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

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

data_0253abc16s
_database_code_depnum_ccdc_archive 'CCDC 1972811'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# cis-POCOP-14.2BH3
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT301_0253abc16s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        59% Note  
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C28 H56 B2 O2 P2'
_chemical_formula_sum            'C28 H56 B2 O2 P2'
_chemical_formula_weight         508.28
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
B B 0.0090 0.0039 '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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   36.2517(2)
_cell_length_b                   6.78334(5)
_cell_length_c                   13.08712(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3218.23(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    26521
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5430
_cell_measurement_theta_min      4.1500
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    1.368
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.548
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.049
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1120
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 4 -4 0.1694
24 0 0 0.0314
-1 -4 4 0.1531
-24 0 0 0.0371
0 4 1 0.1372
0 0 8 0.1173
0 -4 0 0.1115
0 0 -8 0.1110

_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 293 K'
_exptl_crystal_size_max          0.264
_exptl_crystal_size_mid          0.234
_exptl_crystal_size_min          0.072
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
-1.7561 3.9119 -3.8500 -0.0316 -0.0438 0.9985
23.5246 0.0491 -0.1616 0.4465 0.8948 -0.0028
-0.5850 -3.9192 3.8685 -0.0128 -0.0452 -0.9989
-23.5280 0.0514 0.0625 -0.4466 -0.8943 0.0284
-0.1083 4.3906 0.6530 0.4641 -0.2231 0.8572
0.3790 0.0364 8.4926 0.8018 -0.4044 -0.4400
0.1165 -4.3968 -0.4749 -0.4479 0.2150 -0.8679
-0.3864 0.2137 -8.4829 -0.7779 0.3930 0.4902

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0240
_diffrn_reflns_av_unetI/netI     0.0137
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -44
_diffrn_reflns_limit_k_max       8
_diffrn_reflns_limit_k_min       -7
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            39875
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.049
_diffrn_reflns_theta_max         70.049
_diffrn_reflns_theta_min         6.526
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -115.00 -69.00   1.00    2.00    --  -40.77-132.00  27.00   46
  2  ω    -67.00  35.00   1.00    2.00    --  -40.77  37.00 -60.00  102
  3  ω      1.00  83.00   1.00    2.00    --   40.77 -99.00-150.00   82
  4  ω     23.00  98.00   1.00    2.00    --   40.77-125.00 -60.00   75
  5  ω     24.00 109.00   1.00    8.00    --  108.00 -94.00 -90.00   85
  6  ω     80.00 178.00   1.00    8.00    --  108.00  45.00 150.00   98
  7  ω     74.00 178.00   1.00    8.00    --  108.00  77.00 150.00  104
  8  ω    100.00 178.00   1.00    8.00    --  108.00 111.00 120.00   78
  9  ω     77.00 178.00   1.00    8.00    --  108.00  30.00 -90.00  101
 10  ω   -119.00  -7.00   1.00    2.00    --  -40.77 -77.00-120.00  112
 11  ω   -115.00 -11.00   1.00    2.00    --  -40.77 -57.00   0.00  104
 12  ω     29.00 142.00   1.00    8.00    --  108.00 -77.00  60.00  113
 13  ω     80.00 178.00   1.00    8.00    --  108.00  45.00  90.00   98
 14  ω     74.00 178.00   1.00    8.00    --  108.00  77.00 -60.00  104
 15  ω     77.00 178.00   1.00    8.00    --  108.00  30.00  30.00  101
 16  ω   -115.00 -11.00   1.00    2.00    --  -40.77 -57.00 120.00  104
 17  ω      1.00  83.00   1.00    2.00    --   40.77 -99.00  90.00   82
 18  ω     80.00 178.00   1.00    8.00    --  108.00  45.00-150.00   98
 19  ω     74.00 178.00   1.00    8.00    --  108.00  77.00  30.00  104
 20  ω     74.00 178.00   1.00    8.00    --  108.00  77.00  90.00  104
 21  ω     30.00 116.00   1.00    8.00    --  108.00-111.00-120.00   86
 22  ω   -119.00  -7.00   1.00    2.00    --  -40.77 -77.00 -30.00  112
 23  ω   -115.00 -65.00   1.00    2.00    --  -40.77-137.00-148.00   50
 24  ω     74.00 178.00   1.00    8.00    --  108.00  77.00 -90.00  104
 25  ω     74.00 149.00   1.00    8.00    --  108.00  77.00-120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0194287000
_diffrn_orient_matrix_UB_12      0.0923189000
_diffrn_orient_matrix_UB_13      0.0931477000
_diffrn_orient_matrix_UB_21      0.0377867000
_diffrn_orient_matrix_UB_22      -0.0425862000
_diffrn_orient_matrix_UB_23      -0.0491249000
_diffrn_orient_matrix_UB_31      -0.0009034000
_diffrn_orient_matrix_UB_32      0.2030494000
_diffrn_orient_matrix_UB_33      -0.0526359000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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         0.908
_reflns_Friedel_fraction_full    0.998
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                6000
_reflns_number_total             6086
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.562
_refine_diff_density_min         -0.354
_refine_diff_density_rms         0.071
_refine_ls_abs_structure_details 
;
 Flack x determined using 2776 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.011(7)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         6086
_refine_ls_number_restraints     1187
_refine_ls_R_factor_all          0.0721
_refine_ls_R_factor_gt           0.0711
_refine_ls_restrained_S_all      1.185
_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)+(0.1441P)²+2.6672P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2063
_refine_ls_wR_factor_ref         0.2077
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 P2-C117 \\sim P2-C217 \\sim P3-C130
 with sigma of 0.01
 C218-C217 \\sim C118-C117 \\sim C219-C218 \\sim C119-C118 \\sim C220-C219
\\sim C120-C119 \\sim C221-
 C220 \\sim C121-C120 \\sim C222-C221 \\sim C122-C121 \\sim C223-C222 \\sim
C224-C223 \\sim C123-C122 ~
 C225-C224 \\sim C226-C225 \\sim C124-C123 \\sim C227-C226 \\sim C125-C124
\\sim C126-C125 \\sim C228-
 C227 \\sim C127-C126 \\sim C128-C127 \\sim C229-C228 \\sim C129-C128 \\sim
C130-C129 \\sim C229-C130
 with sigma of 0.01
 P2-C209 \\sim P2-C109 \\sim P3-C113
 with sigma of 0.01
 C211-C209 \\sim C111-C109 \\sim C110-C109 \\sim C210-C209 \\sim C212-C209
\\sim C112-C109 \\sim C216-
 C113 \\sim C116-C113 \\sim C115-C113 \\sim C215-C113 \\sim C214-C113 \\sim
C114-C113
 with sigma of 0.01
 C110-C111 \\sim C111-C112 \\sim C112-C110 \\sim C210-C211 \\sim C211-C212
\\sim C212-C210 \\sim C114-
 C115 \\sim C115-C116 \\sim C116-C114 \\sim C214-C215 \\sim C215-C216 \\sim
C216-C214
 with sigma of 0.01
 C211-P2 \\sim C111-P2 \\sim C110-P2 \\sim C210-P2 \\sim C212-P2 \\sim C112-P2
\\sim C216-P3 \\sim C116-P3
 \\sim C115-P3 \\sim C215-P3 \\sim C214-P3 \\sim C114-P3
 with sigma of 0.01
 B3-H3C \\sim B3-H3B \\sim B3-H3A \\sim B2-H2C \\sim B2-H2A \\sim B2-H2B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C109 \\sim C110 \\sim C111 \\sim C112 \\sim C114 \\sim C115 \\sim C116 \\sim
C117 \\sim C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim
C124 \\sim C125 \\sim C126 \\sim C127 \\sim C128 \\sim C129 \\sim C130 \\sim
C209 \\sim C210 \\sim C211 \\sim C212 \\sim C214 \\sim C215 \\sim C216 \\sim
C217 \\sim C218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223 \\sim
C224 \\sim C225 \\sim C226 \\sim C227 \\sim C228 \\sim C229: within 2A with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C130) \\sim Ueq, Uanis(C117) \\sim Ueq, Uanis(C225) \\sim Ueq,
Uanis(C224) \\sim Ueq, Uanis(C129) \\sim Ueq, Uanis(C226) \\sim Ueq,
Uanis(C228) \\sim Ueq, Uanis(C128) \\sim Ueq, Uanis(C229) \\sim Ueq,
Uanis(C227) \\sim Ueq, Uanis(C127) \\sim Ueq, Uanis(C119) \\sim Ueq,
Uanis(C223) \\sim Ueq, Uanis(C222) \\sim Ueq, Uanis(C218) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C125) \\sim Ueq, Uanis(C126) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C219) \\sim Ueq, Uanis(C220) \\sim Ueq,
Uanis(C221) \\sim Ueq, Uanis(C118) \\sim Ueq, Uanis(C217) \\sim Ueq,
Uanis(C109) \\sim Ueq, Uanis(C111) \\sim Ueq, Uanis(C110) \\sim Ueq,
Uanis(C112) \\sim Ueq, Uanis(C209) \\sim Ueq, Uanis(C212) \\sim Ueq,
Uanis(C210) \\sim Ueq, Uanis(C211) \\sim Ueq, Uanis(C114) \\sim Ueq,
Uanis(C214) \\sim Ueq, Uanis(C215) \\sim Ueq, Uanis(C115) \\sim Ueq,
Uanis(C216) \\sim Ueq, Uanis(C116) \\sim Ueq: with sigma of 0.005 and sigma for
terminal atoms of 0.01
4. Others
 Fixed Sof: C109(0.5) C110(0.5) H11A(0.5) H11B(0.5) H11C(0.5) C111(0.5)
 H11D(0.5) H11E(0.5) H11F(0.5) C112(0.5) H11G(0.5) H11H(0.5) H11I(0.5)
 C114(0.5) H11J(0.5) H11K(0.5) H11L(0.5) C115(0.5) H11M(0.5) H11N(0.5)
 H11O(0.5) C116(0.5) H11P(0.5) H11Q(0.5) H11R(0.5) C117(0.5) H11S(0.5)
 H11T(0.5) C118(0.5) H11U(0.5) H11V(0.5) C119(0.5) H11W(0.5) H11X(0.5)
 C120(0.5) H12A(0.5) H12B(0.5) C121(0.5) H12C(0.5) H12D(0.5) C122(0.5)
 H12E(0.5) H12F(0.5) C123(0.5) H12G(0.5) H12H(0.5) C124(0.5) H12I(0.5)
 H12J(0.5) C125(0.5) H12K(0.5) H12L(0.5) C126(0.5) H12M(0.5) H12N(0.5)
 C127(0.5) H12O(0.5) H12P(0.5) C128(0.5) H12Q(0.5) H12R(0.5) C129(0.5)
 H12S(0.5) H12T(0.5) H13A(0.5) H13B(0.5) H13C(0.5) H13D(0.5) C209(0.5)
 C210(0.5) H21A(0.5) H21B(0.5) H21C(0.5) C211(0.5) H21D(0.5) H21E(0.5)
 H21F(0.5) C212(0.5) H21G(0.5) H21H(0.5) H21I(0.5) C214(0.5) H21J(0.5)
 H21K(0.5) H21L(0.5) C215(0.5) H21M(0.5) H21N(0.5) H21O(0.5) C216(0.5)
 H21P(0.5) H21Q(0.5) H21R(0.5) C217(0.5) H21S(0.5) H21T(0.5) C218(0.5)
 H21U(0.5) H21V(0.5) C219(0.5) H21W(0.5) H21X(0.5) C220(0.5) H22A(0.5)
 H22B(0.5) C221(0.5) H22C(0.5) H22D(0.5) C222(0.5) H22E(0.5) H22F(0.5)
 C223(0.5) H22G(0.5) H22H(0.5) C224(0.5) H22I(0.5) H22J(0.5) C225(0.5)
 H22K(0.5) H22L(0.5) C226(0.5) H22M(0.5) H22N(0.5) C227(0.5) H22O(0.5)
 H22P(0.5) C228(0.5) H22Q(0.5) H22R(0.5) C229(0.5) H22S(0.5) H22T(0.5)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C119(H11W,H11X), C120(H12A,H12B), C121(H12C,
 H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L),
 C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,H12R), C129(H12S,H12T), C130(H13A,
 H13B), C130(H13C,H13D), C217(H21S,H21T), C218(H21U,H21V), C219(H21W,H21X),
 C220(H22A,H22B), C221(H22C,H22D), C222(H22E,H22F), C223(H22G,H22H), C224(H22I,
 H22J), C225(H22K,H22L), C226(H22M,H22N), C227(H22O,H22P), C228(H22Q,H22R),
 C229(H22S,H22T)
5.b Aromatic/amide H refined with riding coordinates:
 C101(H101), C103(H103), C104(H104), C105(H105)
5.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R), C210(H21A,H21B,H21C),
 C211(H21D,H21E,H21F), C212(H21G,H21H,H21I), C214(H21J,H21K,H21L), C215(H21M,
 H21N,H21O), C216(H21P,H21Q,H21R)
5.d Idealised Me refined as rotating group with stretchable bonds:
 B3(H3A,H3B,H3C), B2(H2A,H2B,H2C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
P2 P 0.62490(4) 0.03657(19) 0.72937(11) 0.0436(4) Uani 1 1 d D . . . .
