.00   14.00    --  -90.00 -47.00  75.00   25
  8  ω    -95.00 -21.00   1.00    4.00    --  -43.66 -37.00 -90.00   74
  9  ω    -63.00 -27.00   1.00    4.00    --  -43.66 125.00 -30.00   36
 10  ω    -53.00 -28.00   1.00   14.00    --  -90.00  61.00 150.00   25
 11  ω   -104.00 -75.00   1.00   14.00    --  -90.00  61.00 150.00   29
 12  ω   -163.00 -63.00   1.00   14.00    --  -90.00 -29.00 127.50  100
 13  ω   -142.00-116.00   1.00   14.00    --  -90.00-125.00-150.00   26
 14  ω   -172.00-107.00   1.00   14.00    --  -90.00 -94.00 -60.00   65
 15  ω   -142.00-116.00   1.00   14.00    --  -90.00 -73.00 163.59   26
 16  ω   -163.00-137.00   1.00   14.00    --  -90.00 -77.00 150.00   26
 17  ω   -151.00-126.00   1.00   14.00    --  -90.00 -77.00  90.00   25
 18  ω   -161.00-113.00   1.00   14.00    --  -90.00-125.00-180.00   48
 19  ω   -103.00 -46.00   1.00   14.00    --  -90.00  30.00 120.00   57
 20  ω   -103.00 -77.00   1.00   14.00    --  -90.00 125.00 -60.00   26
 21  ω   -158.00-133.00   1.00   14.00    --  -90.00 -77.00-180.00   25
 22  ω    -87.00 -62.00   1.00   14.00    --  -90.00  27.00  34.94   25
 23  ω   -117.00 -91.00   1.00   14.00    --  -90.00  77.00  60.00   26
 24  ω   -112.00 -37.00   1.00   14.00    --  -90.00 125.00 -30.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0600775000
_diffrn_orient_matrix_UB_12      0.0788593000
_diffrn_orient_matrix_UB_13      0.0499646000
_diffrn_orient_matrix_UB_21      -0.1393607000
_diffrn_orient_matrix_UB_22      -0.0580323000
_diffrn_orient_matrix_UB_23      -0.0287374000
_diffrn_orient_matrix_UB_31      0.0476189000
_diffrn_orient_matrix_UB_32      -0.0701360000
_diffrn_orient_matrix_UB_33      0.0799072000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3371
_reflns_number_total             3510
_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 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection       
'CrysAlisPro system (CCD 41.109a 64-bit (release 07-05-2021))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.403
_refine_diff_density_min         -0.303
_refine_diff_density_rms         0.062
_refine_ls_extinction_coef       0.00062(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     229
_refine_ls_number_reflns         3510
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0298
_refine_ls_R_factor_gt           0.0280
_refine_ls_restrained_S_all      1.073
_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)+(0.0459P)²+0.8853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0772
_refine_ls_wR_factor_ref         0.0783
_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:
 C11(H11A,H11B,H11C), C18(H18A,H18B,H18C), C13(H13A,H13B,H13C), C12(H12A,H12B,
 H12C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C14(H14A,
 H14B,H14C), C17(H17A,H17B,H17C), 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
Fe1 Fe 0.65772(3) 0.26817(2) 0.36278(2) 0.00985(11) Uani 1 1 d . . . . .
P1 P 0.77284(5) 0.31135(4) 0.50286(3) 0.01642(13) Uani 1 1 d . . . . .
P3 P 0.63527(5) 0.44422(4) 0.33419(3) 0.01688(14) Uani 1 1 d . . . . .
P2 P 0.59450(5) 0.40145(4) 0.44786(3) 0.01954(14) Uani 1 1 d . . . . .
C7 C 0.64566(19) 0.13325(14) 0.28447(11) 0.0140(4) Uani 1 1 d . . . . .
C3 C 0.5324(2) 0.20171(15) 0.24720(12) 0.0143(4) Uani 1 1 d . . . . .
C1 C 0.86354(19) 0.32481(14) 0.42505(11) 0.0128(4) Uani 1 1 d . . . . .
C2 C 0.80177(19) 0.38393(14) 0.34842(11) 0.0133(4) Uani 1 1 d . . . . .
C5 C 0.5244(2) 0.15526(14) 0.38140(12) 0.0147(4) Uani 1 1 d . . . . .
C4 C 0.4575(2) 0.21534(15) 0.30686(12) 0.0148(4) Uani 1 1 d . . . . .
C6 C 0.64091(19) 0.10465(15) 0.36733(11) 0.0140(4) Uani 1 1 d . . . . .
C8 C 1.0101(2) 0.27298(15) 0.45595(12) 0.0166(4) Uani 1 1 d . . . . .
C11 C 1.0305(2) 0.18478(16) 0.39746(13) 0.0211(4) Uani 1 1 d . . . . .
H11A H 0.990386 0.119935 0.411060 0.032 Uiso 1 1 calc R U . . .
H11B H 1.129349 0.174571 0.406404 0.032 Uiso 1 1 calc R U . . .
H11C H 0.984705 0.203572 0.337601 0.032 Uiso 1 1 calc R U . . .
C18 C 0.4753(2) 0.14165(16) 0.45780(12) 0.0211(4) Uani 1 1 d . . . . .
H18A H 0.554400 0.127620 0.508388 0.032 Uiso 1 1 calc R U . . .
H18B H 0.410624 0.082833 0.448090 0.032 Uiso 1 1 calc R U . . .
H18C H 0.428692 0.205606 0.466938 0.032 Uiso 1 1 calc R U . . .
C13 C 0.9679(2) 0.35714(17) 0.25128(13) 0.0225(4) Uani 1 1 d . . . . .
H13A H 1.048166 0.345118 0.301638 0.034 Uiso 1 1 calc R U . . .
H13B H 0.997231 0.393544 0.207292 0.034 Uiso 1 1 calc R U . . .
H13C H 0.926185 0.289908 0.228758 0.034 Uiso 1 1 calc R U . . .
C9 C 0.8617(2) 0.42419(15) 0.27657(12) 0.0168(4) Uani 1 1 d . . . . .
C12 C 1.1200(2) 0.36003(16) 0.46888(13) 0.0207(4) Uani 1 1 d . . . . .
H12A H 1.113618 0.391941 0.413564 0.031 Uiso 1 1 calc R U . . .
H12B H 1.212156 0.329879 0.493776 0.031 Uiso 1 1 calc R U . . .
H12C H 1.103860 0.413445 0.507513 0.031 Uiso 1 1 calc R U . . .
C19 C 0.7310(2) 0.02666(15) 0.42675(13) 0.0207(4) Uani 1 1 d . . . . .
H19A H 0.815850 0.016428 0.411418 0.031 Uiso 1 1 calc R U . . .
H19B H 0.681777 -0.040014 0.422102 0.031 Uiso 1 1 calc R U . . .
H19C H 0.754268 0.052483 0.485644 0.031 Uiso 1 1 calc R U . . .
C20 C 0.7374(2) 0.08846(16) 0.23740(13) 0.0204(4) Uani 1 1 d . . . . .
H20A H 0.769744 0.144673 0.207800 0.031 Uiso 1 1 calc R U . . .
H20B H 0.685585 0.037119 0.195482 0.031 Uiso 1 1 calc R U . . .
H20C H 0.816808 0.054255 0.278098 0.031 Uiso 1 1 calc R U . . .
C10 C 1.0409(2) 0.22161(17) 0.54499(13) 0.0238(5) Uani 1 1 d . . . . .
H10A H 1.034115 0.274330 0.586810 0.036 Uiso 1 1 calc R U . . .
H10B H 1.134241 0.192114 0.562187 0.036 Uiso 1 1 calc R U . . .
H10C H 0.973769 0.165793 0.542450 0.036 Uiso 1 1 calc R U . . .
C14 C 0.9251(2) 0.53224(16) 0.30698(13) 0.0222(4) Uani 1 1 d . . . . .
H14A H 0.854101 0.578098 0.316588 0.033 Uiso 1 1 calc R U . . .
H14B H 0.960504 0.562976 0.263226 0.033 Uiso 1 1 calc R U . . .
H14C H 1.000791 0.524327 0.360450 0.033 Uiso 1 1 calc R U . . .
C17 C 0.3263(2) 0.27594(17) 0.29112(15) 0.0232(5) Uani 1 1 d . . . . .
H17A H 0.320432 0.304121 0.345379 0.035 Uiso 1 1 calc R U . . .
H17B H 0.247352 0.229776 0.266042 0.035 Uiso 1 1 calc R U . . .
H17C H 0.325083 0.333608 0.251621 0.035 Uiso 1 1 calc R U . . .
C15 C 0.7467(2) 0.44213(19) 0.19104(13) 0.0276(5) Uani 1 1 d . . . . .
H15A H 0.699703 0.375825 0.170932 0.041 Uiso 1 1 calc R U . . .
H15B H 0.787512 0.469052 0.148388 0.041 Uiso 1 1 calc R U . . .
H15C H 0.680015 0.492877 0.199565 0.041 Uiso 1 1 calc R U . . .
C16 C 0.4874(2) 0.23936(17) 0.15679(13) 0.0231(5) Uani 1 1 d . . . . .
H16A H 0.456694 0.312165 0.155034 0.035 Uiso 1 1 calc R U . . .
H16B H 0.411144 0.195838 0.122620 0.035 Uiso 1 1 calc R U . . .
H16C H 0.564975 0.234795 0.133381 0.035 Uiso 1 1 calc R U . . .


_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 2.3061(5) . ?
Fe1 P3 2.2973(5) . ?
Fe1 P2 2.4136(5) . ?
Fe1 C7 2.1334(18) . ?
Fe1 C3 2.1139(19) . ?
Fe1 C1 2.1551(19) . ?
Fe1 C2 2.1470(18) . ?
Fe1 C5 2.0676(19) . ?
Fe1 C4 2.0749(19) . ?
Fe1 C6 2.1019(19) . ?
P1 P2 2.1054(7) . ?
P1 C1 1.7999(19) . ?
P3 P2 2.1056(7) . ?
P3 C2 1.8104(19) . ?
C7 C3 1.428(3) . ?
C7 C6 1.425(3) . ?
C7 C20 1.497(3) . ?
C3 C4 1.425(3) . ?
C3 C16 1.493(3) . ?
C1 C2 1.437(3) . ?
C1 C8 1.568(3) . ?
C2 C9 1.573(3) . ?
C5 C4 1.429(3) . ?
C5 C6 1.430(3) . ?
C5 C18 1.497(3) . ?
C4 C17 1.496(3) . ?
C6 C19 1.496(3) . ?
C8 C11 1.537(3) . ?
C8 C12 1.546(3) . ?
C8 C10 1.545(3) . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C13 C9 1.533(3) . ?
C9 C14 1.542(3) . ?
C9 C15 1.545(3) . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C17 H17A 0.9800 . ?
C17 H17B 0.9800 . ?
C17 H17C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?