P3 P 0.56946(3) 0.47405(15) 0.25089(10) 0.0348(3) Uani 1 1 d D . . . .
O107 O 0.59703(15) 0.1817(6) 0.6690(3) 0.0610(13) Uani 1 1 d . . . . .
O108 O 0.55105(10) 0.4572(5) 0.3642(3) 0.0360(8) Uani 1 1 d . . . . .
C101 C 0.57557(13) 0.3102(7) 0.5140(3) 0.0325(9) Uani 1 1 d . . . . .
H101 H 0.5879 0.4301 0.5296 0.039 Uiso 1 1 calc R . . . .
C102 C 0.57812(16) 0.1500(8) 0.5789(4) 0.0393(11) Uani 1 1 d . . . . .
C103 C 0.56039(18) -0.0265(8) 0.5578(4) 0.0459(13) Uani 1 1 d . . . . .
H103 H 0.5626 -0.1360 0.6026 0.055 Uiso 1 1 calc R . . . .
C104 C 0.53938(18) -0.0394(8) 0.4697(5) 0.0497(14) Uani 1 1 d . . . . .
H104 H 0.5268 -0.1586 0.4546 0.060 Uiso 1 1 calc R . . . .
C105 C 0.53644(16) 0.1181(8) 0.4033(4) 0.0441(12) Uani 1 1 d . . . . .
H105 H 0.5221 0.1074 0.3428 0.053 Uiso 1 1 calc R . . . .
C106 C 0.55477(12) 0.2925(7) 0.4262(3) 0.0310(9) Uani 1 1 d . . . . .
C109 C 0.6142(3) 0.1001(14) 0.8612(6) 0.041(2) Uani 0.5 1 d D U P A 1
C110 C 0.5753(3) 0.022(2) 0.8852(10) 0.077(4) Uani 0.5 1 d D U P A 1
H11A H 0.5572 0.0893 0.8419 0.116 Uiso 0.5 1 calc GR . P A 1
H11B H 0.5695 0.0464 0.9573 0.116 Uiso 0.5 1 calc GR . P A 1
H11C H 0.5744 -0.1203 0.8718 0.116 Uiso 0.5 1 calc GR . P A 1
C111 C 0.6427(4) 0.000(2) 0.9315(8) 0.066(4) Uani 0.5 1 d D U P A 1
H11D H 0.6448 -0.1397 0.9134 0.099 Uiso 0.5 1 calc GR . P A 1
H11E H 0.6348 0.0122 1.0028 0.099 Uiso 0.5 1 calc GR . P A 1
H11F H 0.6668 0.0641 0.9229 0.099 Uiso 0.5 1 calc GR . P A 1
C112 C 0.6153(4) 0.3239(14) 0.8771(9) 0.057(3) Uani 0.5 1 d D U P A 1
H11G H 0.6397 0.3742 0.8578 0.085 Uiso 0.5 1 calc GR . P A 1
H11H H 0.6105 0.3543 0.9491 0.085 Uiso 0.5 1 calc GR . P A 1
H11I H 0.5964 0.3865 0.8344 0.085 Uiso 0.5 1 calc GR . P A 1
C113 C 0.53039(15) 0.5563(7) 0.1727(4) 0.0467(13) Uani 1 1 d D . . . .
C114 C 0.5061(3) 0.3778(16) 0.1488(11) 0.071(5) Uani 0.5 1 d D U P B 1
H11J H 0.5216 0.2691 0.1244 0.107 Uiso 0.5 1 calc GR . P B 1
H11K H 0.4882 0.4130 0.0958 0.107 Uiso 0.5 1 calc GR . P B 1
H11L H 0.4931 0.3368 0.2108 0.107 Uiso 0.5 1 calc GR . P B 1
C115 C 0.5473(4) 0.6361(19) 0.0705(7) 0.063(4) Uani 0.5 1 d D U P B 1
H11M H 0.5598 0.7617 0.0834 0.095 Uiso 0.5 1 calc GR . P B 1
H11N H 0.5276 0.6560 0.0204 0.095 Uiso 0.5 1 calc GR . P B 1
H11O H 0.5651 0.5404 0.0438 0.095 Uiso 0.5 1 calc GR . P B 1
C116 C 0.5090(3) 0.7198(16) 0.2250(10) 0.052(4) Uani 0.5 1 d D U P B 1
H11P H 0.4945 0.6645 0.2813 0.079 Uiso 0.5 1 calc GR . P B 1
H11Q H 0.4925 0.7827 0.1756 0.079 Uiso 0.5 1 calc GR . P B 1
H11R H 0.5263 0.8180 0.2520 0.079 Uiso 0.5 1 calc GR . P B 1
C117 C 0.6674(3) 0.165(2) 0.6987(11) 0.064(3) Uani 0.5 1 d D U P A 1
H11S H 0.6680 0.2872 0.7396 0.077 Uiso 0.5 1 calc R . P A 1
H11T H 0.6881 0.0813 0.7225 0.077 Uiso 0.5 1 calc R . P A 1
C118 C 0.6752(4) 0.221(3) 0.5864(11) 0.080(3) Uani 0.5 1 d D U P A 1
H11U H 0.6583 0.3291 0.5665 0.096 Uiso 0.5 1 calc R . P A 1
H11V H 0.6696 0.1062 0.5424 0.096 Uiso 0.5 1 calc R . P A 1
C119 C 0.7154(4) 0.288(3) 0.5660(12) 0.090(3) Uani 0.5 1 d D U P A 1
H11W H 0.7324 0.1747 0.5754 0.108 Uiso 0.5 1 calc R . P A 1
H11X H 0.7225 0.3922 0.6150 0.108 Uiso 0.5 1 calc R . P A 1
C120 C 0.7184(4) 0.367(3) 0.4545(12) 0.084(4) Uani 0.5 1 d D U P A 1
H12A H 0.7059 0.2734 0.4080 0.101 Uiso 0.5 1 calc R . P A 1
H12B H 0.7052 0.4945 0.4502 0.101 Uiso 0.5 1 calc R . P A 1
C121 C 0.7588(4) 0.397(3) 0.4167(15) 0.085(4) Uani 0.5 1 d D U P A 1
H12C H 0.7723 0.2708 0.4236 0.102 Uiso 0.5 1 calc R . P A 1
H12D H 0.7583 0.4316 0.3432 0.102 Uiso 0.5 1 calc R . P A 1
C122 C 0.7804(5) 0.560(3) 0.4753(18) 0.082(3) Uani 0.5 1 d D U P A 1
H12E H 0.7815 0.5233 0.5485 0.098 Uiso 0.5 1 calc R . P A 1
H12F H 0.8060 0.5636 0.4493 0.098 Uiso 0.5 1 calc R . P A 1
C123 C 0.7637(7) 0.769(3) 0.4664(15) 0.084(4) Uani 0.5 1 d D U P A 1
H12G H 0.7419 0.7785 0.5120 0.101 Uiso 0.5 1 calc R . P A 1
H12H H 0.7821 0.8667 0.4900 0.101 Uiso 0.5 1 calc R . P A 1
C124 C 0.7519(6) 0.821(3) 0.3569(14) 0.088(4) Uani 0.5 1 d D U P A 1
H12I H 0.7347 0.7203 0.3295 0.106 Uiso 0.5 1 calc R . P A 1
H12J H 0.7736 0.8297 0.3113 0.106 Uiso 0.5 1 calc R . P A 1
C125 C 0.7325(5) 1.024(3) 0.3675(17) 0.097(4) Uani 0.5 1 d D U P A 1
H12K H 0.7189 1.0275 0.4331 0.116 Uiso 0.5 1 calc R . P A 1
H12L H 0.7515 1.1287 0.3700 0.116 Uiso 0.5 1 calc R . P A 1
C126 C 0.7054(5) 1.071(3) 0.2799(16) 0.094(4) Uani 0.5 1 d D U P A 1
H12M H 0.7193 1.0889 0.2155 0.113 Uiso 0.5 1 calc R . P A 1
H12N H 0.6922 1.1956 0.2950 0.113 Uiso 0.5 1 calc R . P A 1
C127 C 0.6770(4) 0.902(3) 0.2668(13) 0.078(3) Uani 0.5 1 d D U P A 1
H12O H 0.6909 0.7850 0.2433 0.094 Uiso 0.5 1 calc R . P A 1
H12P H 0.6604 0.9408 0.2103 0.094 Uiso 0.5 1 calc R . P A 1
C128 C 0.6523(4) 0.835(2) 0.3573(11) 0.067(3) Uani 0.5 1 d D U P A 1
H12Q H 0.6319 0.9304 0.3684 0.080 Uiso 0.5 1 calc R . P A 1
H12R H 0.6669 0.8254 0.4210 0.080 Uiso 0.5 1 calc R . P A 1
C129 C 0.6360(3) 0.6206(19) 0.3253(11) 0.056(3) Uani 0.5 1 d D U P A 1
H12S H 0.6536 0.5473 0.2816 0.067 Uiso 0.5 1 calc R . P A 1
H12T H 0.6299 0.5403 0.3861 0.067 Uiso 0.5 1 calc R . P A 1
C130 C 0.60052(16) 0.6792(9) 0.2647(5) 0.0550(14) Uani 1 1 d D U . . .