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 52.927(19) . . ?
P3 Fe1 P1 87.56(2) . . ?
P3 Fe1 P2 53.026(19) . . ?
C7 Fe1 P1 135.48(5) . . ?
C7 Fe1 P3 133.31(5) . . ?
C7 Fe1 P2 160.78(5) . . ?
C7 Fe1 C1 115.21(7) . . ?
C7 Fe1 C2 113.99(7) . . ?
C3 Fe1 P1 166.98(5) . . ?
C3 Fe1 P3 102.47(5) . . ?
C3 Fe1 P2 127.55(6) . . ?
C3 Fe1 C7 39.28(7) . . ?
C3 Fe1 C1 142.41(7) . . ?
C3 Fe1 C2 115.03(7) . . ?
C1 Fe1 P1 47.44(5) . . ?
C1 Fe1 P3 77.80(5) . . ?
C1 Fe1 P2 83.15(5) . . ?
C2 Fe1 P1 77.84(5) . . ?
C2 Fe1 P3 47.93(5) . . ?
C2 Fe1 P2 83.62(5) . . ?
C2 Fe1 C1 39.04(7) . . ?
C5 Fe1 P1 100.09(5) . . ?
C5 Fe1 P3 133.34(6) . . ?
C5 Fe1 P2 95.98(5) . . ?
C5 Fe1 C7 66.74(7) . . ?
C5 Fe1 C3 67.00(7) . . ?
C5 Fe1 C1 138.68(7) . . ?
C5 Fe1 C2 177.70(7) . . ?
C5 Fe1 C4 40.36(7) . . ?
C5 Fe1 C6 40.11(8) . . ?
C4 Fe1 P1 130.47(6) . . ?
C4 Fe1 P3 101.90(6) . . ?
C4 Fe1 P2 94.95(5) . . ?
C4 Fe1 C7 66.58(7) . . ?
C4 Fe1 C3 39.75(7) . . ?
C4 Fe1 C1 177.83(7) . . ?
C4 Fe1 C2 141.91(7) . . ?
C4 Fe1 C6 67.17(7) . . ?
C6 Fe1 P1 102.99(5) . . ?
C6 Fe1 P3 168.14(5) . . ?
C6 Fe1 P2 130.03(5) . . ?
C6 Fe1 C7 39.30(7) . . ?
C6 Fe1 C3 66.32(7) . . ?
C6 Fe1 C1 113.30(7) . . ?
C6 Fe1 C2 139.12(7) . . ?
P2 P1 Fe1 66.16(2) . . ?
C1 P1 Fe1 61.88(6) . . ?
C1 P1 P2 101.85(6) . . ?
P2 P3 Fe1 66.32(2) . . ?
C2 P3 Fe1 61.68(6) . . ?
C2 P3 P2 101.90(6) . . ?
P1 P2 Fe1 60.915(19) . . ?
P1 P2 P3 98.29(3) . . ?
P3 P2 Fe1 60.654(19) . . ?
C3 C7 Fe1 69.62(10) . . ?
C3 C7 C20 124.27(17) . . ?
C6 C7 Fe1 69.16(10) . . ?
C6 C7 C3 107.90(16) . . ?
C6 C7 C20 127.20(18) . . ?
C20 C7 Fe1 133.75(14) . . ?
C7 C3 Fe1 71.10(10) . . ?
C7 C3 C16 125.79(18) . . ?
C4 C3 Fe1 68.65(10) . . ?
C4 C3 C7 108.20(16) . . ?
C4 C3 C16 125.41(18) . . ?
C16 C3 Fe1 132.82(14) . . ?
P1 C1 Fe1 70.69(7) . . ?
C2 C1 Fe1 70.18(10) . . ?
C2 C1 P1 119.36(14) . . ?
C2 C1 C8 128.54(16) . . ?
C8 C1 Fe1 134.53(13) . . ?
C8 C1 P1 111.97(13) . . ?
P3 C2 Fe1 70.39(6) . . ?
C1 C2 Fe1 70.79(10) . . ?
C1 C2 P3 118.54(14) . . ?
C1 C2 C9 131.56(17) . . ?
C9 C2 Fe1 138.04(13) . . ?
C9 C2 P3 109.09(13) . . ?
C4 C5 Fe1 70.10(11) . . ?
C4 C5 C6 107.81(16) . . ?
C4 C5 C18 125.93(18) . . ?
C6 C5 Fe1 71.23(11) . . ?
C6 C5 C18 126.12(17) . . ?
C18 C5 Fe1 127.47(13) . . ?
C3 C4 Fe1 71.60(11) . . ?
C3 C4 C5 107.97(17) . . ?
C3 C4 C17 125.59(18) . . ?
C5 C4 Fe1 69.55(11) . . ?
C5 C4 C17 126.32(18) . . ?
C17 C4 Fe1 127.66(14) . . ?
C7 C6 Fe1 71.54(10) . . ?
C7 C6 C5 108.12(16) . . ?
C7 C6 C19 126.93(18) . . ?
C5 C6 Fe1 68.65(10) . . ?
C5 C6 C19 124.65(17) . . ?
C19 C6 Fe1 130.27(13) . . ?
C11 C8 C1 113.93(16) . . ?
C11 C8 C12 112.59(17) . . ?
C11 C8 C10 104.63(16) . . ?
C12 C8 C1 108.44(15) . . ?
C10 C8 C1 112.49(17) . . ?
C10 C8 C12 104.38(16) . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C5 C18 H18A 109.5 . . ?
C5 C18 H18B 109.5 . . ?
C5 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C9 C13 H13A 109.5 . . ?
C9 C13 H13B 109.5 . . ?
C9 C13 H13C 109.5 . . ?
C13 C9 C2 119.23(16) . . ?
C13 C9 C14 109.26(16) . . ?
C13 C9 C15 103.71(16) . . ?
C14 C9 C2 105.68(15) . . ?
C14 C9 C15 106.63(17) . . ?
C15 C9 C2 111.77(16) . . ?
C8 C12 H12A 109.5 . . ?
C8 C12 H12B 109.5 . . ?
C8 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?
C6 C19 H19A 109.5 . . ?
C6 C19 H19B 109.5 . . ?
C6 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C7 C20 H20A 109.5 . . ?
C7 C20 H20B 109.5 . . ?
C7 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C9 C14 H14A 109.5 . . ?
C9 C14 H14B 109.5 . . ?
C9 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C17 H17A 109.5 . . ?
C4 C17 H17B 109.5 . . ?
C4 C17 H17C 109.5 . . ?
H17A C17 H17B 109.5 . . ?
H17A C17 H17C 109.5 . . ?
H17B C17 H17C 109.5 . . ?
C9 C15 H15A 109.5 . . ?
C9 C15 H15B 109.5 . . ?
C9 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C3 C16 H16A 109.5 . . ?
C3 C16 H16B 109.5 . . ?
C3 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Fe1 P1 C1 C2 52.45(13) . . . . ?
Fe1 P1 C1 C8 -131.29(14) . . . . ?
Fe1 P3 C2 C1 -53.74(13) . . . . ?
Fe1 P3 C2 C9 135.40(13) . . . . ?
Fe1 C7 C3 C4 -58.82(13) . . . . ?
Fe1 C7 C3 C16 129.7(2) . . . . ?
Fe1 C7 C6 C5 59.14(13) . . . . ?
Fe1 C7 C6 C19 -126.99(19) . . . . ?
Fe1 C3 C4 C5 -60.33(13) . . . . ?
Fe1 C3 C4 C17 123.6(2) . . . . ?
Fe1 C1 C2 P3 53.54(11) . . . . ?
Fe1 C1 C2 C9 -138.0(2) . . . . ?
Fe1 C1 C8 C11 35.6(3) . . . . ?
Fe1 C1 C8 C12 161.78(14) . . . . ?
Fe1 C1 C8 C10 -83.3(2) . . . . ?
Fe1 C2 C9 C13 -74.4(3) . . . . ?
Fe1 C2 C9 C14 162.30(16) . . . . ?
Fe1 C2 C9 C15 46.7(3) . . . . ?
Fe1 C5 C4 C3 61.63(13) . . . . ?
Fe1 C5 C4 C17 -122.36(19) . . . . ?
Fe1 C5 C6 C7 -60.95(13) . . . . ?
Fe1 C5 C6 C19 125.00(18) . . . . ?
P1 C1 C2 Fe1 -52.68(11) . . . . ?
P1 C1 C2 P3 0.9(2) . . . . ?
P1 C1 C2 C9 169.29(15) . . . . ?
P1 C1 C8 C11 119.62(16) . . . . ?
P1 C1 C8 C12 -114.16(15) . . . . ?
P1 C1 C8 C10 0.8(2) . . . . ?
P3 C2 C9 C13 -155.94(15) . . . . ?
P3 C2 C9 C14 80.71(16) . . . . ?
P3 C2 C9 C15 -34.9(2) . . . . ?
P2 P1 C1 Fe1 -54.51(4) . . . . ?
P2 P1 C1 C2 -2.06(15) . . . . ?
P2 P1 C1 C8 174.20(11) . . . . ?
P2 P3 C2 Fe1 54.56(4) . . . . ?
P2 P3 C2 C1 0.83(15) . . . . ?
P2 P3 C2 C9 -170.03(11) . . . . ?
C7 C3 C4 Fe1 60.35(13) . . . . ?
C7 C3 C4 C5 0.0(2) . . . . ?
C7 C3 C4 C17 -176.02(18) . . . . ?
C3 C7 C6 Fe1 -59.03(13) . . . . ?
C3 C7 C6 C5 0.1(2) . . . . ?
C3 C7 C6 C19 173.98(18) . . . . ?
C1 C2 C9 C13 34.8(3) . . . . ?
C1 C2 C9 C14 -88.5(2) . . . . ?
C1 C2 C9 C15 155.9(2) . . . . ?
C2 C1 C8 C11 -64.5(3) . . . . ?
C2 C1 C8 C12 61.7(2) . . . . ?
C2 C1 C8 C10 176.59(18) . . . . ?
C4 C5 C6 Fe1 60.87(13) . . . . ?
C4 C5 C6 C7 -0.1(2) . . . . ?
C4 C5 C6 C19 -174.13(17) . . . . ?
C6 C7 C3 Fe1 58.74(13) . . . . ?
C6 C7 C3 C4 -0.1(2) . . . . ?
C6 C7 C3 C16 -171.56(18) . . . . ?
C6 C5 C4 Fe1 -61.59(13) . . . . ?
C6 C5 C4 C3 0.0(2) . . . . ?
C6 C5 C4 C17 176.05(18) . . . . ?
C8 C1 C2 Fe1 131.75(19) . . . . ?
C8 C1 C2 P3 -174.70(14) . . . . ?
C8 C1 C2 C9 -6.3(3) . . . . ?
C18 C5 C4 Fe1 122.46(19) . . . . ?
C18 C5 C4 C3 -175.91(18) . . . . ?
C18 C5 C4 C17 0.1(3) . . . . ?
C18 C5 C6 Fe1 -123.20(19) . . . . ?
C18 C5 C6 C7 175.85(17) . . . . ?
C18 C5 C6 C19 1.8(3) . . . . ?
C20 C7 C3 Fe1 -129.76(18) . . . . ?
C20 C7 C3 C4 171.42(18) . . . . ?
C20 C7 C3 C16 -0.1(3) . . . . ?
C20 C7 C6 Fe1 129.79(19) . . . . ?
C20 C7 C6 C5 -171.07(18) . . . . ?
C20 C7 C6 C19 2.8(3) . . . . ?
C16 C3 C4 Fe1 -128.13(19) . . . . ?
C16 C3 C4 C5 171.54(18) . . . . ?
C16 C3 C4 C17 -4.5(3) . . . . ?

_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 2.354
_oxdiff_exptl_absorpt_empirical_full_min 0.640
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane'
####################################################################### 
# 
# 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_mu297_diphos
_database_code_depnum_ccdc_archive 'CCDC 2346029'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[Rb([18]crown-6)][1,3-P2C3tBu3]'
_chemical_formula_moiety         'C27 H51 O6 P2 Rb'
_chemical_formula_sum            'C27 H51 O6 P2 Rb'
_chemical_formula_weight         619.08
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C27 H51 O6 P2 Rb1 '
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'
O O 0.0492 0.0322 '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'
Rb Rb -0.4688 1.6079 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   9.3862(2)
_cell_length_b                   10.5727(2)
_cell_length_c                   16.3426(4)
_cell_angle_alpha                90.511(2)
_cell_angle_beta                 98.341(2)
_cell_angle_gamma                101.542(2)
_cell_volume                     1570.99(6)
_cell_formula_units_Z            2
_cell_measurement_reflns_used    34160
_cell_measurement_temperature    123.02(10)
_cell_measurement_theta_max      66.8190
_cell_measurement_theta_min      4.7860
_shelx_estimated_absorpt_T_max   0.594
_shelx_estimated_absorpt_T_min   0.459
_exptl_absorpt_coefficient_mu    3.418
_exptl_absorpt_correction_T_max  0.988
_exptl_absorpt_correction_T_min  0.542
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 bluish white'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   bluish
_exptl_crystal_colour_primary    white
_exptl_crystal_density_diffrn    1.309
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             656
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 1 -9 0.1327
4 -5 -6 0.0966
4 -4 4 0.1166
-1 2 10 0.0975
-5 5 -2 0.1227
-4 5 7 0.1225
6 -2 -1 0.0628
3 -2 -9 0.1171
-6 1 -1 0.0747
1 6 -2 0.1027
1 4 7 0.1045
-1 -4 8 0.1141
-1 -6 -3 0.1135
1 1 -10 0.1307

_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
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
-2.1443 1.3375 -9.2367 0.3979 -0.2437 -0.8845
3.9316 -4.8174 -5.9097 -0.6837 0.4187 -0.5977
4.3694 -4.2203 4.3816 -0.7818 0.4788 0.3995
-0.5433 1.6392 10.2193 0.0756 -0.0463 0.9961
-4.6872 4.7620 -2.4323 0.8341 -0.5108 -0.2082
-3.5675 4.5285 6.8814 0.6173 -0.3780 0.6899
6.0899 -1.5763 -1.4912 -0.9967 -0.0787 -0.0211
3.4074 -1.8421 -9.3265 -0.5419 -0.0428 -0.8394
-5.8432 1.1834 -1.4796 0.9617 0.0760 -0.2634
1.4434 6.1426 -2.1907 -0.1302 -0.9911 0.0276
0.6808 4.2951 7.3330 -0.0701 -0.5341 0.8425
-1.2350 -4.2173 8.0905 0.1050 0.7985 0.5927
-1.1680 -5.8214 -3.3187 0.1106 0.8425 -0.5271
0.6475 1.1707 -10.4683 -0.0486 -0.3691 -0.9281

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0608
_diffrn_reflns_av_unetI/netI     0.0226
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            42737
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        66.690
_diffrn_reflns_theta_max         66.690
_diffrn_reflns_theta_min         4.271
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.02(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -89.00   1.00    2.00    --  -43.68 -13.00-166.00   27
  2  ω     81.00 115.00   1.00    2.00    --   43.68  13.00   5.00   34
  3  ω    -35.00  85.00   1.00    2.00    --   43.68 -13.00-166.00  120
  4  ω     24.00  59.00   1.00    2.00    --   43.68  13.00   5.00   35
  5  ω     77.00 102.00   1.00    7.00    --   86.50  13.00   5.00   25
  6  ω     44.00  69.00   1.00    7.00    --   86.50 -13.00-166.00   25
  7  ω   -166.00-134.00   1.00    7.00    --  -90.00 -13.00-166.00   32
  8  ω   -108.00 -63.00   1.00    7.00    --  -90.00 -13.00-166.00   45
  9  ω     -6.00  21.00   1.00    2.00    --   26.00  81.00 148.59   27
 10  ω      5.00  32.00   1.00    2.00    --  -43.68  13.00   5.00   27
 11  ω    -40.00  -3.00   1.00    2.00    --  -43.68 -13.00-166.00   37
 12  ω    -49.00 -24.00   1.00    2.00    --  -43.68  13.00   5.00   25
 13  ω    -94.00 -37.00   1.00    2.00    --  -43.68 125.00  60.00   57
 14  ω     19.00  56.00   1.00    2.00    --   43.68  37.00  60.00   37
 15  ω      7.00  85.00   1.00    2.00    --   43.68-125.00-180.00   78
 16  ω     21.00  55.00   1.00    2.00    --   50.00  69.00 -12.05   34
 17  ω     67.00 110.00   1.00    2.00    --   50.00  71.00-165.57   43
 18  ω     21.00  69.00   1.00    2.00    --   50.00  69.00 -73.37   48
 19  ω     20.00  62.00   1.00    2.00    --   50.00  71.00-165.57   42
 20  ω     60.00  91.00   1.00    2.00    --   50.00  69.00 -12.05   31
 21  ω     64.00  91.00   1.00    2.00    --   54.00  71.00  49.48   27
 22  ω     26.00  55.00   1.00    2.00    --   54.00  71.00  49.48   29
 23  ω     28.00  55.00   1.00    2.00    --   58.00  71.00  98.96   27
 24  ω     34.00  78.00   1.00    2.00    --   62.00  71.00 143.70   44
 25  ω     34.00  67.00   1.00    2.00    --   62.00  71.00 120.33   33
 26  ω     34.00  63.00   1.00    2.00    --   62.00  69.00  65.89   29
 27  ω     98.00 126.00   1.00    2.00    --   62.00  71.00 143.70   28
 28  ω     33.00 103.00   1.00    2.00    --   62.00  70.00-148.13   70
 29  ω     32.00  81.00   1.00    2.00    --   62.00  71.00   1.87   49
 30  ω     38.00  64.00   1.00    2.00    --   66.00  70.00-108.56   26
 31  ω     37.00  64.00   1.00    2.00    --   66.00  70.00 177.48   27
 32  ω     37.00  64.00   1.00    2.00    --   66.00  71.00 -57.21   27
 33  ω     41.00  67.00   1.00    7.00    --   70.00  70.00 -81.28   26
 34  ω     44.00  70.00   1.00    7.00    --   74.00  71.00  21.96   26
 35  ω   -159.00 -63.00   1.00    7.00    --  -90.00 -61.00 130.71   96
 36  ω   -142.00 -61.00   1.00    7.00    --  -90.00 -70.00 -79.56   81
 37  ω   -159.00-131.00   1.00    7.00    --  -90.00 -65.00-119.48   28
 38  ω    -97.00 -63.00   1.00    7.00    --  -90.00 -64.00 -77.22   34
 39  ω   -111.00 -44.00   1.00    7.00    --  -90.00 125.00-150.00   67
 40  ω   -161.00-102.00   1.00    7.00    --  -90.00-125.00  60.00   59
 41  ω    -88.00 -61.00   1.00    7.00    --  -90.00 -67.00 -24.86   27
 42  ω   -159.00-108.00   1.00    7.00    --  -90.00 -67.00 -24.86   51
 43  ω    -89.00 -62.00   1.00    7.00    --  -90.00 -66.00   0.12   27
 44  ω   -133.00 -64.00   1.00    7.00    --  -90.00 -68.00-125.66   69
 45  ω    -85.00 -60.00   1.00    7.00    --  -90.00 -71.00 171.03   25
 46  ω   -153.00 -96.00   1.00    7.00    --  -90.00 -66.00   0.12   57
 47  ω    -75.00 -17.00   1.00    7.00    --  -90.00  77.00  30.00   58
 48  ω    -52.00 -27.00   1.00    7.00    --  -90.00  13.00   5.00   25
 49  ω   -149.00-115.00   1.00    7.00    --  -90.00 -71.00 171.03   34
 50  ω   -161.00-131.00   1.00    7.00    --  -90.00-125.00 -60.00   30
 51  ω   -102.00 -62.00   1.00    7.00    --  -90.00 -64.00 145.97   40
 52  ω   -157.00-122.00   1.00    7.00    --  -90.00 -64.00 145.97   35
 53  ω   -112.00 -38.00   1.00    7.00    --  -90.00 125.00 -60.00   74
 54  ω   -148.00-111.00   1.00    7.00    --  -90.00 -69.00-141.10   37
 55  ω    -90.00 -62.00   1.00    7.00    --  -90.00 -69.00-141.10   28
 56  ω   -161.00-117.00   1.00    7.00    --  -90.00 -68.00 -38.29   44
 57  ω    -99.00 -61.00   1.00    7.00    --  -90.00 -68.00 -38.29   38
 58  ω    -97.00 -53.00   1.00    7.00    --  -90.00  77.00 -60.00   44
 59  ω   -113.00 -88.00   1.00    7.00    --  -90.00  45.00 -60.00   25
 60  ω    -73.00 -32.00   1.00    7.00    --  -90.00  45.00 -60.00   41
 61  ω   -141.00 -61.00   1.00    7.00    --  -90.00 -68.00  26.54   80
 62  ω    -89.00 -60.00   1.00    7.00    --  -90.00 -71.00  78.48   29
 63  ω   -121.00 -70.00   1.00    7.00    --  -90.00  77.00-120.00   51
 64  ω    -99.00 -66.00   1.00    7.00    --  -90.00 -65.00-119.48   33
 65  ω   -153.00-104.00   1.00    7.00    --  -90.00 -71.00  78.48   49
 66  ω   -114.00 -19.00   1.00    7.00    --  -90.00  45.00  30.00   95
 67  ω   -101.00 -61.00   1.00    7.00    --  -90.00 -67.00  60.81   40
 68  ω   -109.00 -61.00   1.00    7.00    --  -90.00 -70.00 -51.59   48
 69  ω   -105.00 -70.00   1.00    7.00    --  -90.00 104.00  54.94   35
 70  ω    -48.00 -12.00   1.00    7.00    --  -90.00 104.00  54.94   36
 71  ω    -86.00 -61.00   1.00    7.00    --  -90.00 -67.00  93.50   25
 72  ω    -54.00 -27.00   1.00    7.00    --  -90.00  61.00-180.00   27
 73  ω   -114.00 -66.00   1.00    7.00    --  -90.00  61.00-180.00   48
 74  ω    -88.00 -61.00   1.00    7.00    --  -90.00 -68.00 107.51   27
 75  ω   -159.00 -61.00   1.00    7.00    --  -90.00 -70.00  53.84   98
 76  ω   -131.00-104.00   1.00    7.00    --  -90.00 -67.00  60.81   27
 77  ω   -152.00 -91.00   1.00    7.00    --  -90.00 -68.00 107.51   61
 78  ω    -87.00 -62.00   1.00    7.00    --  -90.00 -65.00  79.80   25
 79  ω    -87.00 -61.00   1.00    7.00    --  -90.00 -68.00-177.69   26
 80  ω   -107.00 -64.00   1.00    7.00    --  -90.00 -59.00 -23.38   43
 81  ω   -151.00-124.00   1.00    7.00    --  -90.00 -59.00 -23.38   27
 82  ω   -127.00-100.00   1.00    7.00    --  -90.00 -67.00  93.50   27
 83  ω   -158.00 -97.00   1.00    7.00    --  -90.00 -68.00-177.69   61
 84  ω    -96.00 -69.00   1.00    7.00    --  -90.00 125.00 120.00   27
 85  ω   -148.00 -60.00   1.00    7.00    --  -90.00 -71.00 -93.85   88
 86  ω   -112.00 -45.00   1.00    7.00    --  -90.00 125.00-180.00   67
 87  ω    -86.00 -61.00   1.00    7.00    --  -90.00 -71.00 137.75   25
 88  ω   -111.00 -66.00   1.00    7.00    --  -90.00 125.00  60.00   45
 89  ω    -76.00 -19.00   1.00    7.00    --  -90.00  45.00-180.00   57
 90  ω   -125.00 -62.00   1.00    7.00    --  -90.00 -66.00-165.37   63
 91  ω   -120.00 -93.00   1.00    7.00    --  -90.00  84.00  41.78   27
 92  ω    -66.00 -14.00   1.00    7.00    --  -90.00  84.00  41.78   52
 93  ω   -116.00 -76.00   1.00    7.00    --  -90.00  13.00   5.00   40
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.1605872000
_diffrn_orient_matrix_UB_12      0.0152624000
_diffrn_orient_matrix_UB_13      -0.0035845000
_diffrn_orient_matrix_UB_21      -0.0464030000
_diffrn_orient_matrix_UB_22      -0.1446639000
_diffrn_orient_matrix_UB_23      0.0162098000
_diffrn_orient_matrix_UB_31      0.0276712000
_diffrn_orient_matrix_UB_32      0.0314744000
_diffrn_orient_matrix_UB_33      0.0938915000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5447
_reflns_number_total             5528
_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 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection       
'CrysAlisPro system (CCD 42.90a 64-bit (release 14-04-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         1.060
_refine_diff_density_min         -0.475
_refine_diff_density_rms         0.092
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.152
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         5528
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0523
_refine_ls_R_factor_gt           0.0518
_refine_ls_restrained_S_all      1.152
_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)+(0.0244P)²+7.0505P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1228
_refine_ls_wR_factor_ref         0.1230
_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:
 C18(H18A,H18B), C17(H17A,H17B), C23(H23A,H23B), C19(H19A,H19B), C21(H21A,
 H21B), C24(H24A,H24B), C20(H20A,H20B), C16(H16A,H16B), C22(H22A,H22B),
 C25(H25A,H25B), C26(H26A,H26B), C27(H27A,H27B)
2.b Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C5(H5A,H5B,H5C), C9(H9A,H9B,H9C), C7(H7A,H7B,H7C),
 C10(H10A,H10B,H10C), C6(H6A,H6B,H6C), C13(H13A,H13B,H13C), C15(H15A,H15B,H15C),
  C11(H11A,H11B,H11C)
;
_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
Rb1 Rb 0.59218(4) 0.37111(4) 0.25864(2) 0.02314(12) Uani 1 1 d . . . . .
P2 P 0.23376(12) 0.28303(9) 0.14661(6) 0.0229(2) Uani 1 1 d . . . . .
P1 P 0.24784(11) 0.28617(9) 0.32615(6) 0.0218(2) Uani 1 1 d . . . . .
O3 O 0.7490(4) 0.2835(3) 0.41340(19) 0.0338(7) Uani 1 1 d . . . . .
O2 O 0.8176(3) 0.2172(3) 0.2626(2) 0.0335(7) Uani 1 1 d . . . . .
O5 O 0.7519(4) 0.6610(3) 0.2788(2) 0.0380(8) Uani 1 1 d . . . . .
O4 O 0.6518(4) 0.5259(3) 0.41268(19) 0.0348(7) Uani 1 1 d . . . . .
O1 O 0.6714(4) 0.2723(3) 0.1103(2) 0.0375(8) Uani 1 1 d . . . . .
O6 O 0.6754(5) 0.5473(3) 0.1210(2) 0.0479(9) Uani 1 1 d . . . . .
C2 C 0.2674(4) 0.1370(4) 0.2810(2) 0.0205(8) Uani 1 1 d . . . . .
C3 C 0.2611(4) 0.1363(4) 0.1937(2) 0.0226(8) Uani 1 1 d . . . . .
C4 C 0.2073(5) 0.5107(4) 0.2381(3) 0.0259(9) Uani 1 1 d . . . . .
C12 C 0.2579(5) 0.0243(4) 0.1298(3) 0.0263(9) Uani 1 1 d . . . . .
C8 C 0.2874(5) 0.0318(4) 0.3443(3) 0.0257(9) Uani 1 1 d . . . . .
C1 C 0.2273(4) 0.3734(4) 0.2355(2) 0.0225(8) Uani 1 1 d . . . . .
C14 C 0.3711(5) -0.0611(4) 0.1545(3) 0.0331(10) Uani 1 1 d . . . . .
H14A H 0.470216 -0.006971 0.164281 0.050 Uiso 1 1 calc R U . . .
H14B H 0.365016 -0.125241 0.109852 0.050 Uiso 1 1 calc R U . . .
H14C H 0.350059 -0.105272 0.205185 0.050 Uiso 1 1 calc R U . . .
C5 C 0.0820(5) 0.5238(4) 0.2867(3) 0.0313(10) Uani 1 1 d . . . . .
H5A H -0.007724 0.462449 0.263212 0.047 Uiso 1 1 calc R U . . .
H5B H 0.064356 0.611956 0.283108 0.047 Uiso 1 1 calc R U . . .
H5C H 0.109626 0.505176 0.344849 0.047 Uiso 1 1 calc R U . . .
C18 C 0.8456(5) 0.1426(4) 0.3322(3) 0.0373(11) Uani 1 1 d . . . . .
H18A H 0.932693 0.104632 0.328130 0.045 Uiso 1 1 calc R U . . .
H18B H 0.760217 0.071263 0.334451 0.045 Uiso 1 1 calc R U . . .
C9 C 0.2619(5) 0.0702(4) 0.4315(3) 0.0342(10) Uani 1 1 d . . . . .
H9A H 0.330001 0.151238 0.450950 0.051 Uiso 1 1 calc R U . . .
H9B H 0.279043 0.001986 0.469638 0.051 Uiso 1 1 calc R U . . .
H9C H 0.160428 0.081889 0.429306 0.051 Uiso 1 1 calc R U . . .
C7 C 0.1727(6) 0.5591(4) 0.1509(3) 0.0354(10) Uani 1 1 d . . . . .
H7A H 0.252315 0.551854 0.119473 0.053 Uiso 1 1 calc R U . . .
H7B H 0.163711 0.649667 0.154524 0.053 Uiso 1 1 calc R U . . .
H7C H 0.080075 0.506779 0.122770 0.053 Uiso 1 1 calc R U . . .
C10 C 0.1771(5) -0.0963(4) 0.3214(3) 0.0310(10) Uani 1 1 d . . . . .
H10A H 0.076673 -0.081013 0.316074 0.046 Uiso 1 1 calc R U . . .
H10B H 0.191065 -0.157936 0.364788 0.046 Uiso 1 1 calc R U . . .
H10C H 0.193368 -0.131688 0.268653 0.046 Uiso 1 1 calc R U . . .
C6 C 0.3513(5) 0.5981(4) 0.2799(3) 0.0335(10) Uani 1 1 d . . . . .
H6A H 0.382252 0.564393 0.333810 0.050 Uiso 1 1 calc R U . . .
H6B H 0.335428 0.685942 0.287640 0.050 Uiso 1 1 calc R U . . .
H6C H 0.427881 0.599426 0.244850 0.050 Uiso 1 1 calc R U . . .
C17 C 0.8330(5) 0.1557(5) 0.1871(3) 0.0401(12) Uani 1 1 d . . . . .
H17A H 0.757454 0.075237 0.175495 0.048 Uiso 1 1 calc R U . . .
H17B H 0.931231 0.133205 0.191734 0.048 Uiso 1 1 calc R U . . .
C23 C 0.7426(6) 0.7231(4) 0.3554(3) 0.0401(11) Uani 1 1 d . . . . .
H23A H 0.644358 0.744771 0.353405 0.048 Uiso 1 1 calc R U . . .
H23B H 0.817572 0.804308 0.364724 0.048 Uiso 1 1 calc R U . . .
C13 C 0.2948(6) 0.0776(4) 0.0458(3) 0.0366(11) Uani 1 1 d . . . . .
H13A H 0.223677 0.129613 0.023624 0.055 Uiso 1 1 calc R U . . .
H13B H 0.290088 0.005379 0.006737 0.055 Uiso 1 1 calc R U . . .
H13C H 0.394118 0.131379 0.053706 0.055 Uiso 1 1 calc R U . . .
C15 C 0.1013(5) -0.0587(4) 0.1117(3) 0.0341(10) Uani 1 1 d . . . . .
H15A H 0.070904 -0.092574 0.163519 0.051 Uiso 1 1 calc R U . . .
H15B H 0.100139 -0.130769 0.073347 0.051 Uiso 1 1 calc R U . . .
H15C H 0.033279 -0.005612 0.086877 0.051 Uiso 1 1 calc R U . . .
C19 C 0.8728(5) 0.2277(5) 0.4084(3) 0.0377(11) Uani 1 1 d . . . . .
H19A H 0.891358 0.176475 0.457844 0.045 Uiso 1 1 calc R U . . .
H19B H 0.960818 0.296707 0.407115 0.045 Uiso 1 1 calc R U . . .
C21 C 0.6517(6) 0.4394(5) 0.4804(3) 0.0411(12) Uani 1 1 d . . . . .
H21A H 0.555618 0.378377 0.474049 0.049 Uiso 1 1 calc R U . . .
H21B H 0.662598 0.490278 0.532875 0.049 Uiso 1 1 calc R U . . .
C24 C 0.7278(6) 0.7351(5) 0.2093(3) 0.0441(12) Uani 1 1 d . . . . .
H24A H 0.788937 0.823216 0.219605 0.053 Uiso 1 1 calc R U . . .
H24B H 0.623273 0.742386 0.198730 0.053 Uiso 1 1 calc R U . . .
C20 C 0.7709(6) 0.3643(5) 0.4857(3) 0.0431(12) Uani 1 1 d . . . . .
H20A H 0.867800 0.424060 0.490801 0.052 Uiso 1 1 calc R U . . .
H20B H 0.769462 0.311126 0.535286 0.052 Uiso 1 1 calc R U . . .
C16 C 0.8150(6) 0.2470(5) 0.1187(3) 0.0430(12) Uani 1 1 d . . . . .
H16A H 0.888425 0.328689 0.131371 0.052 Uiso 1 1 calc R U . . .
H16B H 0.831097 0.208468 0.066191 0.052 Uiso 1 1 calc R U . . .
C11 C 0.4473(5) 0.0108(5) 0.3566(3) 0.0363(11) Uani 1 1 d . . . . .
H11A H 0.473603 -0.010545 0.303032 0.054 Uiso 1 1 calc R U . . .
H11B H 0.455663 -0.060314 0.393890 0.054 Uiso 1 1 calc R U . . .
H11C H 0.513937 0.089935 0.380763 0.054 Uiso 1 1 calc R U . . .
C22 C 0.7675(6) 0.6352(5) 0.4237(3) 0.0410(11) Uani 1 1 d . . . . .
H22A H 0.862705 0.608586 0.423339 0.049 Uiso 1 1 calc R U . . .
H22B H 0.770443 0.679989 0.477570 0.049 Uiso 1 1 calc R U . . .
C25 C 0.7662(6) 0.6734(5) 0.1370(4) 0.0490(13) Uani 1 1 d . . . . .
H25A H 0.751709 0.726577 0.088072 0.059 Uiso 1 1 calc R U . . .
H25B H 0.870928 0.666773 0.147448 0.059 Uiso 1 1 calc R U . . .
C26 C 0.7129(7) 0.4883(5) 0.0510(3) 0.0508(14) Uani 1 1 d . . . . .
H26A H 0.820273 0.492397 0.058192 0.061 Uiso 1 1 calc R U . . .
H26B H 0.685222 0.534454 0.000639 0.061 Uiso 1 1 calc R U . . .
C27 C 0.6333(8) 0.3517(6) 0.0423(3) 0.0576(16) Uani 1 1 d . . . . .
H27A H 0.526396 0.349843 0.036097 0.069 Uiso 1 1 calc R U . . .
H27B H 0.653068 0.313035 -0.009266 0.069 Uiso 1 1 calc R U . . .


_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
Rb1 P2 3.5307(11) . ?
Rb1 P1 3.5158(11) . ?
Rb1 O3 2.988(3) . ?
Rb1 O2 2.910(3) . ?
Rb1 O5 3.122(3) . ?
Rb1 O4 2.912(3) . ?
Rb1 O1 2.883(3) . ?
Rb1 O6 3.023(3) . ?
Rb1 C2 3.588(4) . ?
Rb1 C3 3.586(4) . ?
Rb1 C1 3.396(4) . ?
Rb1 C27 3.621(5) . ?
P2 C3 1.786(4) . ?
P2 C1 1.747(4) . ?
P1 C2 1.789(4) . ?
P1 C1 1.760(4) . ?
O3 C19 1.416(6) . ?
O3 C20 1.418(6) . ?
O2 C18 1.413(6) . ?
O2 C17 1.428(6) . ?
O5 C23 1.430(6) . ?
O5 C24 1.402(6) . ?
O4 C21 1.442(6) . ?
O4 C22 1.409(6) . ?
O1 C16 1.414(6) . ?
O1 C27 1.446(6) . ?
O6 C25 1.431(6) . ?
O6 C26 1.419(6) . ?
C2 C3 1.419(6) . ?
C2 C8 1.546(5) . ?
C3 C12 1.564(5) . ?
C4 C1 1.501(6) . ?
C4 C5 1.539(6) . ?
C4 C7 1.530(6) . ?
C4 C6 1.539(6) . ?
C12 C14 1.540(6) . ?
C12 C13 1.548(6) . ?
C12 C15 1.540(6) . ?
C8 C9 1.544(6) . ?
C8 C10 1.537(6) . ?
C8 C11 1.546(6) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C19 1.490(7) . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C17 C16 1.498(8) . ?
C23 H23A 0.9900 . ?
C23 H23B 0.9900 . ?
C23 C22 1.482(7) . ?
C13 H13A 0.9800 . ?
C13 H13B 0.9800 . ?
C13 H13C 0.9800 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C21 C20 1.489(7) . ?
C24 H24A 0.9900 . ?
C24 H24B 0.9900 . ?
C24 C25 1.468(8) . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C25 H25A 0.9900 . ?
C25 H25B 0.9900 . ?
C26 H26A 0.9900 . ?
C26 H26B 0.9900 . ?
C26 C27 1.482(8) . ?
C27 H27A 0.9900 . ?
C27 H27B 0.9900 . ?