H13A H 0.6076 0.7280 0.1962 0.066 Uiso 0.5 1 calc R . P A 1
H13B H 0.5878 0.7876 0.3010 0.066 Uiso 0.5 1 calc R . P A 1
H13C H 0.6159 0.6857 0.2022 0.066 Uiso 0.5 1 calc R . P A 2
H13D H 0.5855 0.8010 0.2666 0.066 Uiso 0.5 1 calc R . P A 2
C209 C 0.6009(3) 0.0377(16) 0.8528(7) 0.057(3) Uani 0.5 1 d D U P A 2
C210 C 0.5640(3) -0.075(2) 0.8410(10) 0.068(4) Uani 0.5 1 d D U P A 2
H21A H 0.5493 -0.0132 0.7869 0.102 Uiso 0.5 1 calc GR . P A 2
H21B H 0.5504 -0.0698 0.9056 0.102 Uiso 0.5 1 calc GR . P A 2
H21C H 0.5691 -0.2123 0.8230 0.102 Uiso 0.5 1 calc GR . P A 2
C211 C 0.6248(4) -0.066(2) 0.9335(7) 0.066(4) Uani 0.5 1 d D U P A 2
H21D H 0.6272 -0.2061 0.9161 0.100 Uiso 0.5 1 calc GR . P A 2
H21E H 0.6133 -0.0529 1.0008 0.100 Uiso 0.5 1 calc GR . P A 2
H21F H 0.6494 -0.0055 0.9349 0.100 Uiso 0.5 1 calc GR . P A 2
C212 C 0.5934(5) 0.2513(18) 0.8854(10) 0.082(4) Uani 0.5 1 d D U P A 2
H21G H 0.6169 0.3176 0.8997 0.123 Uiso 0.5 1 calc GR . P A 2
H21H H 0.5781 0.2520 0.9471 0.123 Uiso 0.5 1 calc GR . P A 2
H21I H 0.5806 0.3208 0.8303 0.123 Uiso 0.5 1 calc GR . P A 2
C214 C 0.4972(2) 0.4134(16) 0.1924(9) 0.050(3) Uani 0.5 1 d D U P B 2
H21J H 0.5049 0.2774 0.1789 0.075 Uiso 0.5 1 calc GR . P B 2
H21K H 0.4767 0.4482 0.1470 0.075 Uiso 0.5 1 calc GR . P B 2
H21L H 0.4892 0.4251 0.2637 0.075 Uiso 0.5 1 calc GR . P B 2
C215 C 0.5404(4) 0.549(2) 0.0594(6) 0.066(4) Uani 0.5 1 d D U P B 2
H21M H 0.5646 0.6105 0.0490 0.098 Uiso 0.5 1 calc GR . P B 2
H21N H 0.5218 0.6203 0.0198 0.098 Uiso 0.5 1 calc GR . P B 2
H21O H 0.5414 0.4114 0.0367 0.098 Uiso 0.5 1 calc GR . P B 2
C216 C 0.5182(3) 0.7636(13) 0.2039(10) 0.054(4) Uani 0.5 1 d D U P B 2
H21P H 0.5191 0.7757 0.2785 0.081 Uiso 0.5 1 calc GR . P B 2
H21Q H 0.4930 0.7870 0.1800 0.081 Uiso 0.5 1 calc GR . P B 2
H21R H 0.5348 0.8610 0.1731 0.081 Uiso 0.5 1 calc GR . P B 2
C217 C 0.6656(4) 0.174(3) 0.7557(13) 0.075(3) Uani 0.5 1 d D U P A 2
H21S H 0.6587 0.3083 0.7788 0.090 Uiso 0.5 1 calc R . P A 2
H21T H 0.6794 0.1098 0.8117 0.090 Uiso 0.5 1 calc R . P A 2
C218 C 0.6906(5) 0.190(3) 0.6612(14) 0.091(3) Uani 0.5 1 d D U P A 2
H21U H 0.6768 0.2580 0.6060 0.109 Uiso 0.5 1 calc R . P A 2
H21V H 0.6967 0.0561 0.6369 0.109 Uiso 0.5 1 calc R . P A 2
C219 C 0.7270(5) 0.304(3) 0.6819(19) 0.106(4) Uani 0.5 1 d D U P A 2
H21W H 0.7314 0.3268 0.7556 0.128 Uiso 0.5 1 calc R . P A 2
H21X H 0.7283 0.4309 0.6443 0.128 Uiso 0.5 1 calc R . P A 2
C220 C 0.7532(5) 0.142(3) 0.635(2) 0.109(4) Uani 0.5 1 d D U P A 2
H22A H 0.7583 0.0434 0.6893 0.131 Uiso 0.5 1 calc R . P A 2
H22B H 0.7397 0.0739 0.5800 0.131 Uiso 0.5 1 calc R . P A 2
C221 C 0.7906(5) 0.214(2) 0.5920(17) 0.095(4) Uani 0.5 1 d D U P A 2
H22C H 0.7909 0.2010 0.5167 0.114 Uiso 0.5 1 calc R . P A 2
H22D H 0.8111 0.1355 0.6207 0.114 Uiso 0.5 1 calc R . P A 2
C222 C 0.7948(5) 0.435(2) 0.6231(13) 0.083(4) Uani 0.5 1 d D U P A 2
H22E H 0.7705 0.4915 0.6406 0.099 Uiso 0.5 1 calc R . P A 2
H22F H 0.8111 0.4467 0.6835 0.099 Uiso 0.5 1 calc R . P A 2
C223 C 0.8116(4) 0.546(2) 0.5322(10) 0.065(3) Uani 0.5 1 d D U P A 2
H22G H 0.8317 0.4641 0.5039 0.078 Uiso 0.5 1 calc R . P A 2
H22H H 0.8231 0.6684 0.5589 0.078 Uiso 0.5 1 calc R . P A 2
C224 C 0.7858(4) 0.606(3) 0.4420(12) 0.073(3) Uani 0.5 1 d D U P A 2
H22I H 0.8002 0.6658 0.3856 0.087 Uiso 0.5 1 calc R . P A 2
H22J H 0.7723 0.4898 0.4155 0.087 Uiso 0.5 1 calc R . P A 2
C225 C 0.7589(5) 0.757(4) 0.4895(14) 0.079(3) Uani 0.5 1 d D U P A 2
H22K H 0.7728 0.8737 0.5143 0.095 Uiso 0.5 1 calc R . P A 2
H22L H 0.7458 0.6975 0.5481 0.095 Uiso 0.5 1 calc R . P A 2
C226 C 0.7309(4) 0.820(3) 0.4063(15) 0.083(3) Uani 0.5 1 d D U P A 2
H22M H 0.7211 0.9527 0.4231 0.100 Uiso 0.5 1 calc R . P A 2
H22N H 0.7437 0.8293 0.3396 0.100 Uiso 0.5 1 calc R . P A 2
C227 C 0.6988(3) 0.674(2) 0.3977(13) 0.071(3) Uani 0.5 1 d D U P A 2
H22O H 0.6893 0.6457 0.4670 0.085 Uiso 0.5 1 calc R . P A 2
H22P H 0.7081 0.5489 0.3687 0.085 Uiso 0.5 1 calc R . P A 2
C228 C 0.6665(3) 0.749(2) 0.3304(13) 0.068(3) Uani 0.5 1 d D U P A 2
H22Q H 0.6671 0.8949 0.3311 0.081 Uiso 0.5 1 calc R . P A 2
H22R H 0.6713 0.7067 0.2592 0.081 Uiso 0.5 1 calc R . P A 2
C229 C 0.6269(3) 0.684(3) 0.3582(10) 0.067(3) Uani 0.5 1 d D U P A 2
H22S H 0.6169 0.7753 0.4101 0.080 Uiso 0.5 1 calc R . P A 2
H22T H 0.6279 0.5507 0.3891 0.080 Uiso 0.5 1 calc R . P A 2
B3 B 0.5935(3) 0.2435(11) 0.2031(6) 0.064(2) Uani 1 1 d D . . . .
H3A H 0.6122(15) 0.197(6) 0.256(3) 0.096 Uiso 1 1 calc DGR . . . .
H3B H 0.6068(15) 0.274(3) 0.136(4) 0.096 Uiso 1 1 calc DGR . . . .
H3C H 0.5743(8) 0.135(5) 0.191(5) 0.096 Uiso 1 1 calc DGR . . . .
B2 B 0.6309(3) -0.2304(12) 0.6847(9) 0.079(3) Uani 1 1 d D . . . .
H2A H 0.6070(11) -0.307(4) 0.697(5) 0.119 Uiso 1 1 calc DGR . . . .
H2B H 0.6521(16) -0.295(4) 0.725(4) 0.119 Uiso 1 1 calc DGR . . . .
H2C H 0.6370(18) -0.2322(13) 0.608(3) 0.119 Uiso 1 1 calc DGR . . . .


_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
P2 O107 1.617(4) . ?
P2 C109 1.821(8) . ?
P2 C117 1.812(10) . ?
P2 C209 1.835(10) . ?
P2 C217 1.780(10) . ?
P2 B2 1.915(8) . ?
P3 O108 1.630(4) . ?
P3 C113 1.834(5) . ?
P3 C130 1.799(5) . ?
P3 B3 1.896(7) . ?
O107 C102 1.380(6) . ?
O108 C106 1.387(6) . ?
C101 H101 0.9500 . ?
C101 C102 1.382(7) . ?
C101 C106 1.379(7) . ?
C102 C103 1.387(8) . ?
C103 H103 0.9500 . ?
C103 C104 1.385(9) . ?
C104 H104 0.9500 . ?
C104 C105 1.381(8) . ?
C105 H105 0.9500 . ?
C105 C106 1.390(7) . ?
C109 C110 1.540(9) . ?
C109 C111 1.542(9) . ?
C109 C112 1.533(9) . ?
C110 H11A 0.9800 . ?
C110 H11B 0.9800 . ?
C110 H11C 0.9800 . ?
C111 H11D 0.9800 . ?
C111 H11E 0.9800 . ?
C111 H11F 0.9800 . ?
C112 H11G 0.9800 . ?
C112 H11H 0.9800 . ?
C112 H11I 0.9800 . ?
C113 C114 1.529(8) . ?
C113 C115 1.568(8) . ?
C113 C116 1.516(8) . ?
C113 C214 1.567(8) . ?
C113 C215 1.528(8) . ?
C113 C216 1.529(8) . ?
C114 H11J 0.9800 . ?
C114 H11K 0.9800 . ?
C114 H11L 0.9800 . ?
C115 H11M 0.9800 . ?
C115 H11N 0.9800 . ?
C115 H11O 0.9800 . ?
C116 H11P 0.9800 . ?
C116 H11Q 0.9800 . ?
C116 H11R 0.9800 . ?
C117 H11S 0.9900 . ?
C117 H11T 0.9900 . ?
C117 C118 1.545(10) . ?
C118 H11U 0.9900 . ?
C118 H11V 0.9900 . ?
C118 C119 1.550(10) . ?
C119 H11W 0.9900 . ?
C119 H11X 0.9900 . ?
C119 C120 1.560(11) . ?
C120 H12A 0.9900 . ?
C120 H12B 0.9900 . ?
C120 C121 1.559(11) . ?
C121 H12C 0.9900 . ?
C121 H12D 0.9900 . ?
C121 C122 1.556(11) . ?
C122 H12E 0.9900 . ?
C122 H12F 0.9900 . ?
C122 C123 1.547(11) . ?
C123 H12G 0.9900 . ?
C123 H12H 0.9900 . ?
C123 C124 1.535(11) . ?
C124 H12I 0.9900 . ?
C124 H12J 0.9900 . ?
C124 C125 1.557(11) . ?
C125 H12K 0.9900 . ?
C125 H12L 0.9900 . ?
C125 C126 1.543(11) . ?
C126 H12M 0.9900 . ?
C126 H12N 0.9900 . ?
C126 C127 1.547(11) . ?
C127 H12O 0.9900 . ?
C127 H12P 0.9900 . ?
C127 C128 1.556(10) . ?