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 Rb1 C2 44.79(6) . . ?
P2 Rb1 C3 29.05(6) . . ?
P2 Rb1 C27 73.44(11) . . ?
P1 Rb1 P2 48.92(2) . . ?
P1 Rb1 C2 29.15(6) . . ?
P1 Rb1 C3 44.75(7) . . ?
P1 Rb1 C27 122.15(11) . . ?
O3 Rb1 P2 134.83(6) . . ?
O3 Rb1 P1 92.67(6) . . ?
O3 Rb1 O5 96.85(9) . . ?
O3 Rb1 O6 136.33(10) . . ?
O3 Rb1 C2 90.04(9) . . ?
O3 Rb1 C3 108.45(9) . . ?
O3 Rb1 C1 121.68(9) . . ?
O3 Rb1 C27 133.62(13) . . ?
O2 Rb1 P2 124.73(7) . . ?
O2 Rb1 P1 127.78(6) . . ?
O2 Rb1 O3 55.67(9) . . ?
O2 Rb1 O5 107.40(9) . . ?
O2 Rb1 O4 107.66(9) . . ?
O2 Rb1 O6 99.22(10) . . ?
O2 Rb1 C2 103.40(9) . . ?
O2 Rb1 C3 102.29(9) . . ?
O2 Rb1 C1 147.06(9) . . ?
O2 Rb1 C27 78.15(13) . . ?
O5 Rb1 P2 120.20(6) . . ?
O5 Rb1 P1 117.66(6) . . ?
O5 Rb1 C2 146.67(9) . . ?
O5 Rb1 C3 148.55(9) . . ?
O5 Rb1 C1 105.50(9) . . ?
O5 Rb1 C27 92.74(11) . . ?
O4 Rb1 P2 121.58(7) . . ?
O4 Rb1 P1 80.14(7) . . ?
O4 Rb1 O3 58.58(8) . . ?
O4 Rb1 O5 55.10(9) . . ?
O4 Rb1 O6 108.21(9) . . ?
O4 Rb1 C2 103.44(9) . . ?
O4 Rb1 C3 124.32(9) . . ?
O4 Rb1 C1 92.45(9) . . ?
O4 Rb1 C27 147.80(11) . . ?
O1 Rb1 P2 82.53(7) . . ?
O1 Rb1 P1 125.92(7) . . ?
O1 Rb1 O3 113.07(9) . . ?
O1 Rb1 O2 57.54(9) . . ?
O1 Rb1 O5 105.91(9) . . ?
O1 Rb1 O4 153.91(10) . . ?
O1 Rb1 O6 58.85(9) . . ?
O1 Rb1 C2 101.12(9) . . ?
O1 Rb1 C3 81.45(9) . . ?
O1 Rb1 C1 111.20(10) . . ?
O1 Rb1 C27 22.19(12) . . ?
O6 Rb1 P2 88.52(8) . . ?
O6 Rb1 P1 128.04(8) . . ?
O6 Rb1 O5 53.53(9) . . ?
O6 Rb1 C2 132.88(10) . . ?
O6 Rb1 C3 111.90(10) . . ?
O6 Rb1 C1 98.82(10) . . ?
O6 Rb1 C27 40.36(11) . . ?
C2 Rb1 C27 105.88(12) . . ?
C3 Rb1 C2 22.83(9) . . ?
C3 Rb1 C27 83.30(12) . . ?
C1 Rb1 P2 29.13(7) . . ?
C1 Rb1 P1 29.43(7) . . ?
C1 Rb1 C2 45.32(9) . . ?
C1 Rb1 C3 45.13(9) . . ?
C1 Rb1 C27 98.73(13) . . ?
C3 P2 Rb1 77.18(13) . . ?
C1 P2 Rb1 71.16(13) . . ?
C1 P2 C3 98.93(19) . . ?
C2 P1 Rb1 77.66(12) . . ?
C1 P1 Rb1 71.52(13) . . ?
C1 P1 C2 98.91(18) . . ?
C19 O3 Rb1 118.9(3) . . ?
C19 O3 C20 111.2(4) . . ?
C20 O3 Rb1 117.4(3) . . ?
C18 O2 Rb1 119.1(3) . . ?
C18 O2 C17 112.6(4) . . ?
C17 O2 Rb1 118.2(3) . . ?
C23 O5 Rb1 114.4(3) . . ?
C24 O5 Rb1 115.4(3) . . ?
C24 O5 C23 114.1(4) . . ?
C21 O4 Rb1 108.1(3) . . ?
C22 O4 Rb1 119.6(3) . . ?
C22 O4 C21 114.5(4) . . ?
C16 O1 Rb1 115.1(3) . . ?
C16 O1 C27 115.6(4) . . ?
C27 O1 Rb1 109.0(3) . . ?
C25 O6 Rb1 122.3(3) . . ?
C26 O6 Rb1 116.3(3) . . ?
C26 O6 C25 109.4(4) . . ?
P1 C2 Rb1 73.19(12) . . ?
C3 C2 Rb1 78.5(2) . . ?
C3 C2 P1 114.4(3) . . ?
C3 C2 C8 131.6(3) . . ?
C8 C2 Rb1 116.2(2) . . ?
C8 C2 P1 114.0(3) . . ?
P2 C3 Rb1 73.77(13) . . ?
C2 C3 Rb1 78.7(2) . . ?
C2 C3 P2 115.2(3) . . ?
C2 C3 C12 131.0(3) . . ?
C12 C3 Rb1 120.9(2) . . ?
C12 C3 P2 113.5(3) . . ?
C1 C4 C5 110.8(3) . . ?
C1 C4 C7 111.4(3) . . ?
C1 C4 C6 109.2(3) . . ?
C5 C4 C6 109.4(4) . . ?
C7 C4 C5 108.8(4) . . ?
C7 C4 C6 107.2(4) . . ?
C14 C12 C3 115.0(3) . . ?
C14 C12 C13 103.9(4) . . ?
C13 C12 C3 111.3(3) . . ?
C15 C12 C3 109.5(3) . . ?
C15 C12 C14 110.6(3) . . ?
C15 C12 C13 106.1(4) . . ?
C9 C8 C2 112.6(3) . . ?
C9 C8 C11 104.4(4) . . ?
C10 C8 C2 112.8(3) . . ?
C10 C8 C9 104.6(4) . . ?
C10 C8 C11 111.1(4) . . ?
C11 C8 C2 110.9(3) . . ?
P2 C1 Rb1 79.71(13) . . ?
P2 C1 P1 112.6(2) . . ?
P1 C1 Rb1 79.05(13) . . ?
C4 C1 Rb1 109.2(2) . . ?
C4 C1 P2 125.8(3) . . ?
C4 C1 P1 121.6(3) . . ?
C12 C14 H14A 109.5 . . ?
C12 C14 H14B 109.5 . . ?
C12 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C4 C5 H5A 109.5 . . ?
C4 C5 H5B 109.5 . . ?
C4 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?
O2 C18 H18A 109.9 . . ?
O2 C18 H18B 109.9 . . ?
O2 C18 C19 108.8(4) . . ?
H18A C18 H18B 108.3 . . ?
C19 C18 H18A 109.9 . . ?
C19 C18 H18B 109.9 . . ?
C8 C9 H9A 109.5 . . ?
C8 C9 H9B 109.5 . . ?
C8 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C4 C7 H7A 109.5 . . ?
C4 C7 H7B 109.5 . . ?
C4 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C8 C10 H10A 109.5 . . ?
C8 C10 H10B 109.5 . . ?
C8 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
Rb1 C6 H6A 69.6 . . ?
Rb1 C6 H6B 151.4 . . ?
Rb1 C6 H6C 49.2 . . ?
C4 C6 Rb1 97.1(2) . . ?
C4 C6 H6A 109.5 . . ?
C4 C6 H6B 109.5 . . ?
C4 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
O2 C17 H17A 110.0 . . ?
O2 C17 H17B 110.0 . . ?
O2 C17 C16 108.4(4) . . ?
H17A C17 H17B 108.4 . . ?
C16 C17 H17A 110.0 . . ?
C16 C17 H17B 110.0 . . ?
O5 C23 H23A 109.8 . . ?
O5 C23 H23B 109.8 . . ?
O5 C23 C22 109.2(4) . . ?
H23A C23 H23B 108.3 . . ?
C22 C23 H23A 109.8 . . ?
C22 C23 H23B 109.8 . . ?
C12 C13 H13A 109.5 . . ?
C12 C13 H13B 109.5 . . ?
C12 C13 H13C 109.5 . . ?
H13A C13 H13B 109.5 . . ?
H13A C13 H13C 109.5 . . ?
H13B C13 H13C 109.5 . . ?
C12 C15 H15A 109.5 . . ?
C12 C15 H15B 109.5 . . ?
C12 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
O3 C19 C18 109.8(4) . . ?
O3 C19 H19A 109.7 . . ?
O3 C19 H19B 109.7 . . ?
C18 C19 H19A 109.7 . . ?
C18 C19 H19B 109.7 . . ?
H19A C19 H19B 108.2 . . ?
Rb1 C21 H21A 79.8 . . ?
Rb1 C21 H21B 158.1 . . ?
O4 C21 Rb1 49.71(19) . . ?
O4 C21 H21A 108.9 . . ?
O4 C21 H21B 108.9 . . ?
O4 C21 C20 113.5(4) . . ?
H21A C21 H21B 107.7 . . ?
C20 C21 Rb1 87.1(3) . . ?
C20 C21 H21A 108.9 . . ?
C20 C21 H21B 108.9 . . ?
O5 C24 H24A 109.8 . . ?
O5 C24 H24B 109.8 . . ?
O5 C24 C25 109.4(4) . . ?
H24A C24 H24B 108.2 . . ?
C25 C24 H24A 109.8 . . ?
C25 C24 H24B 109.8 . . ?
O3 C20 C21 109.1(4) . . ?
O3 C20 H20A 109.9 . . ?
O3 C20 H20B 109.9 . . ?
C21 C20 H20A 109.9 . . ?
C21 C20 H20B 109.9 . . ?
H20A C20 H20B 108.3 . . ?
Rb1 C16 H16A 87.5 . . ?
Rb1 C16 H16B 154.5 . . ?
O1 C16 Rb1 44.7(2) . . ?
O1 C16 C17 109.0(4) . . ?
O1 C16 H16A 109.9 . . ?
O1 C16 H16B 109.9 . . ?
C17 C16 Rb1 81.9(3) . . ?
C17 C16 H16A 109.9 . . ?
C17 C16 H16B 109.9 . . ?
H16A C16 H16B 108.3 . . ?
C8 C11 H11A 109.5 . . ?
C8 C11 H11B 109.5 . . ?
C8 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
O4 C22 C23 108.5(4) . . ?
O4 C22 H22A 110.0 . . ?
O4 C22 H22B 110.0 . . ?
C23 C22 H22A 110.0 . . ?
C23 C22 H22B 110.0 . . ?
H22A C22 H22B 108.4 . . ?
O6 C25 C24 109.7(4) . . ?
O6 C25 H25A 109.7 . . ?
O6 C25 H25B 109.7 . . ?
C24 C25 H25A 109.7 . . ?
C24 C25 H25B 109.7 . . ?
H25A C25 H25B 108.2 . . ?
O6 C26 H26A 109.9 . . ?
O6 C26 H26B 109.9 . . ?
O6 C26 C27 108.8(5) . . ?
H26A C26 H26B 108.3 . . ?
C27 C26 H26A 109.9 . . ?
C27 C26 H26B 109.9 . . ?
Rb1 C27 H27A 80.7 . . ?
Rb1 C27 H27B 157.0 . . ?
O1 C27 Rb1 48.8(2) . . ?
O1 C27 C26 115.0(5) . . ?
O1 C27 H27A 108.5 . . ?
O1 C27 H27B 108.5 . . ?
C26 C27 Rb1 88.1(3) . . ?
C26 C27 H27A 108.5 . . ?
C26 C27 H27B 108.5 . . ?
H27A C27 H27B 107.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
Rb1 P2 C3 C2 68.7(3) . . . . ?
Rb1 P2 C3 C12 -117.2(3) . . . . ?
Rb1 P2 C1 P1 -73.46(18) . . . . ?
Rb1 P2 C1 C4 106.3(3) . . . . ?
Rb1 P1 C2 C3 -68.6(3) . . . . ?
Rb1 P1 C2 C8 111.7(3) . . . . ?
Rb1 P1 C1 P2 73.88(18) . . . . ?
Rb1 P1 C1 C4 -105.9(3) . . . . ?
Rb1 O3 C19 C18 -39.4(4) . . . . ?
Rb1 O3 C20 C21 27.8(5) . . . . ?
Rb1 O2 C18 C19 -52.4(4) . . . . ?
Rb1 O2 C17 C16 40.0(4) . . . . ?
Rb1 O5 C23 C22 43.1(5) . . . . ?
Rb1 O5 C24 C25 -54.7(5) . . . . ?
Rb1 O4 C21 C20 63.8(5) . . . . ?
Rb1 O4 C22 C23 56.7(4) . . . . ?
Rb1 O1 C16 C17 56.0(4) . . . . ?
Rb1 O1 C27 C26 62.9(6) . . . . ?
Rb1 O6 C25 C24 -39.0(6) . . . . ?
Rb1 O6 C26 C27 28.5(6) . . . . ?
Rb1 C2 C3 P2 -65.9(2) . . . . ?
Rb1 C2 C3 C12 121.3(4) . . . . ?
Rb1 C2 C8 C9 91.3(4) . . . . ?
Rb1 C2 C8 C10 -150.6(3) . . . . ?
Rb1 C2 C8 C11 -25.3(4) . . . . ?
Rb1 C3 C12 C14 56.4(4) . . . . ?
Rb1 C3 C12 C13 -61.5(4) . . . . ?
Rb1 C3 C12 C15 -178.4(3) . . . . ?
Rb1 C21 C20 O3 -19.9(4) . . . . ?
P2 C3 C12 C14 141.0(3) . . . . ?
P2 C3 C12 C13 23.1(4) . . . . ?
P2 C3 C12 C15 -93.8(4) . . . . ?
P1 C2 C3 Rb1 65.4(2) . . . . ?
P1 C2 C3 P2 -0.5(4) . . . . ?
P1 C2 C3 C12 -173.3(3) . . . . ?
P1 C2 C8 C9 9.0(4) . . . . ?
P1 C2 C8 C10 127.1(3) . . . . ?
P1 C2 C8 C11 -107.6(4) . . . . ?
O2 C18 C19 O3 58.6(5) . . . . ?
O2 C17 C16 Rb1 -26.7(3) . . . . ?
O2 C17 C16 O1 -62.8(5) . . . . ?
O5 C23 C22 O4 -64.8(5) . . . . ?
O5 C24 C25 O6 60.8(6) . . . . ?
O4 C21 C20 O3 -63.2(6) . . . . ?
O6 C26 C27 Rb1 -20.9(4) . . . . ?
O6 C26 C27 O1 -63.0(7) . . . . ?
C2 P1 C1 Rb1 -73.71(14) . . . . ?
C2 P1 C1 P2 0.2(2) . . . . ?
C2 P1 C1 C4 -179.6(3) . . . . ?
C2 C3 C12 C14 -46.1(6) . . . . ?
C2 C3 C12 C13 -164.0(4) . . . . ?
C2 C3 C12 C15 79.1(5) . . . . ?
C3 P2 C1 Rb1 73.09(14) . . . . ?
C3 P2 C1 P1 -0.4(2) . . . . ?
C3 P2 C1 C4 179.4(3) . . . . ?
C3 C2 C8 C9 -170.6(4) . . . . ?
C3 C2 C8 C10 -52.6(6) . . . . ?
C3 C2 C8 C11 72.7(5) . . . . ?
C8 C2 C3 Rb1 -114.9(4) . . . . ?
C8 C2 C3 P2 179.2(3) . . . . ?
C8 C2 C3 C12 6.4(7) . . . . ?
C1 P2 C3 Rb1 -68.22(14) . . . . ?
C1 P2 C3 C2 0.5(3) . . . . ?
C1 P2 C3 C12 174.6(3) . . . . ?
C1 P1 C2 Rb1 68.73(13) . . . . ?
C1 P1 C2 C3 0.2(3) . . . . ?
C1 P1 C2 C8 -179.6(3) . . . . ?
C1 C4 C6 Rb1 17.5(3) . . . . ?
C5 C4 C1 Rb1 -140.3(3) . . . . ?
C5 C4 C1 P2 128.7(4) . . . . ?
C5 C4 C1 P1 -51.6(5) . . . . ?
C5 C4 C6 Rb1 138.8(3) . . . . ?
C18 O2 C17 C16 -174.8(4) . . . . ?
C7 C4 C1 Rb1 98.4(3) . . . . ?
C7 C4 C1 P2 7.4(5) . . . . ?
C7 C4 C1 P1 -172.9(3) . . . . ?
C7 C4 C6 Rb1 -103.3(3) . . . . ?
C6 C4 C1 Rb1 -19.8(4) . . . . ?
C6 C4 C1 P2 -110.9(4) . . . . ?
C6 C4 C1 P1 68.9(4) . . . . ?
C17 O2 C18 C19 162.7(4) . . . . ?
C23 O5 C24 C25 169.7(4) . . . . ?
C19 O3 C20 C21 169.4(4) . . . . ?
C21 O4 C22 C23 -172.6(4) . . . . ?
C24 O5 C23 C22 179.1(4) . . . . ?
C20 O3 C19 C18 179.5(4) . . . . ?
C16 O1 C27 Rb1 -131.4(4) . . . . ?
C16 O1 C27 C26 -68.4(6) . . . . ?
C22 O4 C21 Rb1 -136.1(4) . . . . ?
C22 O4 C21 C20 -72.3(5) . . . . ?
C25 O6 C26 C27 172.2(5) . . . . ?
C26 O6 C25 C24 179.9(5) . . . . ?
C27 O1 C16 Rb1 128.4(4) . . . . ?
C27 O1 C16 C17 -175.6(4) . . . . ?

_olex2_date_sample_data_collection 2023-05-05
_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 1.843
_oxdiff_exptl_absorpt_empirical_full_min 0.760
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane/THF'
####################################################################### 
# 
# 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_mu321_2_mc
_database_code_depnum_ccdc_archive 'CCDC 2346032'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        tBu4C4P6
_chemical_formula_moiety         'C20 H36 P6'
_chemical_formula_sum            'C20 H36 P6'
_chemical_formula_weight         462.31
_chemical_melting_point          ?
_chemical_oxdiff_formula         'C20 H36 P6'
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      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                   19.2177(5)
_cell_length_b                   12.5176(3)
_cell_length_c                   22.1442(6)
_cell_angle_alpha                90
_cell_angle_beta                 112.755(3)
_cell_angle_gamma                90
_cell_volume                     4912.4(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    8453
_cell_measurement_temperature    123.00(10)
_cell_measurement_theta_max      74.7690
_cell_measurement_theta_min      4.3280
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    4.088
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.738
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.43.36a (Rigaku Oxford Diffraction, 2022)
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 brownish colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   brownish
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1968
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 8 0 0.0224
-4 -2 -10 0.0509
0 -8 4 0.0308
4 2 10 0.0232
12 0 -10 0.0171
-12 0 10 0.0095

_exptl_crystal_size_max          0.097
_exptl_crystal_size_mid          0.072
_exptl_crystal_size_min          0.029
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
1.6040 8.0557 -0.2998 0.5743 0.1750 -0.7997
-3.8627 -2.3575 -10.2787 0.5130 0.1489 0.8454
-0.3075 -7.7577 4.0682 -0.8014 -0.2415 0.5472
3.8504 2.0603 10.4329 -0.5436 -0.1581 -0.8243
11.7606 -0.0622 -9.6643 -0.1840 0.9818 -0.0462
-11.6480 0.2877 9.9161 0.1839 -0.9829 0.0092

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0389
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.982
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            39101
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.982
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         75.400
_diffrn_reflns_theta_min         4.324
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 10.0000
_diffrn_detector_type            'HyPix-Arc 150'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω     34.00  59.00   0.50    1.42    --   62.92  15.00 -30.00   50
  2  ω     28.00  57.00   0.50    1.42    --   62.92 -95.00  90.00   58
  3  ω     68.00 107.00   0.50    1.42    --   62.92  15.00 -30.00   78
  4  ω     26.00  68.00   0.50    1.42    --   62.92 -95.00-150.00   84
  5  ω     26.00  51.00   0.50    1.42    --   62.92 -95.00  60.00   50
  6  ω    -60.00 -25.00   0.50    1.42    --  -63.82 125.00 -60.00   70
  7  ω   -106.00 -70.00   0.50    1.42    --  -63.82 -15.00 150.00   72
  8  ω    -74.00 -24.00   0.50    1.42    --  -63.82 125.00  90.00  100
  9  ω    -97.00 -54.00   0.50    1.42    --  -73.68 125.00-180.00   86
 10  ω   -100.00 -68.00   0.50    1.42    --  -73.68 125.00  60.00   64
 11  ω   -117.00 -47.00   0.50    1.42    --  -73.68 -15.00-120.00  140
 12  ω   -110.00 -40.00   0.50    1.42    --  -73.68   0.00 -30.00  140
 13  ω   -100.00 -38.00   0.50    1.42    --  -73.68 125.00 -90.00  124
 14  ω     42.00  68.00   0.50    1.42    --   75.56 -95.00-120.00   52
 15  ω     40.00  65.00   0.50    1.42    --   75.87 -95.00 150.00   50
 16  ω     42.00  68.00   0.50    1.42    --   75.87 -95.00-180.00   52
 17  ω     52.00  77.00   0.50    1.42    --   75.87  15.00 -30.00   50
 18  ω    -73.00 -46.00   0.50    1.42    --  -76.65 -15.00  90.00   54
 19  ω   -114.00 -88.00   0.50    1.42    --  -78.25-172.00 -55.85   52
 20  ω   -111.00 -80.00   0.50    1.42    --  -78.25 -86.00-149.68   62
 21  ω    -69.00 -43.00   0.50    1.42    --  -78.25  89.00  58.97   52
 22  ω   -112.00 -76.00   0.50    1.42    --  -78.25 135.00  -7.59   72
 23  ω    -64.00 -37.00   0.50    1.42    --  -78.25 120.00  61.17   54
 24  ω    -88.00 -62.00   0.50    1.42    --  -78.25 121.00 -35.80   52
 25  ω   -103.00 -77.00   0.50    1.42    --  -78.25 140.00 147.91   52
 26  ω   -112.00 -86.00   0.50    1.42    --  -78.25 135.00-151.69   52
 27  ω    -92.00 -66.00   0.50    1.42    --  -78.25 115.00 168.52   52
 28  ω    -74.00 -48.00   0.50    1.42    --  -78.25 125.00 -90.85   52
 29  ω   -112.00 -81.00   0.50    1.42    --  -78.25 135.00-177.57   62
 30  ω    -67.00 -40.00   0.50    1.42    --  -78.25 135.00-177.57   54
 31  ω   -103.00 -58.00   0.50    1.42    --  -78.25 122.00 136.84   90
 32  ω   -112.00 -87.00   0.50    1.42    --  -78.25 -33.00 -26.81   50
 33  ω   -102.00 -74.00   0.50    1.42    --  -78.25 120.00  61.17   56
 34  ω    -66.00 -38.00   0.50    1.42    --  -78.25 110.00-144.96   56
 35  ω   -113.00 -62.00   0.50    1.42    --  -78.25 137.00 -75.36  102
 36  ω    -89.00 -41.00   0.50    1.42    --  -78.25 118.00-137.77   96
 37  ω   -100.00 -51.00   0.50    1.42    --  -78.25 116.00  55.86   98
 38  ω   -108.00 -82.00   0.50    1.42    --  -78.25 131.00  67.58   52
 39  ω   -104.00 -59.00   0.50    1.42    --  -78.25 123.00 104.06   90
 40  ω   -105.00 -80.00   0.50    1.42    --  -78.25 125.00 -90.85   50
 41  ω    -80.00 -45.00   0.50    1.42    --  -78.25-172.00 -55.85   70
 42  ω     59.00 125.00   0.50    1.42    --   79.75  19.00-151.64  132
 43  ω     40.00  68.00   0.50    1.42    --   79.75 -64.00  -4.88   56
 44  ω     58.00 101.00   0.50    1.42    --   79.75  20.00  -0.26   86
 45  ω     91.00 123.00   0.50    1.42    --   79.75  21.00  78.60   64
 46  ω     65.00 101.00   0.50    1.42    --   79.75  22.00  51.17   72
 47  ω     65.00 111.00   0.50    1.42    --   79.75  22.00 136.70   92
 48  ω     40.00  70.00   0.50    1.42    --   79.75  -4.00 -52.45   60
 49  ω     44.00 110.00   0.50    1.42    --   79.75   0.00 162.79  132
 50  ω     56.00  86.00   0.50    1.42    --   79.75-111.00 -43.15   60
 51  ω     47.00  83.00   0.50    1.42    --   79.75  -4.00-129.61   72
 52  ω     71.00 109.00   0.50    1.42    --   79.75-128.00  76.96   76
 53  ω     43.00  68.00   0.50    1.42    --   79.75-128.00  76.96   50
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy R, DW system, HyPix-Arc 150'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0545368000
_diffrn_orient_matrix_UB_12      0.0803719000
_diffrn_orient_matrix_UB_13      -0.0478477000
_diffrn_orient_matrix_UB_21      0.0533296000
_diffrn_orient_matrix_UB_22      0.0097412000
_diffrn_orient_matrix_UB_23      -0.0367604000
_diffrn_orient_matrix_UB_31      -0.0416706000
_diffrn_orient_matrix_UB_32      -0.0926615000
_diffrn_orient_matrix_UB_33      -0.0453337000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'Rotating-anode X-ray tube'
_diffrn_source_type              'Rigaku (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                4366
_reflns_number_total             5007
_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 1.171.43.36a (Rigaku OD, 2022)'
_computing_data_collection       
'CrysAlisPro system (CCD 42.92a 64-bit (release 29-05-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.36a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_refine_diff_density_max         0.955
_refine_diff_density_min         -0.336
_refine_diff_density_rms         0.068
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5007
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0471
_refine_ls_R_factor_gt           0.0411
_refine_ls_restrained_S_all      1.041
_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)+(0.0734P)²+4.2853P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1128
_refine_ls_wR_factor_ref         0.1174
_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:
 C8(H8A,H8B,H8C), C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C6(H6A,H6B,H6C),
 C18(H18A,H18B,H18C), C16(H16A,H16B,H16C), C7(H7A,H7B,H7C), C11(H11A,H11B,H11C),
  C10(H10A,H10B,H10C), C19(H19A,H19B,H19C), C20(H20A,H20B,H20C), C12(H12A,H12B,
 H12C)
;
_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 0.76794(3) 0.40955(4) 0.62345(3) 0.03021(14) Uani 1 1 d . . . . .
P2 P 0.69482(3) 0.30020(4) 0.55026(3) 0.03232(14) Uani 1 1 d . . . . .
P6 P 0.69721(3) 0.55762(4) 0.60155(3) 0.03465(15) Uani 1 1 d . . . . .
P3 P 0.68697(3) 0.41398(5) 0.47168(3) 0.03317(15) Uani 1 1 d . . . . .
P4 P 0.58353(3) 0.37269(5) 0.54082(3) 0.03574(15) Uani 1 1 d . . . . .
P5 P 0.61426(3) 0.52195(5) 0.50427(3) 0.04030(16) Uani 1 1 d . . . . .
C1 C 0.82307(11) 0.44670(16) 0.57283(10) 0.0291(4) Uani 1 1 d . . . . .
C2 C 0.78189(11) 0.47609(15) 0.50968(10) 0.0275(4) Uani 1 1 d . . . . .
C13 C 0.57732(12) 0.33080(17) 0.66511(11) 0.0334(4) Uani 1 1 d . . . . .
C5 C 0.79954(13) 0.55481(17) 0.46337(11) 0.0341(5) Uani 1 1 d . . . . .
C3 C 0.60076(11) 0.41623(17) 0.62526(10) 0.0305(4) Uani 1 1 d . . . . .
C4 C 0.63343(12) 0.51440(17) 0.64282(11) 0.0328(4) Uani 1 1 d . . . . .
C8 C 0.83581(14) 0.49901(19) 0.42110(12) 0.0397(5) Uani 1 1 d . . . . .
H8A H 0.885433 0.471139 0.449281 0.060 Uiso 1 1 calc R U . . .
H8B H 0.841647 0.550339 0.389967 0.060 Uiso 1 1 calc R U . . .
H8C H 0.803499 0.439927 0.397043 0.060 Uiso 1 1 calc R U . . .
C17 C 0.63288(14) 0.59684(18) 0.69491(11) 0.0375(5) Uani 1 1 d . . . . .
C14 C 0.49486(13) 0.3422(2) 0.65720(12) 0.0411(5) Uani 1 1 d . . . . .
H14A H 0.487177 0.412760 0.672755 0.062 Uiso 1 1 calc R U . . .
H14B H 0.482846 0.286718 0.682896 0.062 Uiso 1 1 calc R U . . .
H14C H 0.461809 0.334314 0.610908 0.062 Uiso 1 1 calc R U . . .
C9 C 0.90898(12) 0.44631(19) 0.61434(11) 0.0381(5) Uani 1 1 d . . . . .
C15 C 0.58606(15) 0.21870(19) 0.64026(14) 0.0460(6) Uani 1 1 d . . . . .
H15A H 0.550138 0.210283 0.594890 0.069 Uiso 1 1 calc R U . . .
H15B H 0.576009 0.164512 0.667798 0.069 Uiso 1 1 calc R U . . .
H15C H 0.637586 0.209966 0.642271 0.069 Uiso 1 1 calc R U . . .
C6 C 0.72453(15) 0.6036(2) 0.41532(13) 0.0472(6) Uani 1 1 d . . . . .
H6A H 0.692954 0.547140 0.387412 0.071 Uiso 1 1 calc R U . . .
H6B H 0.735288 0.657451 0.387961 0.071 Uiso 1 1 calc R U . . .
H6C H 0.697883 0.637244 0.440184 0.071 Uiso 1 1 calc R U . . .
C18 C 0.56632(17) 0.5866(2) 0.71618(14) 0.0500(6) Uani 1 1 d . . . . .
H18A H 0.518935 0.588885 0.677497 0.075 Uiso 1 1 calc R U . . .
H18B H 0.567505 0.645817 0.745533 0.075 Uiso 1 1 calc R U . . .
H18C H 0.569884 0.518649 0.739141 0.075 Uiso 1 1 calc R U . . .
C16 C 0.63125(14) 0.3309(2) 0.73761(12) 0.0431(5) Uani 1 1 d . . . . .
H16A H 0.683329 0.323291 0.740856 0.065 Uiso 1 1 calc R U . . .
H16B H 0.618756 0.271143 0.760209 0.065 Uiso 1 1 calc R U . . .
H16C H 0.626020 0.398306 0.757966 0.065 Uiso 1 1 calc R U . . .
C7 C 0.84641(17) 0.65042(18) 0.50107(13) 0.0466(6) Uani 1 1 d . . . . .
H7A H 0.821555 0.683233 0.527635 0.070 Uiso 1 1 calc R U . . .
H7B H 0.850713 0.703088 0.469952 0.070 Uiso 1 1 calc R U . . .
H7C H 0.896872 0.625930 0.529671 0.070 Uiso 1 1 calc R U . . .
C11 C 0.92769(14) 0.3429(2) 0.65605(14) 0.0515(7) Uani 1 1 d . . . . .
H11A H 0.902036 0.344333 0.686637 0.077 Uiso 1 1 calc R U . . .
H11B H 0.982329 0.338199 0.680700 0.077 Uiso 1 1 calc R U . . .
H11C H 0.910549 0.280652 0.627200 0.077 Uiso 1 1 calc R U . . .
C10 C 0.95919(13) 0.4407(2) 0.57501(14) 0.0483(6) Uani 1 1 d . . . . .
H10A H 0.944439 0.379095 0.545420 0.072 Uiso 1 1 calc R U . . .
H10B H 1.012030 0.433060 0.605070 0.072 Uiso 1 1 calc R U . . .
H10C H 0.953250 0.506319 0.549354 0.072 Uiso 1 1 calc R U . . .
C19 C 0.62491(19) 0.70934(19) 0.66461(15) 0.0553(7) Uani 1 1 d . . . . .
H19A H 0.670681 0.726931 0.657222 0.083 Uiso 1 1 calc R U . . .
H19B H 0.617708 0.761763 0.694556 0.083 Uiso 1 1 calc R U . . .
H19C H 0.581266 0.710844 0.622794 0.083 Uiso 1 1 calc R U . . .
C20 C 0.70762(17) 0.5929(2) 0.75444(13) 0.0528(7) Uani 1 1 d . . . . .
H20A H 0.712927 0.523116 0.775851 0.079 Uiso 1 1 calc R U . . .
H20B H 0.708317 0.649290 0.785354 0.079 Uiso 1 1 calc R U . . .
H20C H 0.749502 0.603687 0.740256 0.079 Uiso 1 1 calc R U . . .
C12 C 0.92949(16) 0.5427(2) 0.66115(13) 0.0540(7) Uani 1 1 d . . . . .
H12A H 0.919733 0.608992 0.635646 0.081 Uiso 1 1 calc R U . . .
H12B H 0.983039 0.539103 0.689990 0.081 Uiso 1 1 calc R U . . .
H12C H 0.898763 0.541446 0.687626 0.081 Uiso 1 1 calc R U . . .