C128 H12Q 0.9900 . ?
C128 H12R 0.9900 . ?
C128 C129 1.626(10) . ?
C129 H12S 0.9900 . ?
C129 H12T 0.9900 . ?
C129 C130 1.561(9) . ?
C130 H13A 0.9900 . ?
C130 H13B 0.9900 . ?
C130 H13C 0.9900 . ?
C130 H13D 0.9900 . ?
C130 C229 1.554(10) . ?
C209 C210 1.545(10) . ?
C209 C211 1.537(9) . ?
C209 C212 1.535(9) . ?
C210 H21A 0.9800 . ?
C210 H21B 0.9800 . ?
C210 H21C 0.9800 . ?
C211 H21D 0.9800 . ?
C211 H21E 0.9800 . ?
C211 H21F 0.9800 . ?
C212 H21G 0.9800 . ?
C212 H21H 0.9800 . ?
C212 H21I 0.9800 . ?
C214 H21J 0.9800 . ?
C214 H21K 0.9800 . ?
C214 H21L 0.9800 . ?
C215 H21M 0.9800 . ?
C215 H21N 0.9800 . ?
C215 H21O 0.9800 . ?
C216 H21P 0.9800 . ?
C216 H21Q 0.9800 . ?
C216 H21R 0.9800 . ?
C217 H21S 0.9900 . ?
C217 H21T 0.9900 . ?
C217 C218 1.536(11) . ?
C218 H21U 0.9900 . ?
C218 H21V 0.9900 . ?
C218 C219 1.553(11) . ?
C219 H21W 0.9900 . ?
C219 H21X 0.9900 . ?
C219 C220 1.577(11) . ?
C220 H22A 0.9900 . ?
C220 H22B 0.9900 . ?
C220 C221 1.549(11) . ?
C221 H22C 0.9900 . ?
C221 H22D 0.9900 . ?
C221 C222 1.559(11) . ?
C222 H22E 0.9900 . ?
C222 H22F 0.9900 . ?
C222 C223 1.535(10) . ?
C223 H22G 0.9900 . ?
C223 H22H 0.9900 . ?
C223 C224 1.558(11) . ?
C224 H22I 0.9900 . ?
C224 H22J 0.9900 . ?
C224 C225 1.546(10) . ?
C225 H22K 0.9900 . ?
C225 H22L 0.9900 . ?
C225 C226 1.550(11) . ?
C226 H22M 0.9900 . ?
C226 H22N 0.9900 . ?
C226 C227 1.535(10) . ?
C227 H22O 0.9900 . ?
C227 H22P 0.9900 . ?
C227 C228 1.550(10) . ?
C228 H22Q 0.9900 . ?
C228 H22R 0.9900 . ?
C228 C229 1.543(10) . ?
C229 H22S 0.9900 . ?
C229 H22T 0.9900 . ?
B3 H3A 1.03(4) . ?
B3 H3B 1.03(4) . ?
B3 H3C 1.03(4) . ?
B2 H2A 1.03(4) . ?
B2 H2B 1.03(4) . ?
B2 H2C 1.03(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O107 P2 C109 100.7(3) . . ?
O107 P2 C117 97.5(6) . . ?
O107 P2 C209 97.6(4) . . ?
O107 P2 C217 107.0(6) . . ?
O107 P2 B2 119.9(3) . . ?
C109 P2 B2 122.5(5) . . ?
C117 P2 C109 106.1(6) . . ?
C117 P2 B2 106.7(7) . . ?
C209 P2 B2 109.1(5) . . ?
C217 P2 C209 102.8(7) . . ?
C217 P2 B2 117.4(7) . . ?
O108 P3 C113 102.3(2) . . ?
O108 P3 C130 102.6(3) . . ?
O108 P3 B3 115.5(3) . . ?
C113 P3 B3 114.9(3) . . ?
C130 P3 C113 107.7(2) . . ?
C130 P3 B3 112.6(4) . . ?
C102 O107 P2 129.3(4) . . ?
C106 O108 P3 123.3(3) . . ?
C102 C101 H101 120.6 . . ?
C106 C101 H101 120.6 . . ?
C106 C101 C102 118.7(4) . . ?
O107 C102 C101 115.8(5) . . ?
O107 C102 C103 122.3(5) . . ?
C101 C102 C103 121.7(5) . . ?
C102 C103 H103 120.8 . . ?
C104 C103 C102 118.4(5) . . ?
C104 C103 H103 120.8 . . ?
C103 C104 H104 119.4 . . ?
C105 C104 C103 121.2(5) . . ?
C105 C104 H104 119.4 . . ?
C104 C105 H105 120.5 . . ?
C104 C105 C106 119.1(5) . . ?
C106 C105 H105 120.5 . . ?
O108 C106 C105 120.8(4) . . ?
C101 C106 O108 118.1(4) . . ?
C101 C106 C105 121.0(4) . . ?
C110 C109 P2 107.9(6) . . ?
C110 C109 C111 110.0(7) . . ?
C111 C109 P2 108.5(6) . . ?
C112 C109 P2 110.9(6) . . ?
C112 C109 C110 109.8(7) . . ?
C112 C109 C111 109.7(7) . . ?
C109 C110 H11A 109.5 . . ?
C109 C110 H11B 109.5 . . ?
C109 C110 H11C 109.5 . . ?
H11A C110 H11B 109.5 . . ?
H11A C110 H11C 109.5 . . ?
H11B C110 H11C 109.5 . . ?
C109 C111 H11D 109.5 . . ?
C109 C111 H11E 109.5 . . ?
C109 C111 H11F 109.5 . . ?
H11D C111 H11E 109.5 . . ?
H11D C111 H11F 109.5 . . ?
H11E C111 H11F 109.5 . . ?
C109 C112 H11G 109.5 . . ?
C109 C112 H11H 109.5 . . ?
C109 C112 H11I 109.5 . . ?
H11G C112 H11H 109.5 . . ?
H11G C112 H11I 109.5 . . ?
H11H C112 H11I 109.5 . . ?
C114 C113 P3 108.5(5) . . ?
C114 C113 C115 108.8(6) . . ?
C115 C113 P3 106.2(5) . . ?
C116 C113 P3 111.4(5) . . ?
C116 C113 C114 112.2(7) . . ?
C116 C113 C115 109.4(6) . . ?
C214 C113 P3 108.3(5) . . ?
C215 C113 P3 110.3(5) . . ?
C215 C113 C214 108.8(6) . . ?
C215 C113 C216 110.9(6) . . ?
C216 C113 P3 110.7(5) . . ?
C216 C113 C214 107.7(6) . . ?
C113 C114 H11J 109.5 . . ?
C113 C114 H11K 109.5 . . ?
C113 C114 H11L 109.5 . . ?
H11J C114 H11K 109.5 . . ?
H11J C114 H11L 109.5 . . ?
H11K C114 H11L 109.5 . . ?
C113 C115 H11M 109.5 . . ?
C113 C115 H11N 109.5 . . ?
C113 C115 H11O 109.5 . . ?
H11M C115 H11N 109.5 . . ?
H11M C115 H11O 109.5 . . ?
H11N C115 H11O 109.5 . . ?
C113 C116 H11P 109.5 . . ?
C113 C116 H11Q 109.5 . . ?
C113 C116 H11R 109.5 . . ?
H11P C116 H11Q 109.5 . . ?
H11P C116 H11R 109.5 . . ?
H11Q C116 H11R 109.5 . . ?
P2 C117 H11S 107.6 . . ?
P2 C117 H11T 107.6 . . ?
H11S C117 H11T 107.0 . . ?
C118 C117 P2 119.0(10) . . ?
C118 C117 H11S 107.6 . . ?
C118 C117 H11T 107.6 . . ?
C117 C118 H11U 108.7 . . ?
C117 C118 H11V 108.7 . . ?
C117 C118 C119 114.1(12) . . ?
H11U C118 H11V 107.6 . . ?
C119 C118 H11U 108.7 . . ?
C119 C118 H11V 108.7 . . ?
C118 C119 H11W 109.9 . . ?
C118 C119 H11X 109.9 . . ?
C118 C119 C120 109.1(12) . . ?
H11W C119 H11X 108.3 . . ?
C120 C119 H11W 109.9 . . ?
C120 C119 H11X 109.9 . . ?
C119 C120 H12A 108.7 . . ?
C119 C120 H12B 108.7 . . ?
H12A C120 H12B 107.6 . . ?
C121 C120 C119 114.1(14) . . ?
C121 C120 H12A 108.7 . . ?
C121 C120 H12B 108.7 . . ?
C120 C121 H12C 108.7 . . ?
C120 C121 H12D 108.7 . . ?
H12C C121 H12D 107.6 . . ?
C122 C121 C120 114.1(15) . . ?
C122 C121 H12C 108.7 . . ?
C122 C121 H12D 108.7 . . ?
C121 C122 H12E 108.6 . . ?
C121 C122 H12F 108.6 . . ?
H12E C122 H12F 107.6 . . ?
C123 C122 C121 114.6(18) . . ?
C123 C122 H12E 108.6 . . ?
C123 C122 H12F 108.6 . . ?
C122 C123 H12G 109.0 . . ?
C122 C123 H12H 109.0 . . ?
H12G C123 H12H 107.8 . . ?
C124 C123 C122 112.8(17) . . ?
C124 C123 H12G 109.0 . . ?
C124 C123 H12H 109.0 . . ?
C123 C124 H12I 110.9 . . ?
C123 C124 H12J 110.9 . . ?
C123 C124 C125 104.2(15) . . ?
H12I C124 H12J 108.9 . . ?
C125 C124 H12I 110.9 . . ?
C125 C124 H12J 110.9 . . ?
C124 C125 H12K 108.8 . . ?
C124 C125 H12L 108.8 . . ?
H12K C125 H12L 107.7 . . ?
C126 C125 C124 113.8(17) . . ?
C126 C125 H12K 108.8 . . ?
C126 C125 H12L 108.8 . . ?
C125 C126 H12M 109.5 . . ?
C125 C126 H12N 109.5 . . ?
C125 C126 C127 110.7(16) . . ?
H12M C126 H12N 108.1 . . ?
C127 C126 H12M 109.5 . . ?
C127 C126 H12N 109.5 . . ?
C126 C127 H12O 107.1 . . ?
C126 C127 H12P 107.1 . . ?
C126 C127 C128 121.0(14) . . ?
H12O C127 H12P 106.8 . . ?
C128 C127 H12O 107.1 . . ?
C128 C127 H12P 107.1 . . ?
C127 C128 H12Q 110.5 . . ?
C127 C128 H12R 110.5 . . ?
C127 C128 C129 106.0(11) . . ?
H12Q C128 H12R 108.7 . . ?
C129 C128 H12Q 110.5 . . ?
C129 C128 H12R 110.5 . . ?
C128 C129 H12S 111.4 . . ?
C128 C129 H12T 111.4 . . ?
H12S C129 H12T 109.3 . . ?
C130 C129 C128 101.6(9) . . ?
C130 C129 H12S 111.4 . . ?
C130 C129 H12T 111.4 . . ?
P3 C130 H13A 109.3 . . ?
P3 C130 H13B 109.3 . . ?
P3 C130 H13C 107.6 . . ?
P3 C130 H13D 107.6 . . ?
C129 C130 P3 111.7(6) . . ?
C129 C130 H13A 109.3 . . ?
C129 C130 H13B 109.3 . . ?
H13A C130 H13B 107.9 . . ?
H13C C130 H13D 107.1 . . ?
C229 C130 P3 118.7(7) . . ?