_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 P2 2.1709(8) . ?
P1 P6 2.2380(8) . ?
P1 C1 1.875(2) . ?
P2 P3 2.2082(8) . ?
P2 P4 2.2571(8) . ?
P6 P5 2.1736(9) . ?
P6 C4 1.870(2) . ?
P3 P5 2.2540(8) . ?
P3 C2 1.858(2) . ?
P4 P5 2.2054(9) . ?
P4 C3 1.851(2) . ?
C1 C2 1.364(3) . ?
C1 C9 1.548(3) . ?
C2 C5 1.551(3) . ?
C13 C3 1.560(3) . ?
C13 C14 1.532(3) . ?
C13 C15 1.540(3) . ?
C13 C16 1.538(3) . ?
C5 C8 1.535(3) . ?
C5 C6 1.548(3) . ?
C5 C7 1.536(3) . ?
C3 C4 1.366(3) . ?
C4 C17 1.551(3) . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C17 C18 1.530(3) . ?
C17 C19 1.542(3) . ?
C17 C20 1.529(4) . ?
C14 H14A 0.9800 . ?
C14 H14B 0.9800 . ?
C14 H14C 0.9800 . ?
C9 C11 1.550(3) . ?
C9 C10 1.531(3) . ?
C9 C12 1.540(4) . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C7 H7A 0.9800 . ?
C7 H7B 0.9800 . ?
C7 H7C 0.9800 . ?
C11 H11A 0.9800 . ?
C11 H11B 0.9800 . ?
C11 H11C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
C20 H20A 0.9800 . ?
C20 H20B 0.9800 . ?
C20 H20C 0.9800 . ?
C12 H12A 0.9800 . ?
C12 H12B 0.9800 . ?
C12 H12C 0.9800 . ?

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 P1 P6 101.35(3) . . ?
C1 P1 P2 93.58(7) . . ?
C1 P1 P6 95.82(7) . . ?
P1 P2 P3 90.50(3) . . ?
P1 P2 P4 97.60(3) . . ?
P3 P2 P4 83.93(3) . . ?
P5 P6 P1 101.29(3) . . ?
C4 P6 P1 96.46(7) . . ?
C4 P6 P5 93.26(7) . . ?
P2 P3 P5 89.78(3) . . ?
C2 P3 P2 99.04(7) . . ?
C2 P3 P5 103.05(6) . . ?
P5 P4 P2 89.77(3) . . ?
C3 P4 P2 103.42(7) . . ?
C3 P4 P5 98.78(7) . . ?
P6 P5 P3 97.62(3) . . ?
P6 P5 P4 90.47(3) . . ?
P4 P5 P3 84.07(3) . . ?
C2 C1 P1 116.22(15) . . ?
C2 C1 C9 132.23(19) . . ?
C9 C1 P1 111.33(14) . . ?
C1 C2 P3 115.47(15) . . ?
C1 C2 C5 131.33(19) . . ?
C5 C2 P3 113.18(15) . . ?
C14 C13 C3 112.58(18) . . ?
C14 C13 C15 107.14(19) . . ?
C14 C13 C16 111.64(18) . . ?
C15 C13 C3 109.11(17) . . ?
C16 C13 C3 111.39(18) . . ?
C16 C13 C15 104.55(19) . . ?
C8 C5 C2 112.40(17) . . ?
C8 C5 C6 106.40(19) . . ?
C8 C5 C7 112.1(2) . . ?
C6 C5 C2 108.76(18) . . ?
C7 C5 C2 111.58(18) . . ?
C7 C5 C6 105.1(2) . . ?
C13 C3 P4 113.07(15) . . ?
C4 C3 P4 115.81(16) . . ?
C4 C3 C13 131.09(19) . . ?
C3 C4 P6 115.92(15) . . ?
C3 C4 C17 132.50(19) . . ?
C17 C4 P6 111.43(15) . . ?
C5 C8 H8A 109.5 . . ?
C5 C8 H8B 109.5 . . ?
C5 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C18 C17 C4 114.9(2) . . ?
C18 C17 C19 104.8(2) . . ?
C19 C17 C4 108.19(19) . . ?
C20 C17 C4 110.19(19) . . ?
C20 C17 C18 110.5(2) . . ?
C20 C17 C19 107.9(2) . . ?
C13 C14 H14A 109.5 . . ?
C13 C14 H14B 109.5 . . ?
C13 C14 H14C 109.5 . . ?
H14A C14 H14B 109.5 . . ?
H14A C14 H14C 109.5 . . ?
H14B C14 H14C 109.5 . . ?
C1 C9 C11 107.75(18) . . ?
C10 C9 C1 115.10(19) . . ?
C10 C9 C11 104.4(2) . . ?
C10 C9 C12 111.4(2) . . ?
C12 C9 C1 109.5(2) . . ?
C12 C9 C11 108.3(2) . . ?
C13 C15 H15A 109.5 . . ?
C13 C15 H15B 109.5 . . ?
C13 C15 H15C 109.5 . . ?
H15A C15 H15B 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C5 C6 H6A 109.5 . . ?
C5 C6 H6B 109.5 . . ?
C5 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18B 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C13 C16 H16A 109.5 . . ?
C13 C16 H16B 109.5 . . ?
C13 C16 H16C 109.5 . . ?
H16A C16 H16B 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C5 C7 H7A 109.5 . . ?
C5 C7 H7B 109.5 . . ?
C5 C7 H7C 109.5 . . ?
H7A C7 H7B 109.5 . . ?
H7A C7 H7C 109.5 . . ?
H7B C7 H7C 109.5 . . ?
C9 C11 H11A 109.5 . . ?
C9 C11 H11B 109.5 . . ?
C9 C11 H11C 109.5 . . ?
H11A C11 H11B 109.5 . . ?
H11A C11 H11C 109.5 . . ?
H11B C11 H11C 109.5 . . ?
C9 C10 H10A 109.5 . . ?
C9 C10 H10B 109.5 . . ?
C9 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19B 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
C17 C20 H20A 109.5 . . ?
C17 C20 H20B 109.5 . . ?
C17 C20 H20C 109.5 . . ?
H20A C20 H20B 109.5 . . ?
H20A C20 H20C 109.5 . . ?
H20B C20 H20C 109.5 . . ?
C9 C12 H12A 109.5 . . ?
C9 C12 H12B 109.5 . . ?
C9 C12 H12C 109.5 . . ?
H12A C12 H12B 109.5 . . ?
H12A C12 H12C 109.5 . . ?
H12B C12 H12C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
P1 P6 C4 C3 -51.31(17) . . . . ?
P1 P6 C4 C17 124.75(15) . . . . ?
P1 C1 C2 P3 -29.4(2) . . . . ?
P1 C1 C2 C5 149.37(18) . . . . ?
P1 C1 C9 C11 45.7(2) . . . . ?
P1 C1 C9 C10 161.66(18) . . . . ?
P1 C1 C9 C12 -71.9(2) . . . . ?
P2 P1 C1 C2 50.12(15) . . . . ?
P2 P1 C1 C9 -134.56(14) . . . . ?
P2 P3 C2 C1 -6.96(16) . . . . ?
P2 P3 C2 C5 174.08(12) . . . . ?
P2 P4 C3 C13 -93.31(14) . . . . ?
P2 P4 C3 C4 84.73(16) . . . . ?
P6 P1 C1 C2 -51.69(16) . . . . ?
P6 P1 C1 C9 123.63(14) . . . . ?
P6 C4 C17 C18 162.43(18) . . . . ?
P6 C4 C17 C19 45.7(2) . . . . ?
P6 C4 C17 C20 -72.0(2) . . . . ?
P3 C2 C5 C8 -88.7(2) . . . . ?
P3 C2 C5 C6 28.8(2) . . . . ?
P3 C2 C5 C7 144.29(17) . . . . ?
P4 C3 C4 P6 -29.6(2) . . . . ?
P4 C3 C4 C17 155.4(2) . . . . ?
P5 P6 C4 C3 50.45(17) . . . . ?
P5 P6 C4 C17 -133.49(15) . . . . ?
P5 P3 C2 C1 84.92(15) . . . . ?
P5 P3 C2 C5 -94.04(13) . . . . ?
P5 P4 C3 C13 174.82(13) . . . . ?
P5 P4 C3 C4 -7.15(17) . . . . ?
C1 C2 C5 C8 92.5(3) . . . . ?
C1 C2 C5 C6 -149.9(2) . . . . ?
C1 C2 C5 C7 -34.5(3) . . . . ?
C2 C1 C9 C11 -140.0(2) . . . . ?
C2 C1 C9 C10 -24.0(3) . . . . ?
C2 C1 C9 C12 102.4(3) . . . . ?
C13 C3 C4 P6 148.01(18) . . . . ?
C13 C3 C4 C17 -27.0(4) . . . . ?
C3 C4 C17 C18 -22.4(4) . . . . ?
C3 C4 C17 C19 -139.1(3) . . . . ?
C3 C4 C17 C20 103.2(3) . . . . ?
C14 C13 C3 P4 -89.23(19) . . . . ?
C14 C13 C3 C4 93.1(3) . . . . ?
C9 C1 C2 P3 156.54(19) . . . . ?
C9 C1 C2 C5 -24.7(4) . . . . ?
C15 C13 C3 P4 29.6(2) . . . . ?
C15 C13 C3 C4 -148.1(2) . . . . ?
C16 C13 C3 P4 144.48(16) . . . . ?
C16 C13 C3 C4 -33.2(3) . . . . ?

_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 1.239
_oxdiff_exptl_absorpt_empirical_full_min 0.756
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-pentane'
####################################################################### 
# 
# 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_mu025_tp
_database_code_depnum_ccdc_archive 'CCDC 2346027'
loop_
_audit_author_name
_audit_author_address
'Maria Uttendorfer'
;University of Regensburg
Germany
;
_audit_update_record             
;
2024-04-05 deposited with the CCDC.	2024-05-08 downloaded from the CCDC.
;
_audit_creation_date             2024-04-04
_audit_creation_method           
;
Olex2 1.5-alpha
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_shelx_SHELXL_version_number     2016/6
_chemical_name_common            ?
_chemical_name_systematic        '[K([18]crown-6)][1,2,3-P3C2tBu2]'
_chemical_formula_moiety         'C22 H42 K O6 P3'
_chemical_formula_sum            'C22 H42 K O6 P3'
_chemical_formula_weight         534.56
_chemical_absolute_configuration ?
_chemical_melting_point          ?
_chemical_oxdiff_formula         C22H42KO6P3
_chemical_oxdiff_usercomment     'crystals from toluene nhex'
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'
K K 0.3868 1.0657 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 '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      orthorhombic
_space_group_IT_number           19
_space_group_name_H-M_alt        'P 21 21 21'
_space_group_name_Hall           'P 2ac 2ab'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, -y, z+1/2'
'-x, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z'

_cell_length_a                   9.58810(10)
_cell_length_b                   17.15960(10)
_cell_length_c                   17.26040(10)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     2839.82(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    42511
_cell_measurement_temperature    123.01(10)
_cell_measurement_theta_max      66.7810
_cell_measurement_theta_min      4.5500
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_exptl_absorpt_coefficient_mu    3.503
_exptl_absorpt_correction_T_max  0.835
_exptl_absorpt_correction_T_min  0.275
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.41.91a (Rigaku Oxford Diffraction, 2020)
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 light yellow'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.250
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             1144
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-1 2 2 0.1412
-4 9 -2 0.1273
-2 7 -8 0.1281
3 -8 5 0.1418
4 -8 -4 0.1323
5 6 3 0.1352
-4 -2 9 0.1794
2 4 9 0.2370
-5 -5 3 0.1634
-1 -3 -10 0.1650
5 3 -7 0.1239
5 5 0 0.1159
6 2 1 0.1239
5 1 -6 0.1209
6 2 -3 0.1122
-6 -2 1 0.1749
6 -3 0 0.1286
-6 3 0 0.1599
-5 3 -5 0.1571
-3 2 -10 0.1599
5 -5 3 0.1368
5 -5 0 0.1267
-5 5 5 0.1567
0 -2 11 0.2344
4 -9 2 0.1255
2 -10 -2 0.1400
2 -10 2 0.1469
-2 10 1 0.1406
-2 10 -4 0.1281
0 11 -1 0.1277
0 -11 0 0.1524
-1 -8 8 0.1711
0 -10 5 0.1627
1 -8 -8 0.1575
1 9 -7 0.1180
1 4 -10 0.1428
0 11 1 0.1360
0 11 -3 0.1278
2 11 0 0.1292
2 9 -5 0.1148
2 7 -8 0.1196
-1 -9 -6 0.1744
-2 -10 3 0.1595
-2 -8 6 0.1725
4 9 0 0.1188
4 8 -4 0.1130

_exptl_crystal_size_max          0.419
_exptl_crystal_size_mid          0.287
_exptl_crystal_size_min          0.253
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
-0.9975 1.9948 2.0043 0.0844 -0.1844 -0.2207
-3.7801 8.5735 -2.2105 0.3341 -0.9425 0.0090
-2.4134 6.8811 -7.6721 0.2808 -0.7924 0.5416
3.1444 -7.9440 5.4520 -0.3168 0.8940 -0.3167
3.9811 -7.6291 -3.9011 -0.2847 0.8030 0.5236
5.1594 5.6736 2.5753 0.8770 0.4765 -0.0613
-3.7285 -2.1092 8.7212 -0.4119 -0.2236 -0.8834
2.4210 4.2052 9.4092 0.5835 0.3172 -0.7476
-5.3876 -4.9211 2.6445 -0.8040 -0.4368 -0.4036
-1.3374 -3.3056 -10.4209 -0.4318 -0.2348 0.8708
4.5162 3.2254 -6.9993 0.5737 0.3115 0.7575
5.4329 5.4299 -0.1822 0.8628 0.4688 0.1892
6.0300 2.3490 1.4441 0.6856 0.7229 0.0857
5.1761 1.2548 -6.0957 0.4823 0.5083 0.7135
5.8851 1.8184 -3.1575 0.6030 0.6357 0.4820
-6.0847 -2.1139 1.0128 -0.6561 -0.6917 -0.3019
6.0169 -2.8468 0.0703 0.2761 0.9331 0.2304
-6.0170 2.8466 -0.0231 -0.2759 -0.9322 -0.2345
-5.3146 2.5476 -5.2382 -0.2750 -0.9297 0.2452
-3.1227 1.5384 -9.5684 -0.2006 -0.6785 0.7067
5.2263 -5.4706 2.5987 0.0259 0.9997 -0.0049
5.4232 -5.4643 -0.0683 0.0252 0.9720 0.2336
-4.9451 4.6046 4.9798 -0.0201 -0.7701 -0.6376
-0.0192 -1.6328 11.0857 -0.0550 0.2954 -0.9538
3.7618 -8.5645 2.3432 -0.3340 0.9423 -0.0213
2.4945 -9.9949 -2.0575 -0.5768 0.7513 0.3207
2.0244 -10.2620 2.3966 -0.6070 0.7905 -0.0815
-2.4283 10.1927 1.1269 0.5914 -0.7703 -0.2386
-1.7056 9.8381 -4.2732 0.5884 -0.7663 0.2582
-0.1990 11.0365 -1.4780 0.8225 -0.5649 0.0654
0.4124 -11.1122 -0.1474 -0.8214 0.5642 0.0838
-0.7061 -8.0541 7.6441 -0.6275 0.4309 -0.6485
-0.2687 -10.0507 4.8161 -0.7635 0.5243 -0.3771
1.2734 -7.7507 -7.7046 -0.5413 0.3720 0.7540
0.5264 9.0159 -6.5212 0.6940 -0.4766 0.5397
1.1639 4.2676 -10.1410 0.3578 -0.2456 0.9009
-0.4838 11.0811 0.7060 0.8168 -0.5610 -0.1347
-0.0241 10.7974 -2.7617 0.8102 -0.5564 0.1844
1.8810 10.6123 0.2910 0.9724 -0.2331 -0.0091
2.3462 9.0628 -4.9693 0.8573 -0.2055 0.4720
2.3439 6.8710 -7.7525 0.6705 -0.1606 0.7243
-0.7878 -9.1807 -6.1716 -0.8107 0.1945 0.5522
-2.1954 -10.1064 2.5720 -0.9407 0.2255 -0.2534
-2.3747 -8.2257 6.2389 -0.7870 0.1886 -0.5874
3.9732 8.5707 -0.1763 0.9844 0.1299 0.1190
4.0670 7.5197 -3.8448 0.8874 0.1172 0.4458

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_diffrn_reflns_av_R_equivalents  0.0493
_diffrn_reflns_av_unetI/netI     0.0178
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            53964
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        66.826
_diffrn_reflns_theta_max         66.826
_diffrn_reflns_theta_min         3.632
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      123.01(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 4.2047
_diffrn_detector_type            TitanS2
_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    -88.00 -63.00   1.00    2.00    --  -43.66 127.00   7.00   25
  2  ω    -96.00 -71.00   1.00    2.00    --  -43.66 143.00 176.00   25
  3  ω     48.00  75.00   1.00    2.00    --   43.66-143.00 121.00   27
  4  ω     28.00  55.00   1.00    2.00    --   43.66-127.00 -68.00   27
  5  ω     67.00  92.00   1.00    2.00    --   43.66 143.00 176.00   25
  6  ω     92.00 117.00   1.00    8.00    --   86.50 127.00   7.00   25
  7  ω     33.00  58.00   1.00    8.00    --   86.50-143.00 121.00   25
  8  ω     26.00  51.00   1.00    8.00    --   86.50-127.00 -68.00   25
  9  ω   -154.00-129.00   1.00    8.00    --  -90.00-127.00 -68.00   25
 10  ω   -149.00-124.00   1.00    8.00    --  -90.00-143.00 121.00   25
 11  ω   -105.00 -80.00   1.00    8.00    --  -90.00 143.00 176.00   25
 12  ω    -97.00 -71.00   1.00    8.00    --  -90.00 127.00   7.00   26
 13  ω    -77.00 -49.00   1.00    2.00    --  -43.66 125.00-180.00   28
 14  ω    -94.00 -43.00   1.00    2.00    --  -43.66 125.00-120.00   51
 15  ω     18.00 113.00   1.00    2.00    --   43.66  57.00  60.00   95
 16  ω     20.00 112.00   1.00    2.00    --   43.66  57.00-180.00   92
 17  ω     44.00 113.00   1.00    2.00    --   43.66  57.00 -60.00   69
 18  ω   -153.00-114.00   1.00    8.00    --  -90.00 -61.00-180.00   39
 19  ω    -59.00 -29.00   1.00    8.00    --  -90.00  77.00   0.00   30
 20  ω    -61.00 -36.00   1.00    8.00    --  -90.00 125.00 -30.00   25
 21  ω    -46.00 -19.00   1.00    8.00    --  -90.00 109.00-123.93   27
 22  ω    -69.00 -44.00   1.00    8.00    --  -90.00 125.00 120.00   25
 23  ω    -48.00 -21.00   1.00    8.00    --  -90.00  77.00  30.00   27
 24  ω   -153.00-107.00   1.00    8.00    --  -90.00 -77.00  60.00   46
 25  ω   -163.00-119.00   1.00    8.00    --  -90.00 -94.00  90.00   44
 26  ω    -75.00 -47.00   1.00    8.00    --  -90.00  97.00  92.22   28
 27  ω   -112.00 -70.00   1.00    8.00    --  -90.00 125.00 -30.00   42
 28  ω   -110.00 -72.00   1.00    8.00    --  -90.00 125.00 120.00   38
 29  ω   -158.00-131.00   1.00    8.00    --  -90.00-125.00 -60.00   27
 30  ω    -98.00 -67.00   1.00    8.00    --  -90.00 -51.00  -5.69   31
 31  ω   -167.00-117.00   1.00    8.00    --  -90.00 -15.00 -60.00   50
 32  ω   -108.00 -60.00   1.00    8.00    --  -90.00 109.00-123.93   48
 33  ω   -161.00-106.00   1.00    8.00    --  -90.00-125.00   0.00   55
 34  ω   -100.00 -73.00   1.00    8.00    --  -90.00  77.00  30.00   27
 35  ω   -106.00 -69.00   1.00    8.00    --  -90.00 125.00-120.00   37
 36  ω    -95.00 -16.00   1.00    8.00    --  -90.00  77.00-120.00   79
 37  ω    -96.00 -71.00   1.00    8.00    --  -90.00 125.00  30.00   25
 38  ω   -111.00 -56.00   1.00    8.00    --  -90.00 125.00  60.00   55
 39  ω   -161.00-117.00   1.00    8.00    --  -90.00 -15.00 150.00   44
 40  ω    -76.00 -51.00   1.00    8.00    --  -90.00 -15.00 150.00   25
 41  ω    -74.00 -21.00   1.00    8.00    --  -90.00  45.00-150.00   53
 42  ω   -105.00 -74.00   1.00    8.00    --  -90.00  30.00  60.00   31
 43  ω   -113.00 -25.00   1.00    8.00    --  -90.00  45.00  90.00   88
 44  ω    -92.00 -64.00   1.00    8.00    --  -90.00 113.00   4.30   28
 45  ω   -107.00 -67.00   1.00    8.00    --  -90.00  45.00 -30.00   40
 46  ω   -158.00-133.00   1.00    8.00    --  -90.00-125.00 -30.00   25
 47  ω   -121.00 -93.00   1.00    8.00    --  -90.00 -61.00 -30.00   28
 48  ω   -157.00-115.00   1.00    8.00    --  -90.00 -61.00 120.00   42
 49  ω    -98.00 -71.00   1.00    8.00    --  -90.00 -61.00 120.00   27
 50  ω   -128.00 -66.00   1.00    8.00    --  -90.00  15.00-180.00   62
 51  ω    -49.00 -22.00   1.00    8.00    --  -90.00  30.00  60.00   27
 52  ω   -163.00-138.00   1.00    8.00    --  -90.00 -77.00 -30.00   25
 53  ω   -134.00-109.00   1.00    8.00    --  -90.00-125.00-180.00   25
 54  ω   -133.00-108.00   1.00    8.00    --  -90.00-125.00-150.00   25
 55  ω   -127.00 -54.00   1.00    8.00    --  -90.00 145.00-129.06   73
 56  ω    -99.00 -64.00   1.00    8.00    --  -90.00 -61.00-180.00   35
 57  ω    -94.00 -46.00   1.00    8.00    --  -90.00 125.00  90.00   48
 58  ω    -84.00 -59.00   1.00    8.00    --  -90.00 125.00-180.00   25
 59  ω    -54.00 -27.00   1.00    8.00    --  -90.00  61.00-150.00   27
 60  ω    -94.00 -66.00   1.00    8.00    --  -90.00 125.00 -60.00   28
 61  ω    -53.00 -28.00   1.00    8.00    --  -90.00 125.00 -60.00   25
 62  ω   -110.00 -83.00   1.00    8.00    --  -90.00 116.00  65.02   27
 63  ω   -106.00 -81.00   1.00    8.00    --  -90.00  50.00 115.08   25
 64  ω    -94.00 -69.00   1.00    8.00    --  -90.00  39.00-118.09   25
 65  ω    -75.00 -48.00   1.00    8.00    --  -90.00  39.00  18.24   27
 66  ω    -87.00 -60.00   1.00    8.00    --  -90.00  61.00-120.00   27
 67  ω    -63.00 -28.00   1.00    8.00    --  -90.00  30.00 150.00   35
 68  ω    -81.00 -56.00   1.00    8.00    --  -90.00  77.00 -90.00   25
 69  ω   -106.00 -81.00   1.00    8.00    --  -90.00  82.00 149.49   25
 70  ω   -162.00-126.00   1.00    8.00    --  -90.00 -15.00 -30.00   36
 71  ω    -67.00 -22.00   1.00    8.00    --  -90.00   0.00 -30.00   45
 72  ω   -145.00-104.00   1.00    8.00    --  -90.00 -77.00-150.00   41
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dualflex, TitanS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0821941000
_diffrn_orient_matrix_UB_12      0.0768822000
_diffrn_orient_matrix_UB_13      0.0065037000
_diffrn_orient_matrix_UB_21      0.1330327000
_diffrn_orient_matrix_UB_22      -0.0461002000
_diffrn_orient_matrix_UB_23      0.0200830000
_diffrn_orient_matrix_UB_31      0.0369319000
_diffrn_orient_matrix_UB_32      -0.0050215000
_diffrn_orient_matrix_UB_33      -0.0867146000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_reflns_Friedel_coverage         0.763
_reflns_Friedel_fraction_full    0.996
_reflns_Friedel_fraction_max     0.996
_reflns_number_gt                4990
_reflns_number_total             5040
_reflns_odcompleteness_completeness 98.33
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     67.46
_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 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_collection       'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_data_reduction        'CrysAlisPro 1.171.41.91a (Rigaku OD, 2020)'
_computing_molecular_graphics    'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5-alpha (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2016/6 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_refine_diff_density_max         0.315
_refine_diff_density_min         -0.130
_refine_diff_density_rms         0.037
_refine_ls_abs_structure_details 
;
 Flack x determined using 2132 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.001(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.069
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     295
_refine_ls_number_reflns         5040
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0238
_refine_ls_R_factor_gt           0.0236
_refine_ls_restrained_S_all      1.069
_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)+(0.0409P)²+0.4491P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0632
_refine_ls_wR_factor_ref         0.0634
_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:
 C14(H14A,H14B), C18(H18A,H18B), C17(H17A,H17B), C15(H15A,H15B), C22(H22A,
 H22B), C11(H11A,H11B), C19(H19A,H19B), C16(H16A,H16B), C12(H12A,H12B),
 C20(H20A,H20B), C21(H21A,H21B), C13(H13A,H13B)
2.b Idealised Me refined as rotating group:
 C8(H8A,H8B,H8C), C6(H6A,H6B,H6C), C9(H9A,H9B,H9C), C4(H4A,H4B,H4C), C10(H10A,
 H10B,H10C), C5(H5A,H5B,H5C)
;
_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
K1 K 0.42055(5) 0.65134(3) 0.70757(2) 0.02695(12) Uani 1 1 d . . . . .
P1 P 0.25467(6) 0.55694(3) 0.55532(3) 0.02467(13) Uani 1 1 d . . . . .
P2 P 0.42532(6) 0.59944(3) 0.49434(3) 0.02801(13) Uani 1 1 d . . . . .
P3 P 0.55522(6) 0.50427(3) 0.51109(3) 0.02910(14) Uani 1 1 d . . . . .
O6 O 0.50924(17) 0.76871(10) 0.61220(9) 0.0318(4) Uani 1 1 d . . . . .
O1 O 0.24017(17) 0.78102(9) 0.67117(8) 0.0302(3) Uani 1 1 d . . . . .
O2 O 0.14666(17) 0.66743(9) 0.77652(9) 0.0300(3) Uani 1 1 d . . . . .
O3 O 0.36016(16) 0.59184(9) 0.85755(9) 0.0280(3) Uani 1 1 d . . . . .
O5 O 0.71801(17) 0.68052(10) 0.68550(9) 0.0326(4) Uani 1 1 d . . . . .
O4 O 0.62380(16) 0.56687(10) 0.78983(9) 0.0317(3) Uani 1 1 d . . . . .
C2 C 0.4507(2) 0.44012(12) 0.56768(11) 0.0240(4) Uani 1 1 d . . . . .
C14 C 0.0700(3) 0.73572(13) 0.75894(13) 0.0320(5) Uani 1 1 d . . . . .
H14A H 0.098382 0.778542 0.794006 0.038 Uiso 1 1 calc R U . . .
H14B H -0.030882 0.726040 0.766291 0.038 Uiso 1 1 calc R U . . .
C18 C 0.5964(2) 0.55143(14) 0.86932(13) 0.0315(5) Uani 1 1 d . . . . .
H18A H 0.615082 0.598574 0.900704 0.038 Uiso 1 1 calc R U . . .
H18B H 0.657697 0.508980 0.888034 0.038 Uiso 1 1 calc R U . . .
C17 C 0.4466(2) 0.52804(13) 0.87723(13) 0.0309(5) Uani 1 1 d . . . . .
H17A H 0.426468 0.483479 0.842560 0.037 Uiso 1 1 calc R U . . .
H17B H 0.427582 0.511616 0.931195 0.037 Uiso 1 1 calc R U . . .
C15 C 0.1332(2) 0.64630(14) 0.85544(12) 0.0282(5) Uani 1 1 d . . . . .
H15A H 0.033967 0.636484 0.867811 0.034 Uiso 1 1 calc R U . . .
H15B H 0.166685 0.689374 0.888771 0.034 Uiso 1 1 calc R U . . .
C7 C 0.5357(3) 0.36597(13) 0.59323(14) 0.0329(5) Uani 1 1 d . . . . .
C22 C 0.6526(3) 0.78569(15) 0.60309(13) 0.0341(5) Uani 1 1 d . . . . .
H22A H 0.683297 0.822517 0.643816 0.041 Uiso 1 1 calc R U . . .
H22B H 0.669055 0.810179 0.551961 0.041 Uiso 1 1 calc R U . . .
C11 C 0.4231(3) 0.83395(13) 0.59648(14) 0.0352(5) Uani 1 1 d . . . . .
H11A H 0.447964 0.856704 0.545615 0.042 Uiso 1 1 calc R U . . .
H11B H 0.436837 0.874329 0.636731 0.042 Uiso 1 1 calc R U . . .
C3 C 0.1935(3) 0.41675(13) 0.62774(13) 0.0297(5) Uani 1 1 d . . . . .
C19 C 0.7674(2) 0.58115(16) 0.77625(15) 0.0373(5) Uani 1 1 d . . . . .
H19A H 0.821912 0.533029 0.785498 0.045 Uiso 1 1 calc R U . . .
H19B H 0.801704 0.621986 0.812018 0.045 Uiso 1 1 calc R U . . .
C1 C 0.3131(2) 0.46376(12) 0.58695(11) 0.0234(4) Uani 1 1 d . . . . .
C16 C 0.2171(2) 0.57448(13) 0.87074(13) 0.0283(5) Uani 1 1 d . . . . .
H16A H 0.203385 0.557253 0.924945 0.034 Uiso 1 1 calc R U . . .
H16B H 0.186621 0.531944 0.835882 0.034 Uiso 1 1 calc R U . . .
C12 C 0.2740(3) 0.80802(14) 0.59582(13) 0.0338(5) Uani 1 1 d . . . . .
H12A H 0.212516 0.852035 0.581382 0.041 Uiso 1 1 calc R U . . .
H12B H 0.260961 0.765703 0.557518 0.041 Uiso 1 1 calc R U . . .
C20 C 0.7854(3) 0.60723(15) 0.69401(16) 0.0382(5) Uani 1 1 d . . . . .
H20A H 0.885762 0.612173 0.681519 0.046 Uiso 1 1 calc R U . . .
H20B H 0.743503 0.568620 0.658297 0.046 Uiso 1 1 calc R U . . .
C21 C 0.7338(3) 0.71092(14) 0.60913(12) 0.0321(5) Uani 1 1 d . . . . .
H21A H 0.698691 0.672804 0.570739 0.038 Uiso 1 1 calc R U . . .
H21B H 0.833619 0.720791 0.598224 0.038 Uiso 1 1 calc R U . . .
C8 C 0.4605(3) 0.28721(14) 0.58355(16) 0.0408(6) Uani 1 1 d . . . . .
H8A H 0.378185 0.285869 0.617210 0.061 Uiso 1 1 calc R U . . .
H8B H 0.523910 0.244793 0.597820 0.061 Uiso 1 1 calc R U . . .
H8C H 0.431437 0.280881 0.529479 0.061 Uiso 1 1 calc R U . . .
C6 C 0.2364(3) 0.38076(15) 0.70606(13) 0.0378(6) Uani 1 1 d . . . . .
H6A H 0.305541 0.339638 0.697291 0.057 Uiso 1 1 calc R U . . .
H6B H 0.154099 0.358516 0.731453 0.057 Uiso 1 1 calc R U . . .
H6C H 0.276800 0.421256 0.739215 0.057 Uiso 1 1 calc R U . . .
C9 C 0.6708(3) 0.35583(17) 0.54547(18) 0.0472(7) Uani 1 1 d . . . . .
H9A H 0.647172 0.350842 0.490452 0.071 Uiso 1 1 calc R U . . .
H9B H 0.719889 0.308843 0.562712 0.071 Uiso 1 1 calc R U . . .
H9C H 0.730952 0.401381 0.552951 0.071 Uiso 1 1 calc R U . . .
C4 C 0.0672(3) 0.46832(16) 0.64869(15) 0.0416(6) Uani 1 1 d . . . . .
H4A H 0.097557 0.510587 0.682958 0.062 Uiso 1 1 calc R U . . .
H4B H -0.003309 0.436700 0.675135 0.062 Uiso 1 1 calc R U . . .
H4C H 0.027278 0.490433 0.601283 0.062 Uiso 1 1 calc R U . . .
C10 C 0.5849(3) 0.37798(16) 0.67761(15) 0.0445(6) Uani 1 1 d . . . . .
H10A H 0.646771 0.423359 0.680183 0.067 Uiso 1 1 calc R U . . .
H10B H 0.635336 0.331542 0.695150 0.067 Uiso 1 1 calc R U . . .
H10C H 0.503753 0.386645 0.711048 0.067 Uiso 1 1 calc R U . . .
C13 C 0.0983(2) 0.75814(14) 0.67628(14) 0.0329(5) Uani 1 1 d . . . . .
H13A H 0.080219 0.713372 0.641530 0.039 Uiso 1 1 calc R U . . .
H13B H 0.036811 0.801741 0.660648 0.039 Uiso 1 1 calc R U . . .
C5 C 0.1359(3) 0.35485(15) 0.57128(14) 0.0370(5) Uani 1 1 d . . . . .
H5A H 0.094437 0.380784 0.526250 0.055 Uiso 1 1 calc R U . . .
H5B H 0.064663 0.323597 0.597599 0.055 Uiso 1 1 calc R U . . .
H5C H 0.212042 0.320857 0.554164 0.055 Uiso 1 1 calc R U . . .