C229 C130 H13C 107.6 . . ?
C229 C130 H13D 107.6 . . ?
C210 C209 P2 108.7(6) . . ?
C211 C209 P2 109.5(7) . . ?
C211 C209 C210 109.3(7) . . ?
C212 C209 P2 109.4(7) . . ?
C212 C209 C210 110.0(8) . . ?
C212 C209 C211 110.0(8) . . ?
C209 C210 H21A 109.5 . . ?
C209 C210 H21B 109.5 . . ?
C209 C210 H21C 109.5 . . ?
H21A C210 H21B 109.5 . . ?
H21A C210 H21C 109.5 . . ?
H21B C210 H21C 109.5 . . ?
C209 C211 H21D 109.5 . . ?
C209 C211 H21E 109.5 . . ?
C209 C211 H21F 109.5 . . ?
H21D C211 H21E 109.5 . . ?
H21D C211 H21F 109.5 . . ?
H21E C211 H21F 109.5 . . ?
C209 C212 H21G 109.5 . . ?
C209 C212 H21H 109.5 . . ?
C209 C212 H21I 109.5 . . ?
H21G C212 H21H 109.5 . . ?
H21G C212 H21I 109.5 . . ?
H21H C212 H21I 109.5 . . ?
C113 C214 H21J 109.5 . . ?
C113 C214 H21K 109.5 . . ?
C113 C214 H21L 109.5 . . ?
H21J C214 H21K 109.5 . . ?
H21J C214 H21L 109.5 . . ?
H21K C214 H21L 109.5 . . ?
C113 C215 H21M 109.5 . . ?
C113 C215 H21N 109.5 . . ?
C113 C215 H21O 109.5 . . ?
H21M C215 H21N 109.5 . . ?
H21M C215 H21O 109.5 . . ?
H21N C215 H21O 109.5 . . ?
C113 C216 H21P 109.5 . . ?
C113 C216 H21Q 109.5 . . ?
C113 C216 H21R 109.5 . . ?
H21P C216 H21Q 109.5 . . ?
H21P C216 H21R 109.5 . . ?
H21Q C216 H21R 109.5 . . ?
P2 C217 H21S 109.3 . . ?
P2 C217 H21T 109.3 . . ?
H21S C217 H21T 107.9 . . ?
C218 C217 P2 111.7(10) . . ?
C218 C217 H21S 109.3 . . ?
C218 C217 H21T 109.3 . . ?
C217 C218 H21U 108.9 . . ?
C217 C218 H21V 108.9 . . ?
C217 C218 C219 113.3(14) . . ?
H21U C218 H21V 107.7 . . ?
C219 C218 H21U 108.9 . . ?
C219 C218 H21V 108.9 . . ?
C218 C219 H21W 112.6 . . ?
C218 C219 H21X 112.6 . . ?
C218 C219 C220 95.6(15) . . ?
H21W C219 H21X 110.1 . . ?
C220 C219 H21W 112.6 . . ?
C220 C219 H21X 112.6 . . ?
C219 C220 H22A 108.1 . . ?
C219 C220 H22B 108.1 . . ?
H22A C220 H22B 107.3 . . ?
C221 C220 C219 116.7(16) . . ?
C221 C220 H22A 108.1 . . ?
C221 C220 H22B 108.1 . . ?
C220 C221 H22C 110.3 . . ?
C220 C221 H22D 110.3 . . ?
C220 C221 C222 107.1(15) . . ?
H22C C221 H22D 108.5 . . ?
C222 C221 H22C 110.3 . . ?
C222 C221 H22D 110.3 . . ?
C221 C222 H22E 110.1 . . ?
C221 C222 H22F 110.1 . . ?
H22E C222 H22F 108.4 . . ?
C223 C222 C221 108.0(14) . . ?
C223 C222 H22E 110.1 . . ?
C223 C222 H22F 110.1 . . ?
C222 C223 H22G 107.7 . . ?
C222 C223 H22H 107.7 . . ?
C222 C223 C224 118.4(13) . . ?
H22G C223 H22H 107.1 . . ?
C224 C223 H22G 107.7 . . ?
C224 C223 H22H 107.7 . . ?
C223 C224 H22I 110.9 . . ?
C223 C224 H22J 110.9 . . ?
H22I C224 H22J 108.9 . . ?
C225 C224 C223 104.2(12) . . ?
C225 C224 H22I 110.9 . . ?
C225 C224 H22J 110.9 . . ?
C224 C225 H22K 110.0 . . ?
C224 C225 H22L 110.0 . . ?
C224 C225 C226 108.4(14) . . ?
H22K C225 H22L 108.4 . . ?
C226 C225 H22K 110.0 . . ?
C226 C225 H22L 110.0 . . ?
C225 C226 H22M 109.3 . . ?
C225 C226 H22N 109.3 . . ?
H22M C226 H22N 107.9 . . ?
C227 C226 C225 111.8(16) . . ?
C227 C226 H22M 109.3 . . ?
C227 C226 H22N 109.3 . . ?
C226 C227 H22O 108.8 . . ?
C226 C227 H22P 108.8 . . ?
C226 C227 C228 113.8(12) . . ?
H22O C227 H22P 107.7 . . ?
C228 C227 H22O 108.8 . . ?
C228 C227 H22P 108.8 . . ?
C227 C228 H22Q 107.8 . . ?
C227 C228 H22R 107.8 . . ?
H22Q C228 H22R 107.1 . . ?
C229 C228 C227 118.2(11) . . ?
C229 C228 H22Q 107.8 . . ?
C229 C228 H22R 107.8 . . ?
C130 C229 H22S 109.0 . . ?
C130 C229 H22T 109.0 . . ?
C228 C229 C130 113.1(10) . . ?
C228 C229 H22S 109.0 . . ?
C228 C229 H22T 109.0 . . ?
H22S C229 H22T 107.8 . . ?
P3 B3 H3A 109.5 . . ?
P3 B3 H3B 109.5 . . ?
P3 B3 H3C 109.5 . . ?
H3A B3 H3B 109.5 . . ?
H3A B3 H3C 109.5 . . ?
H3B B3 H3C 109.5 . . ?
P2 B2 H2A 109.5 . . ?
P2 B2 H2B 109.5 . . ?
P2 B2 H2C 109.5 . . ?
H2A B2 H2B 109.5 . . ?
H2A B2 H2C 109.5 . . ?
H2B B2 H2C 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
P2 O107 C102 C101 -141.5(5) . . . . ?
P2 O107 C102 C103 43.1(8) . . . . ?
P2 C117 C118 C119 -167.3(14) . . . . ?
P2 C217 C218 C219 -178.3(15) . . . . ?
P3 O108 C106 C101 111.4(4) . . . . ?
P3 O108 C106 C105 -72.0(6) . . . . ?
P3 C130 C229 C228 137.0(11) . . . . ?
O107 P2 C109 C110 70.0(7) . . . . ?
O107 P2 C109 C111 -170.9(7) . . . . ?
O107 P2 C109 C112 -50.2(7) . . . . ?
O107 P2 C117 C118 -49.3(14) . . . . ?
O107 P2 C209 C210 69.4(7) . . . . ?
O107 P2 C209 C211 -171.2(7) . . . . ?
O107 P2 C209 C212 -50.7(8) . . . . ?
O107 P2 C217 C218 -78.5(14) . . . . ?
O107 C102 C103 C104 174.4(6) . . . . ?
O108 P3 C113 C114 -79.3(7) . . . . ?
O108 P3 C113 C115 163.8(6) . . . . ?
O108 P3 C113 C116 44.7(6) . . . . ?
O108 P3 C113 C214 -51.8(5) . . . . ?
O108 P3 C113 C215 -170.7(6) . . . . ?
O108 P3 C113 C216 66.0(6) . . . . ?
O108 P3 C130 C129 75.8(7) . . . . ?
O108 P3 C130 C229 48.5(8) . . . . ?
C101 C102 C103 C104 -0.7(9) . . . . ?
C102 C101 C106 O108 177.1(4) . . . . ?
C102 C101 C106 C105 0.5(7) . . . . ?
C102 C103 C104 C105 0.9(10) . . . . ?
C103 C104 C105 C106 -0.4(10) . . . . ?
C104 C105 C106 O108 -176.8(5) . . . . ?
C104 C105 C106 C101 -0.3(8) . . . . ?
C106 C101 C102 O107 -175.4(4) . . . . ?
C106 C101 C102 C103 0.0(8) . . . . ?
C109 P2 O107 C102 -144.9(6) . . . . ?
C109 P2 C117 C118 -152.8(13) . . . . ?
C113 P3 O108 C106 130.4(4) . . . . ?
C113 P3 C130 C129 -176.8(7) . . . . ?
C113 P3 C130 C229 155.9(8) . . . . ?
C117 P2 O107 C102 107.0(7) . . . . ?
C117 P2 C109 C110 171.2(8) . . . . ?
C117 P2 C109 C111 -69.7(9) . . . . ?
C117 P2 C109 C112 50.9(9) . . . . ?
C117 C118 C119 C120 -172.4(16) . . . . ?
C118 C119 C120 C121 -167.8(17) . . . . ?
C119 C120 C121 C122 -65(2) . . . . ?
C120 C121 C122 C123 -62(2) . . . . ?
C121 C122 C123 C124 -44(3) . . . . ?
C122 C123 C124 C125 174.4(18) . . . . ?
C123 C124 C125 C126 -157.3(19) . . . . ?
C124 C125 C126 C127 53(2) . . . . ?
C125 C126 C127 C128 57(2) . . . . ?
C126 C127 C128 C129 -163.5(15) . . . . ?
C127 C128 C129 C130 -87.5(13) . . . . ?
C128 C129 C130 P3 -163.1(7) . . . . ?
C130 P3 O108 C106 -118.0(4) . . . . ?
C130 P3 C113 C114 173.0(7) . . . . ?
C130 P3 C113 C115 56.1(6) . . . . ?
C130 P3 C113 C116 -63.0(7) . . . . ?
C130 P3 C113 C214 -159.5(6) . . . . ?
C130 P3 C113 C215 81.5(7) . . . . ?
C130 P3 C113 C216 -41.7(7) . . . . ?
C209 P2 O107 C102 -124.4(6) . . . . ?
C209 P2 C217 C218 179.4(13) . . . . ?
C217 P2 O107 C102 129.7(8) . . . . ?
C217 P2 C209 C210 178.8(9) . . . . ?
C217 P2 C209 C211 -61.8(10) . . . . ?
C217 P2 C209 C212 58.8(10) . . . . ?
C217 C218 C219 C220 129.2(19) . . . . ?
C218 C219 C220 C221 153(2) . . . . ?
C219 C220 C221 C222 9(3) . . . . ?
C220 C221 C222 C223 -140.0(18) . . . . ?
C221 C222 C223 C224 79.2(19) . . . . ?
C222 C223 C224 C225 66(2) . . . . ?
C223 C224 C225 C226 -177.9(15) . . . . ?
C224 C225 C226 C227 84(2) . . . . ?
C225 C226 C227 C228 169.3(15) . . . . ?
C226 C227 C228 C229 -147.8(16) . . . . ?
C227 C228 C229 C130 -152.8(14) . . . . ?
B3 P3 O108 C106 4.9(5) . . . . ?
B3 P3 C113 C114 46.6(7) . . . . ?
B3 P3 C113 C115 -70.3(6) . . . . ?
B3 P3 C113 C116 170.7(6) . . . . ?
B3 P3 C113 C214 74.1(6) . . . . ?
B3 P3 C113 C215 -44.8(7) . . . . ?