_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
K1 P1 3.4727(7) . ?
K1 P2 3.7869(7) . ?
K1 O6 2.7367(16) . ?
K1 O1 2.8876(17) . ?
K1 O2 2.8964(17) . ?
K1 O3 2.8424(16) . ?
K1 O5 2.9206(17) . ?
K1 O4 2.8133(16) . ?
P1 P2 2.0777(8) . ?
P1 C1 1.780(2) . ?
P2 P3 2.0740(8) . ?
P3 C2 1.780(2) . ?
O6 C22 1.414(3) . ?
O6 C11 1.418(3) . ?
O1 C12 1.418(3) . ?
O1 C13 1.418(3) . ?
O2 C14 1.416(3) . ?
O2 C15 1.415(3) . ?
O3 C17 1.414(3) . ?
O3 C16 1.422(3) . ?
O5 C20 1.422(3) . ?
O5 C21 1.426(3) . ?
O4 C18 1.422(3) . ?
O4 C19 1.418(3) . ?
C2 C7 1.574(3) . ?
C2 C1 1.420(3) . ?
C14 H14A 0.9900 . ?
C14 H14B 0.9900 . ?
C14 C13 1.502(3) . ?
C18 H18A 0.9900 . ?
C18 H18B 0.9900 . ?
C18 C17 1.498(3) . ?
C17 H17A 0.9900 . ?
C17 H17B 0.9900 . ?
C15 H15A 0.9900 . ?
C15 H15B 0.9900 . ?
C15 C16 1.495(3) . ?
C7 C8 1.541(4) . ?
C7 C9 1.545(4) . ?
C7 C10 1.545(3) . ?
C22 H22A 0.9900 . ?
C22 H22B 0.9900 . ?
C22 C21 1.504(4) . ?
C11 H11A 0.9900 . ?
C11 H11B 0.9900 . ?
C11 C12 1.497(4) . ?
C3 C1 1.569(3) . ?
C3 C6 1.542(3) . ?
C3 C4 1.543(4) . ?
C3 C5 1.544(3) . ?
C19 H19A 0.9900 . ?
C19 H19B 0.9900 . ?
C19 C20 1.498(4) . ?
C16 H16A 0.9900 . ?
C16 H16B 0.9900 . ?
C12 H12A 0.9900 . ?
C12 H12B 0.9900 . ?
C20 H20A 0.9900 . ?
C20 H20B 0.9900 . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C8 H8A 0.9800 . ?
C8 H8B 0.9800 . ?
C8 H8C 0.9800 . ?
C6 H6A 0.9800 . ?
C6 H6B 0.9800 . ?
C6 H6C 0.9800 . ?
C9 H9A 0.9800 . ?
C9 H9B 0.9800 . ?
C9 H9C 0.9800 . ?
C4 H4A 0.9800 . ?
C4 H4B 0.9800 . ?
C4 H4C 0.9800 . ?
C10 H10A 0.9800 . ?
C10 H10B 0.9800 . ?
C10 H10C 0.9800 . ?
C13 H13A 0.9900 . ?
C13 H13B 0.9900 . ?
C5 H5A 0.9800 . ?
C5 H5B 0.9800 . ?
C5 H5C 0.9800 . ?

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 K1 P2 32.898(13) . . ?
O6 K1 P1 91.74(4) . . ?
O6 K1 P2 65.46(4) . . ?
O6 K1 O1 59.21(5) . . ?
O6 K1 O2 117.30(5) . . ?
O6 K1 O3 151.10(5) . . ?
O6 K1 O5 59.46(5) . . ?
O6 K1 O4 117.87(5) . . ?
O1 K1 P1 85.44(3) . . ?
O1 K1 P2 88.68(3) . . ?
O1 K1 O2 58.19(4) . . ?
O1 K1 O5 115.11(5) . . ?
O2 K1 P1 86.57(3) . . ?
O2 K1 P2 115.64(3) . . ?
O2 K1 O5 157.32(5) . . ?
O3 K1 P1 115.36(4) . . ?
O3 K1 P2 143.43(4) . . ?
O3 K1 O1 110.67(5) . . ?
O3 K1 O2 58.35(4) . . ?
O3 K1 O5 112.29(5) . . ?
O5 K1 P1 115.37(4) . . ?
O5 K1 P2 84.36(3) . . ?
O4 K1 P1 117.31(4) . . ?
O4 K1 P2 111.16(4) . . ?
O4 K1 O1 157.19(5) . . ?
O4 K1 O2 118.02(5) . . ?
O4 K1 O3 59.76(5) . . ?
O4 K1 O5 58.52(5) . . ?
P2 P1 K1 81.89(2) . . ?
C1 P1 K1 92.44(7) . . ?
C1 P1 P2 102.86(8) . . ?
P1 P2 K1 65.21(2) . . ?
P3 P2 K1 93.27(2) . . ?
P3 P2 P1 97.24(3) . . ?
C2 P3 P2 103.02(7) . . ?
C22 O6 K1 121.37(14) . . ?
C22 O6 C11 112.50(18) . . ?
C11 O6 K1 121.01(13) . . ?
C12 O1 K1 108.32(13) . . ?
C12 O1 C13 111.52(18) . . ?
C13 O1 K1 110.34(12) . . ?
C14 O2 K1 117.47(13) . . ?
C15 O2 K1 116.96(13) . . ?
C15 O2 C14 111.78(17) . . ?
C17 O3 K1 112.17(12) . . ?
C17 O3 C16 111.38(16) . . ?
C16 O3 K1 114.68(12) . . ?
C20 O5 K1 106.17(13) . . ?
C20 O5 C21 111.77(18) . . ?
C21 O5 K1 106.68(13) . . ?
C18 O4 K1 117.07(13) . . ?
C19 O4 K1 120.01(13) . . ?
C19 O4 C18 111.78(18) . . ?
C7 C2 P3 111.23(16) . . ?
C1 C2 P3 118.35(15) . . ?
C1 C2 C7 130.28(19) . . ?
O2 C14 H14A 109.9 . . ?
O2 C14 H14B 109.9 . . ?
O2 C14 C13 108.78(18) . . ?
H14A C14 H14B 108.3 . . ?
C13 C14 H14A 109.9 . . ?
C13 C14 H14B 109.9 . . ?
O4 C18 H18A 110.0 . . ?
O4 C18 H18B 110.0 . . ?
O4 C18 C17 108.37(18) . . ?
H18A C18 H18B 108.4 . . ?
C17 C18 H18A 110.0 . . ?
C17 C18 H18B 110.0 . . ?
O3 C17 C18 109.43(18) . . ?
O3 C17 H17A 109.8 . . ?
O3 C17 H17B 109.8 . . ?
C18 C17 H17A 109.8 . . ?
C18 C17 H17B 109.8 . . ?
H17A C17 H17B 108.2 . . ?
O2 C15 H15A 109.8 . . ?
O2 C15 H15B 109.8 . . ?
O2 C15 C16 109.41(18) . . ?
H15A C15 H15B 108.2 . . ?
C16 C15 H15A 109.8 . . ?
C16 C15 H15B 109.8 . . ?
C8 C7 C2 115.8(2) . . ?
C8 C7 C9 103.6(2) . . ?
C8 C7 C10 111.2(2) . . ?
C9 C7 C2 112.06(19) . . ?
C10 C7 C2 108.32(18) . . ?
C10 C7 C9 105.2(2) . . ?
O6 C22 H22A 110.0 . . ?
O6 C22 H22B 110.0 . . ?
O6 C22 C21 108.64(19) . . ?
H22A C22 H22B 108.3 . . ?
C21 C22 H22A 110.0 . . ?
C21 C22 H22B 110.0 . . ?
O6 C11 H11A 109.9 . . ?
O6 C11 H11B 109.9 . . ?
O6 C11 C12 108.85(18) . . ?
H11A C11 H11B 108.3 . . ?
C12 C11 H11A 109.9 . . ?
C12 C11 H11B 109.9 . . ?
C6 C3 C1 113.8(2) . . ?
C6 C3 C4 103.5(2) . . ?
C6 C3 C5 111.91(19) . . ?
C4 C3 C1 112.58(19) . . ?
C4 C3 C5 105.2(2) . . ?
C5 C3 C1 109.40(18) . . ?
O4 C19 H19A 110.0 . . ?
O4 C19 H19B 110.0 . . ?
O4 C19 C20 108.6(2) . . ?
H19A C19 H19B 108.3 . . ?
C20 C19 H19A 110.0 . . ?
C20 C19 H19B 110.0 . . ?
C2 C1 P1 118.52(16) . . ?
C2 C1 C3 129.61(19) . . ?
C3 C1 P1 111.66(15) . . ?
O3 C16 C15 108.53(17) . . ?
O3 C16 H16A 110.0 . . ?
O3 C16 H16B 110.0 . . ?
C15 C16 H16A 110.0 . . ?
C15 C16 H16B 110.0 . . ?
H16A C16 H16B 108.4 . . ?
O1 C12 C11 107.98(19) . . ?
O1 C12 H12A 110.1 . . ?
O1 C12 H12B 110.1 . . ?
C11 C12 H12A 110.1 . . ?
C11 C12 H12B 110.1 . . ?
H12A C12 H12B 108.4 . . ?
O5 C20 C19 108.1(2) . . ?
O5 C20 H20A 110.1 . . ?
O5 C20 H20B 110.1 . . ?
C19 C20 H20A 110.1 . . ?
C19 C20 H20B 110.1 . . ?
H20A C20 H20B 108.4 . . ?
O5 C21 C22 108.73(18) . . ?
O5 C21 H21A 109.9 . . ?
O5 C21 H21B 109.9 . . ?
C22 C21 H21A 109.9 . . ?
C22 C21 H21B 109.9 . . ?
H21A C21 H21B 108.3 . . ?
C7 C8 H8A 109.5 . . ?
C7 C8 H8B 109.5 . . ?
C7 C8 H8C 109.5 . . ?
H8A C8 H8B 109.5 . . ?
H8A C8 H8C 109.5 . . ?
H8B C8 H8C 109.5 . . ?
C3 C6 H6A 109.5 . . ?
C3 C6 H6B 109.5 . . ?
C3 C6 H6C 109.5 . . ?
H6A C6 H6B 109.5 . . ?
H6A C6 H6C 109.5 . . ?
H6B C6 H6C 109.5 . . ?
C7 C9 H9A 109.5 . . ?
C7 C9 H9B 109.5 . . ?
C7 C9 H9C 109.5 . . ?
H9A C9 H9B 109.5 . . ?
H9A C9 H9C 109.5 . . ?
H9B C9 H9C 109.5 . . ?
C3 C4 H4A 109.5 . . ?
C3 C4 H4B 109.5 . . ?
C3 C4 H4C 109.5 . . ?
H4A C4 H4B 109.5 . . ?
H4A C4 H4C 109.5 . . ?
H4B C4 H4C 109.5 . . ?
C7 C10 H10A 109.5 . . ?
C7 C10 H10B 109.5 . . ?
C7 C10 H10C 109.5 . . ?
H10A C10 H10B 109.5 . . ?
H10A C10 H10C 109.5 . . ?
H10B C10 H10C 109.5 . . ?
O1 C13 C14 107.63(18) . . ?
O1 C13 H13A 110.2 . . ?
O1 C13 H13B 110.2 . . ?
C14 C13 H13A 110.2 . . ?
C14 C13 H13B 110.2 . . ?
H13A C13 H13B 108.5 . . ?
C3 C5 H5A 109.5 . . ?
C3 C5 H5B 109.5 . . ?
C3 C5 H5C 109.5 . . ?
H5A C5 H5B 109.5 . . ?
H5A C5 H5C 109.5 . . ?
H5B C5 H5C 109.5 . . ?

loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
K1 P1 C1 C2 -81.14(15) . . . . ?
K1 P1 C1 C3 103.67(14) . . . . ?
K1 O6 C22 C21 33.4(2) . . . . ?
K1 O6 C11 C12 -33.4(2) . . . . ?
K1 O1 C12 C11 -60.73(19) . . . . ?
K1 O1 C13 C14 63.31(19) . . . . ?
K1 O2 C14 C13 36.2(2) . . . . ?
K1 O2 C15 C16 -40.0(2) . . . . ?
K1 O3 C17 C18 55.1(2) . . . . ?
K1 O3 C16 C15 -56.13(19) . . . . ?
K1 O5 C20 C19 -65.9(2) . . . . ?
K1 O5 C21 C22 60.83(19) . . . . ?
K1 O4 C18 C17 42.4(2) . . . . ?
K1 O4 C19 C20 -29.7(3) . . . . ?
P2 P1 C1 C2 1.10(16) . . . . ?
P2 P1 C1 C3 -174.10(13) . . . . ?
P2 P3 C2 C7 -175.10(13) . . . . ?
P2 P3 C2 C1 0.93(16) . . . . ?
P3 C2 C7 C8 -134.54(19) . . . . ?
P3 C2 C7 C9 -15.9(2) . . . . ?
P3 C2 C7 C10 99.7(2) . . . . ?
P3 C2 C1 P1 -1.4(2) . . . . ?
P3 C2 C1 C3 172.80(17) . . . . ?
O6 C22 C21 O5 -64.7(2) . . . . ?
O6 C11 C12 O1 63.6(2) . . . . ?
O2 C14 C13 O1 -67.0(2) . . . . ?
O2 C15 C16 O3 63.4(2) . . . . ?
O4 C18 C17 O3 -65.4(2) . . . . ?
O4 C19 C20 O5 65.7(3) . . . . ?
C14 O2 C15 C16 -179.49(18) . . . . ?
C18 O4 C19 C20 -172.6(2) . . . . ?
C17 O3 C16 C15 175.12(17) . . . . ?
C15 O2 C14 C13 175.50(18) . . . . ?
C7 C2 C1 P1 173.75(17) . . . . ?
C7 C2 C1 C3 -12.0(4) . . . . ?
C22 O6 C11 C12 171.61(19) . . . . ?
C11 O6 C22 C21 -171.63(18) . . . . ?
C19 O4 C18 C17 -173.56(19) . . . . ?
C1 C2 C7 C8 50.0(3) . . . . ?
C1 C2 C7 C9 168.7(2) . . . . ?
C1 C2 C7 C10 -75.7(3) . . . . ?
C16 O3 C17 C18 -174.88(17) . . . . ?
C12 O1 C13 C14 -176.26(18) . . . . ?
C20 O5 C21 C22 176.47(19) . . . . ?
C21 O5 C20 C19 178.17(19) . . . . ?
C6 C3 C1 P1 -131.51(18) . . . . ?
C6 C3 C1 C2 54.0(3) . . . . ?
C4 C3 C1 P1 -14.1(2) . . . . ?
C4 C3 C1 C2 171.4(2) . . . . ?
C13 O1 C12 C11 177.66(19) . . . . ?
C5 C3 C1 P1 102.46(19) . . . . ?
C5 C3 C1 C2 -72.1(3) . . . . ?

_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 2.372
_oxdiff_exptl_absorpt_empirical_full_min 0.548
_exptl_crystal_recrystallization_method 
'Re-crystallisation from solvent: n-hexane/toluene'