B3 P3 C113 C216 -168.0(7) . . . . ?
B3 P3 C130 C129 -49.1(8) . . . . ?
B3 P3 C130 C229 -76.3(9) . . . . ?
B2 P2 O107 C102 -7.3(8) . . . . ?
B2 P2 C109 C110 -66.2(8) . . . . ?
B2 P2 C109 C111 52.9(8) . . . . ?
B2 P2 C109 C112 173.6(7) . . . . ?
B2 P2 C117 C118 75.0(15) . . . . ?
B2 P2 C209 C210 -55.9(8) . . . . ?
B2 P2 C209 C211 63.5(8) . . . . ?
B2 P2 C209 C212 -175.9(8) . . . . ?
B2 P2 C217 C218 59.7(16) . . . . ?

_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 1.713
_oxdiff_exptl_absorpt_empirical_full_min 0.722
####################################################################### 
# 
# 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_0471abc19s
_database_code_depnum_ccdc_archive 'CCDC 1972816'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# [Rh(POCOP-14)Cl2(CO)]
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT301_0471abc19s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        11% Note 
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================


_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C29 H49 Cl2 O3 P2 Rh'
_chemical_formula_sum            'C29 H49 Cl2 O3 P2 Rh'
_chemical_formula_weight         681.43
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Cl Cl 0.3639 0.7018 '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'
Rh Rh 0.0927 3.6045 '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                   12.40495(16)
_cell_length_b                   13.12123(13)
_cell_length_c                   39.3620(5)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6406.88(13)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    18605
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.3900
_cell_measurement_theta_min      4.1820
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    7.004
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.448
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.413
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             2848
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
6 -6 3 0.0732
-6 -6 -1 0.0342
-6 6 -3 0.0684
6 6 1 0.0523
0 0 -26 0.0077
-6 6 3 0.0671
0 0 26 0.0124

_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 293 K'
_exptl_crystal_size_max          0.146
_exptl_crystal_size_mid          0.089
_exptl_crystal_size_min          0.023
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
5.5396 -6.0866 3.3239 0.0052 0.0074 1.0000
-5.7772 -5.9309 -0.7158 0.8950 -0.4461 -0.0014
-5.6193 6.0036 -3.3335 0.0072 -0.0136 -0.9999
5.5721 6.1481 0.5946 -0.8946 0.4455 -0.0350
0.2335 0.0807 -25.5226 0.4436 0.8874 -0.1254
-5.6366 5.9791 3.4084 -0.1130 -0.2458 -0.9627
-0.0482 -0.3853 25.6085 -0.4351 -0.8892 0.1671

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       48
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            54793
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.068
_diffrn_reflns_theta_max         70.068
_diffrn_reflns_theta_min         6.660
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_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    -66.00  33.00   1.00    6.00    --  -41.82  37.00 -30.00   99
  2  ω     23.00  98.00   1.00    6.00    --   41.82-125.00 -60.00   75
  3  ω     72.00 118.00   1.00    6.00    --   41.82 160.00-102.00   46
  4  ω     94.00 178.00   1.00   24.00    --  107.00 125.00   0.00   84
  5  ω     34.00 118.00   1.00   24.00    --  107.00-125.00  60.00   84
  6  ω     94.00 178.00   1.00   24.00    --  107.00 125.00 -90.00   84
  7  ω     94.00 178.00   1.00   24.00    --  107.00 125.00 120.00   84
  8  ω     34.00 133.00   1.00   24.00    --  107.00 -45.00 150.00   99
  9  ω     35.00 136.00   1.00   24.00    --  107.00 -61.00   0.00  101
 10  ω     24.00 110.00   1.00   24.00    --  107.00 -94.00 -90.00   86
 11  ω   -114.00 -13.00   1.00    6.00    --  -41.82 -59.00  90.00  101
 12  ω   -114.00 -14.00   1.00    6.00    --  -41.82 -57.00 -30.00  100
 13  ω   -114.00 -14.00   1.00    6.00    --  -41.82 -57.00-150.00  100
 14  ω     81.00 178.00   1.00   24.00    --  107.00  45.00 -30.00   97
 15  ω     81.00 178.00   1.00   24.00    --  107.00  45.00  90.00   97
 16  ω     81.00 171.00   1.00   24.00    --  107.00  45.00  30.00   90
 17  ω     81.00 178.00   1.00   24.00    --  107.00  45.00 150.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0731563000
_diffrn_orient_matrix_UB_12      -0.0774331000
_diffrn_orient_matrix_UB_13      -0.0182936000
_diffrn_orient_matrix_UB_21      0.0526707000
_diffrn_orient_matrix_UB_22      0.0280389000
_diffrn_orient_matrix_UB_23      -0.0341999000
_diffrn_orient_matrix_UB_31      0.0853942000
_diffrn_orient_matrix_UB_32      -0.0836048000
_diffrn_orient_matrix_UB_33      0.0054285000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                5477
_reflns_number_total             6061
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.795
_refine_diff_density_min         -1.028
_refine_diff_density_rms         0.097
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.267
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6061
_refine_ls_number_restraints     258
_refine_ls_R_factor_all          0.0564
_refine_ls_R_factor_gt           0.0514
_refine_ls_restrained_S_all      1.253
_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)+34.5544P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1078
_refine_ls_wR_factor_ref         0.1100
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C219-C118 \\sim C119-C118 \\sim C220-C219 \\sim C120-C119 \\sim C220-C121
\\sim C121-C120 \\sim C122-
 C121 \\sim C222-C121 \\sim C123-C122 \\sim C223-C222 \\sim C223-C124 \\sim
C124-C123
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim
C219 \\sim C220 \\sim C222 \\sim C223: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C220) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C219) \\sim Ueq, Uanis(C223) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
4. Others
 Sof(H11W)=Sof(H11X)=Sof(H12E)=Sof(H12F)=Sof(H12M)=Sof(H12N)=Sof(C219)=
 Sof(H21A)=Sof(H21B)=Sof(C220)=Sof(H22A)=Sof(H22B)=Sof(C222)=Sof(H22C)=
 Sof(H22D)=Sof(C223)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H11U)=Sof(H11V)=Sof(C119)=Sof(H11Y)=Sof(H)=Sof(C120)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(H12D)=Sof(C122)=Sof(H12G)=Sof(H12H)=Sof(C123)=Sof(H12I)=
 Sof(H12J)=Sof(H12K)=Sof(H12L)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C118(H11W,H11X), C119(H11Y,H), C120(H12A,
 H12B), C121(H12C,H12D), C121(H12E,H12F), C122(H12G,H12H), C123(H12I,H12J),
 C124(H12K,H12L), C124(H12M,H12N), C125(H12O,H12P), C126(H12Q,H12R), C127(H12S,
 H12T), C128(H12U,H12V), C129(H12W,H12X), C130(H13A,H13B), C219(H21A,H21B),
 C220(H22A,H22B), C222(H22C,H22D), C223(H22E,H22F)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
5.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Rh1 Rh 0.54801(3) 0.72002(3) 0.39629(2) 0.01853(10) Uani 1 1 d . . . . .
Cl6 Cl 0.44837(10) 0.59341(10) 0.42515(3) 0.0317(3) Uani 1 1 d . . . . .
Cl7 Cl 0.64699(10) 0.83940(10) 0.36445(3) 0.0311(3) Uani 1 1 d . . . . .
P2 P 0.64694(10) 0.77662(10) 0.44302(3) 0.0254(3) Uani 1 1 d . . . . .
P3 P 0.40372(9) 0.71763(9) 0.35658(3) 0.0201(2) Uani 1 1 d . . . . .
O5 O 0.7042(4) 0.5476(3) 0.37645(11) 0.0469(11) Uani 1 1 d . . . . .
O107 O 0.5858(3) 0.8830(3) 0.45389(10) 0.0376(9) Uani 1 1 d . . . . .
O108 O 0.3069(3) 0.7705(3) 0.37905(8) 0.0255(7) Uani 1 1 d . . . . .
C4 C 0.6488(4) 0.6095(4) 0.38200(13) 0.0285(11) Uani 1 1 d . . . . .
C101 C 0.4484(4) 0.8274(4) 0.41532(12) 0.0249(10) Uani 1 1 d . . . . .
C102 C 0.4823(4) 0.8954(4) 0.44056(13) 0.0300(11) Uani 1 1 d . . . . .
C103 C 0.4166(5) 0.9723(4) 0.45298(14) 0.0366(13) Uani 1 1 d . . . . .
H103 H 0.4416 1.0176 0.4701 0.044 Uiso 1 1 calc R . . . .
C104 C 0.3138(5) 0.9814(4) 0.43987(13) 0.0347(13) Uani 1 1 d . . . . .
H104 H 0.2684 1.0348 0.4476 0.042 Uiso 1 1 calc R . . . .
C105 C 0.2758(4) 0.9138(4) 0.41564(12) 0.0299(11) Uani 1 1 d . . . . .
H105 H 0.2043 0.9194 0.4072 0.036 Uiso 1 1 calc R . . . .
C106 C 0.3444(4) 0.8378(4) 0.40392(11) 0.0253(10) Uani 1 1 d . . . . .
C109 C 0.6530(4) 0.7041(4) 0.48345(13) 0.0302(11) Uani 1 1 d . . . . .
C110 C 0.5406(5) 0.7045(5) 0.49957(15) 0.0430(15) Uani 1 1 d . . . . .
H11A H 0.5207 0.7745 0.5056 0.065 Uiso 1 1 calc GR . . . .
H11B H 0.5411 0.6621 0.5201 0.065 Uiso 1 1 calc GR . . . .
H11C H 0.4881 0.6772 0.4833 0.065 Uiso 1 1 calc GR . . . .
C111 C 0.6882(5) 0.5948(4) 0.47583(14) 0.0341(12) Uani 1 1 d . . . . .
H11D H 0.6370 0.5635 0.4600 0.051 Uiso 1 1 calc GR . . . .
H11E H 0.6899 0.5555 0.4970 0.051 Uiso 1 1 calc GR . . . .
H11F H 0.7602 0.5954 0.4656 0.051 Uiso 1 1 calc GR . . . .
C112 C 0.7322(5) 0.7554(5) 0.50797(14) 0.0399(14) Uani 1 1 d . . . . .
H11G H 0.8061 0.7459 0.4997 0.060 Uiso 1 1 calc GR . . . .
H11H H 0.7252 0.7246 0.5305 0.060 Uiso 1 1 calc GR . . . .
H11I H 0.7161 0.8284 0.5094 0.060 Uiso 1 1 calc GR . . . .
C113 C 0.3969(4) 0.7992(4) 0.31744(12) 0.0248(10) Uani 1 1 d . . . . .
C114 C 0.4024(5) 0.9107(4) 0.32843(13) 0.0310(11) Uani 1 1 d . . . . .
H11J H 0.3381 0.9277 0.3417 0.047 Uiso 1 1 calc GR . . . .
H11K H 0.4056 0.9544 0.3083 0.047 Uiso 1 1 calc GR . . . .
H11L H 0.4669 0.9215 0.3423 0.047 Uiso 1 1 calc GR . . . .
C115 C 0.4899(5) 0.7756(4) 0.29291(13) 0.0352(12) Uani 1 1 d . . . . .
H11M H 0.5588 0.7839 0.3048 0.053 Uiso 1 1 calc GR . . . .
H11N H 0.4869 0.8225 0.2736 0.053 Uiso 1 1 calc GR . . . .
H11O H 0.4833 0.7053 0.2848 0.053 Uiso 1 1 calc GR . . . .
C116 C 0.2872(5) 0.7818(4) 0.30004(14) 0.0371(13) Uani 1 1 d . . . . .
H11P H 0.2850 0.7130 0.2904 0.056 Uiso 1 1 calc GR . . . .
H11Q H 0.2774 0.8320 0.2819 0.056 Uiso 1 1 calc GR . . . .
H11R H 0.2293 0.7893 0.3168 0.056 Uiso 1 1 calc GR . . . .
C117 C 0.7811(4) 0.8246(4) 0.43457(14) 0.0338(12) Uani 1 1 d . . . . .
H11S H 0.7753 0.8806 0.4178 0.041 Uiso 1 1 calc R . . . .
H11T H 0.8099 0.8543 0.4558 0.041 Uiso 1 1 calc R . . . .
C118 C 0.8612(4) 0.7480(5) 0.42142(15) 0.0392(13) Uani 1 1 d D U . . .
H11U H 0.8248 0.6984 0.4063 0.047 Uiso 0.759(7) 1 calc R . P A 1
H11V H 0.8940 0.7103 0.4406 0.047 Uiso 0.759(7) 1 calc R . P A 1
H11W H 0.8257 0.7157 0.4016 0.047 Uiso 0.241(7) 1 calc R . P A 2
H11X H 0.8653 0.6947 0.4392 0.047 Uiso 0.241(7) 1 calc R . P A 2
C119 C 0.9487(6) 0.8060(5) 0.40163(19) 0.0358(16) Uani 0.759(7) 1 d D U P A 1
H11Y H 0.9148 0.8450 0.3829 0.043 Uiso 0.759(7) 1 calc R . P A 1
H H 0.9849 0.8550 0.4170 0.043 Uiso 0.759(7) 1 calc R . P A 1
C120 C 1.0325(6) 0.7322(6) 0.38690(19) 0.0411(17) Uani 0.759(7) 1 d D U P A 1
H12A H 1.0942 0.7727 0.3784 0.049 Uiso 0.759(7) 1 calc R . P A 1
H12B H 1.0596 0.6886 0.4056 0.049 Uiso 0.759(7) 1 calc R . P A 1
C121 C 0.9927(5) 0.6631(5) 0.35813(15) 0.0477(14) Uani 1 1 d D U . . .
H12C H 1.0557 0.6270 0.3484 0.057 Uiso 0.759(7) 1 calc R . P A 1
H12D H 0.9444 0.6109 0.3680 0.057 Uiso 0.759(7) 1 calc R . P A 1
H12E H 0.9283 0.6229 0.3646 0.057 Uiso 0.241(7) 1 calc R . P A 2
H12F H 1.0587 0.6277 0.3659 0.057 Uiso 0.241(7) 1 calc R . P A 2
C122 C 0.9330(7) 0.7157(6) 0.32928(16) 0.0428(16) Uani 0.759(7) 1 d D U P A 1
H12G H 0.9660 0.7833 0.3251 0.051 Uiso 0.759(7) 1 calc R . P A 1
H12H H 0.8571 0.7268 0.3361 0.051 Uiso 0.759(7) 1 calc R . P A 1
C123 C 0.9358(8) 0.6534(6) 0.2963(2) 0.0485(19) Uani 0.759(7) 1 d D U P A 1
H12I H 0.9142 0.6984 0.2772 0.058 Uiso 0.759(7) 1 calc R . P A 1
H12J H 1.0110 0.6315 0.2921 0.058 Uiso 0.759(7) 1 calc R . P A 1
C124 C 0.8633(6) 0.5590(5) 0.29590(17) 0.0522(16) Uani 1 1 d D U . . .
H12K H 0.8915 0.5126 0.2782 0.063 Uiso 0.759(7) 1 calc R . P A 1
H12L H 0.8729 0.5240 0.3180 0.063 Uiso 0.759(7) 1 calc R . P A 1
H12M H 0.9004 0.5271 0.2763 0.063 Uiso 0.241(7) 1 calc R . P A 2
H12N H 0.8796 0.5206 0.3169 0.063 Uiso 0.241(7) 1 calc R . P A 2
C125 C 0.7441(6) 0.5701(5) 0.29002(16) 0.0487(16) Uani 1 1 d . . . . .
H12O H 0.7323 0.6047 0.2680 0.058 Uiso 1 1 calc R . . . .
H12P H 0.7134 0.6140 0.3080 0.058 Uiso 1 1 calc R . . . .
C126 C 0.6842(5) 0.4682(5) 0.28985(15) 0.0446(15) Uani 1 1 d . . . . .
H12Q H 0.7113 0.4268 0.2706 0.053 Uiso 1 1 calc R . . . .
H12R H 0.7018 0.4312 0.3111 0.053 Uiso 1 1 calc R . . . .
C127 C 0.5616(5) 0.4763(5) 0.28692(14) 0.0419(14) Uani 1 1 d . . . . .
H12S H 0.5435 0.5198 0.2672 0.050 Uiso 1 1 calc R . . . .
H12T H 0.5314 0.4076 0.2827 0.050 Uiso 1 1 calc R . . . .
C128 C 0.5092(5) 0.5207(4) 0.31861(13) 0.0322(12) Uani 1 1 d . . . . .
H12U H 0.5230 0.4741 0.3379 0.039 Uiso 1 1 calc R . . . .
H12V H 0.5443 0.5866 0.3239 0.039 Uiso 1 1 calc R . . . .
C129 C 0.3892(5) 0.5378(4) 0.31582(14) 0.0347(12) Uani 1 1 d . . . . .
H12W H 0.3530 0.4708 0.3141 0.042 Uiso 1 1 calc R . . . .
H12X H 0.3743 0.5757 0.2946 0.042 Uiso 1 1 calc R . . . .
C130 C 0.3404(4) 0.5966(4) 0.34572(13) 0.0296(11) Uani 1 1 d . . . . .
H13A H 0.3429 0.5522 0.3660 0.036 Uiso 1 1 calc R . . . .
H13B H 0.2636 0.6098 0.3406 0.036 Uiso 1 1 calc R . . . .
C219 C 0.9788(9) 0.766(2) 0.4102(5) 0.040(3) Uani 0.241(7) 1 d D U P A 2
H21A H 1.0056 0.8303 0.4205 0.048 Uiso 0.241(7) 1 calc R . P A 2
H21B H 1.0246 0.7097 0.4184 0.048 Uiso 0.241(7) 1 calc R . P A 2
C220 C 0.987(2) 0.7734(9) 0.3714(5) 0.041(3) Uani 0.241(7) 1 d D U P A 2
H22A H 1.0522 0.8118 0.3647 0.049 Uiso 0.241(7) 1 calc R . P A 2
H22B H 0.9228 0.8086 0.3619 0.049 Uiso 0.241(7) 1 calc R . P A 2
C222 C 0.996(2) 0.687(2) 0.3196(3) 0.051(3) Uani 0.241(7) 1 d D U P A 2
H22C H 1.0202 0.7579 0.3167 0.061 Uiso 0.241(7) 1 calc R . P A 2
H22D H 1.0512 0.6423 0.3091 0.061 Uiso 0.241(7) 1 calc R . P A 2
C223 C 0.891(2) 0.6732(8) 0.2993(8) 0.047(3) Uani 0.241(7) 1 d D U P A 2
H22E H 0.8987 0.7038 0.2765 0.057 Uiso 0.241(7) 1 calc R . P A 2
H22F H 0.8309 0.7089 0.3111 0.057 Uiso 0.241(7) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Cl6 2.3616(12) . ?
Rh1 Cl7 2.3521(12) . ?
Rh1 P2 2.3324(12) . ?
Rh1 P3 2.3768(11) . ?
Rh1 C4 1.996(6) . ?
Rh1 C101 2.018(5) . ?
P2 O107 1.646(4) . ?
P2 C109 1.856(5) . ?
P2 C117 1.810(5) . ?
P3 O108 1.645(3) . ?
P3 C113 1.877(5) . ?
P3 C130 1.822(5) . ?
O5 C4 1.086(7) . ?
O107 C102 1.397(6) . ?
O108 C106 1.398(6) . ?
C101 C102 1.400(7) . ?
C101 C106 1.373(7) . ?
C102 C103 1.387(7) . ?
C103 C104 1.380(8) . ?
C104 C105 1.385(8) . ?
C105 C106 1.391(7) . ?
C109 C110 1.532(7) . ?
C109 C111 1.528(7) . ?
C109 C112 1.533(7) . ?
C113 C114 1.527(7) . ?
C113 C115 1.535(7) . ?
C113 C116 1.542(7) . ?
C117 C118 1.506(8) . ?
C118 C119 1.537(6) . ?
C118 C219 1.542(8) . ?
C119 C120 1.534(6) . ?
C120 C121 1.533(6) . ?
C121 C122 1.521(6) . ?
C121 C220 1.540(8) . ?
C121 C222 1.549(8) . ?
C122 C123 1.536(7) . ?
C123 C124 1.530(7) . ?
C124 C125 1.504(10) . ?
C124 C223 1.542(8) . ?
C125 C126 1.531(9) . ?
C126 C127 1.529(9) . ?
C127 C128 1.522(7) . ?
C128 C129 1.509(8) . ?
C129 C130 1.532(7) . ?
C219 C220 1.536(8) . ?
C222 C223 1.540(8) . ?

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
Cl6 Rh1 P3 85.00(4) . . ?
Cl7 Rh1 Cl6 176.32(5) . . ?
Cl7 Rh1 P3 92.94(4) . . ?
P2 Rh1 Cl6 96.90(5) . . ?
P2 Rh1 Cl7 86.19(5) . . ?
P2 Rh1 P3 156.80(5) . . ?
C4 Rh1 Cl6 87.24(15) . . ?
C4 Rh1 Cl7 90.40(15) . . ?
C4 Rh1 P2 97.14(15) . . ?
C4 Rh1 P3 106.06(15) . . ?
C4 Rh1 C101 174.6(2) . . ?
C101 Rh1 Cl6 89.56(14) . . ?
C101 Rh1 Cl7 92.99(14) . . ?
C101 Rh1 P2 78.88(14) . . ?
C101 Rh1 P3 78.01(14) . . ?
O107 P2 Rh1 103.46(14) . . ?
O107 P2 C109 103.4(2) . . ?
O107 P2 C117 100.1(2) . . ?
C109 P2 Rh1 122.30(18) . . ?
C117 P2 Rh1 116.71(18) . . ?
C117 P2 C109 107.4(2) . . ?
O108 P3 Rh1 100.99(12) . . ?
O108 P3 C113 99.7(2) . . ?
O108 P3 C130 100.3(2) . . ?
C113 P3 Rh1 124.46(17) . . ?
C130 P3 Rh1 119.36(18) . . ?
C130 P3 C113 106.6(2) . . ?
C102 O107 P2 115.1(3) . . ?
C106 O108 P3 113.6(3) . . ?
O5 C4 Rh1 175.2(5) . . ?
C102 C101 Rh1 121.6(4) . . ?
C106 C101 Rh1 121.6(4) . . ?
C106 C101 C102 116.8(5) . . ?
O107 C102 C101 118.0(5) . . ?
C103 C102 O107 119.5(5) . . ?
C103 C102 C101 122.5(5) . . ?
C104 C103 C102 118.3(5) . . ?
C103 C104 C105 121.1(5) . . ?
C104 C105 C106 118.6(5) . . ?
C101 C106 O108 118.6(4) . . ?
C101 C106 C105 122.6(5) . . ?
C105 C106 O108 118.8(4) . . ?
C110 C109 P2 108.4(4) . . ?
C110 C109 C112 108.7(5) . . ?
C111 C109 P2 108.9(3) . . ?
C111 C109 C110 110.1(5) . . ?
C111 C109 C112 110.6(5) . . ?
C112 C109 P2 109.9(4) . . ?
C114 C113 P3 108.2(3) . . ?
C114 C113 C115 109.8(4) . . ?
C114 C113 C116 107.8(4) . . ?
C115 C113 P3 111.6(3) . . ?
C115 C113 C116 110.7(4) . . ?
C116 C113 P3 108.7(4) . . ?
C118 C117 P2 116.0(4) . . ?
C117 C118 C119 108.1(5) . . ?
C117 C118 C219 128.2(12) . . ?
C120 C119 C118 111.0(6) . . ?
C121 C120 C119 115.7(6) . . ?
C122 C121 C120 116.1(6) . . ?
C220 C121 C222 98.4(14) . . ?
C121 C122 C123 112.3(7) . . ?
C124 C123 C122 115.2(6) . . ?
C125 C124 C123 120.0(7) . . ?
C125 C124 C223 97.7(10) . . ?
C124 C125 C126 113.2(5) . . ?
C127 C126 C125 115.0(5) . . ?
C128 C127 C126 112.9(5) . . ?
C129 C128 C127 114.7(5) . . ?
C128 C129 C130 114.1(4) . . ?
C129 C130 P3 116.7(4) . . ?
C220 C219 C118 110.8(14) . . ?
C219 C220 C121 106.4(15) . . ?
C223 C222 C121 117.6(18) . . ?
C222 C223 C124 109.9(17) . . ?

_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 48.321
_oxdiff_exptl_absorpt_empirical_full_min 0.472
####################################################################### 
# 
# 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_0553abc19s
_database_code_depnum_ccdc_archive 'CCDC 1972813'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
#====================================================================

_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C31 H53 O P2 Rh'
_chemical_formula_sum            'C31 H53 O P2 Rh'
_chemical_formula_weight         606.58
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Rh Rh 0.0927 3.6045 '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                   10.93786(5)
_cell_length_b                   13.59304(6)
_cell_length_c                   20.93330(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3112.34(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    23122
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4310
_cell_measurement_theta_min      3.1940
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    5.550
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.234
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.295
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-2 8 6 0.0702
-1 -8 7 0.1065
1 7 -8 0.1185
2 -6 -9 0.1326
6 0 6 0.1151
-1 -2 13 0.1412
0 2 -13 0.1468
-6 0 -7 0.1379
-6 -2 6 0.2065
6 4 3 0.0986
3 2 -12 0.1586
0 -5 -11 0.1125
-3 -8 4 0.1208
1 7 8 0.0848
4 -5 8 0.1075
6 -4 1 0.1462

_exptl_crystal_recrystallization_method 'Crystals grown from TMS at 293 K'
_exptl_crystal_size_max          0.355
_exptl_crystal_size_mid          0.269
_exptl_crystal_size_min          0.216
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
-1.6374 7.7274 5.7625 -0.4448 0.8591 0.2532
-0.6179 -7.5165 7.0251 0.3329 -0.6250 0.7061
0.8772 6.9353 -8.2363 -0.2933 0.5474 -0.7838
2.0775 -6.0467 -9.0586 0.3840 -0.7481 -0.5411
6.2282 0.4395 6.4866 0.8746 0.4538 0.1706
-0.7802 -1.9771 13.1562 0.1728 0.0799 0.9817
-0.0829 1.8117 -13.2957 -0.2786 -0.1353 -0.9508
-6.2138 -0.4586 -6.5340 -0.8727 -0.4563 -0.1739
-6.1491 -2.0262 6.0323 -0.6171 -0.3142 0.7215
6.2394 3.6734 3.1680 0.6945 0.7052 -0.1428
2.9086 2.4640 -11.7989 0.0998 0.0891 -0.9910
-0.0813 -5.3766 -10.7690 0.0547 -0.8087 -0.5857
-2.6008 -7.8300 3.8154 0.0449 -0.8144 0.5785
0.7690 6.8355 8.4628 -0.0603 0.9307 0.3608
4.1948 -4.8478 8.0312 0.8544 -0.1321 0.5025
6.1863 -4.2375 1.3789 0.9879 -0.1470 -0.0500

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0335
_diffrn_reflns_av_unetI/netI     0.0230
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            26942
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        70.067
_diffrn_reflns_theta_max         70.067
_diffrn_reflns_theta_min         6.513
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00 -30.00  100
  2  ω     27.00  98.00   1.00    1.00    --   41.82-125.00 150.00   71
  3  ω     14.00 115.00   1.00    1.00    --   41.82  57.00-150.00  101
  4  ω     34.00 112.00   1.00    1.50    --  107.00-125.00  60.00   78
  5  ω     34.00 112.00   1.00    1.50    --  107.00-125.00   0.00   78
  6  ω     24.00 107.00   1.00    1.50    --  107.00 -94.00 150.00   83
  7  ω     31.00 140.00   1.00    1.50    --  107.00 -77.00 -60.00  109
  8  ω    103.00 178.00   1.00    1.50    --  107.00  77.00 -30.00   75
  9  ω     34.00 133.00   1.00    1.50    --  107.00 -45.00 150.00   99
 10  ω    -66.00  33.00   1.00    1.00    --  -41.82  37.00   0.00   99
 11  ω   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00  60.00   99
 12  ω   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00-120.00   99
 13  ω     81.00 178.00   1.00    1.50    --  107.00  45.00  60.00   97
 14  ω     81.00 178.00   1.00    1.50    --  107.00  45.00 150.00   97
 15  ω     78.00 171.00   1.00    1.50    --  107.00  61.00 -60.00   93
 16  ω     81.00 178.00   1.00    1.50    --  107.00  45.00-120.00   97
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.1282018000
_diffrn_orient_matrix_UB_12      -0.0412366000
_diffrn_orient_matrix_UB_13      0.0145363000
_diffrn_orient_matrix_UB_21      0.0408380000
_diffrn_orient_matrix_UB_22      0.1020596000
_diffrn_orient_matrix_UB_23      0.0238290000
_diffrn_orient_matrix_UB_31      -0.0416566000
_diffrn_orient_matrix_UB_32      -0.0268599000
_diffrn_orient_matrix_UB_33      0.0681139000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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         0.766
_reflns_Friedel_fraction_full    0.985
_reflns_Friedel_fraction_max     0.985
_reflns_number_gt                5847
_reflns_number_total             5884
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.238
_refine_diff_density_min         -0.813
_refine_diff_density_rms         0.063
_refine_ls_abs_structure_details 
;
 Flack x determined using 2501 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.011(3)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.074
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         5884
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0194
_refine_ls_R_factor_gt           0.0189
_refine_ls_restrained_S_all      1.074
_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)+(0.0285P)²+0.4538P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0484
_refine_ls_wR_factor_ref         0.0486
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11S,H11T), C118(H11U,H11V), C119(H11W,
 H11X), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H),
 C124(H12I,H12J), C125(H12K,H12L), C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,
 H12R), C129(H12S,H12T), C130(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
2.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Rh1 Rh 0.60678(2) 0.37738(2) 0.29966(2) 0.01716(6) Uani 1 1 d . . . . .
P2 P 0.66409(6) 0.41510(4) 0.40170(3) 0.01831(13) Uani 1 1 d . . . . .
P3 P 0.49318(5) 0.36722(5) 0.20898(3) 0.01905(13) Uani 1 1 d . . . . .
O5 O 0.84955(19) 0.30771(15) 0.24901(11) 0.0347(5) Uani 1 1 d . . . . .
C4 C 0.7580(2) 0.33803(19) 0.26746(13) 0.0219(5) Uani 1 1 d . . . . .
C101 C 0.4329(2) 0.39887(18) 0.33773(13) 0.0213(5) Uani 1 1 d . . . . .
C102 C 0.4160(2) 0.43872(18) 0.39972(13) 0.0217(5) Uani 1 1 d . . . . .
C103 C 0.3002(3) 0.44612(19) 0.42670(13) 0.0254(6) Uani 1 1 d . . . . .
H103 H 0.2912 0.4715 0.4687 0.030 Uiso 1 1 calc R . . . .
C104 C 0.1976(3) 0.4167(2) 0.39274(14) 0.0295(6) Uani 1 1 d . . . . .
H104 H 0.1187 0.4221 0.4114 0.035 Uiso 1 1 calc R . . . .
C105 C 0.2105(2) 0.3793(2) 0.33154(13) 0.0293(6) Uani 1 1 d . . . . .
H105 H 0.1402 0.3599 0.3080 0.035 Uiso 1 1 calc R . . . .
C106 C 0.3263(2) 0.36997(19) 0.30432(12) 0.0240(5) Uani 1 1 d . . . . .
C107 C 0.5275(3) 0.47606(19) 0.43429(13) 0.0231(5) Uani 1 1 d . . . . .
H10A H 0.5203 0.4619 0.4805 0.028 Uiso 1 1 calc R . . . .
H10B H 0.5345 0.5482 0.4287 0.028 Uiso 1 1 calc R . . . .
C108 C 0.3415(3) 0.3297(2) 0.23735(13) 0.0270(6) Uani 1 1 d . . . . .
H10C H 0.2772 0.3564 0.2089 0.032 Uiso 1 1 calc R . . . .
H10D H 0.3348 0.2571 0.2377 0.032 Uiso 1 1 calc R . . . .
C109 C 0.6969(3) 0.31103(19) 0.45700(13) 0.0234(5) Uani 1 1 d . . . . .
C110 C 0.5800(3) 0.2497(2) 0.46296(15) 0.0307(6) Uani 1 1 d . . . . .
H11A H 0.5158 0.2894 0.4830 0.046 Uiso 1 1 calc GR . . . .
H11B H 0.5963 0.1916 0.4893 0.046 Uiso 1 1 calc GR . . . .
H11C H 0.5532 0.2289 0.4204 0.046 Uiso 1 1 calc GR . . . .
C111 C 0.7976(3) 0.2480(2) 0.42644(14) 0.0291(6) Uani 1 1 d . . . . .
H11D H 0.7698 0.2242 0.3847 0.044 Uiso 1 1 calc GR . . . .
H11E H 0.8157 0.1917 0.4542 0.044 Uiso 1 1 calc GR . . . .
H11F H 0.8716 0.2878 0.4209 0.044 Uiso 1 1 calc GR . . . .
C112 C 0.7384(3) 0.3454(2) 0.52346(13) 0.0324(7) Uani 1 1 d . . . . .
H11G H 0.8152 0.3821 0.5196 0.049 Uiso 1 1 calc GR . . . .
H11H H 0.7510 0.2880 0.5510 0.049 Uiso 1 1 calc GR . . . .
H11I H 0.6755 0.3880 0.5421 0.049 Uiso 1 1 calc GR . . . .
C113 C 0.4710(3) 0.4881(2) 0.16758(13) 0.0245(6) Uani 1 1 d . . . . .
C114 C 0.3942(3) 0.5559(2) 0.21081(14) 0.0319(6) Uani 1 1 d . . . . .
H11J H 0.3114 0.5292 0.2150 0.048 Uiso 1 1 calc GR . . . .
H11K H 0.3902 0.6218 0.1918 0.048 Uiso 1 1 calc GR . . . .
H11L H 0.4323 0.5600 0.2531 0.048 Uiso 1 1 calc GR . . . .
C115 C 0.5966(3) 0.5372(2) 0.15849(15) 0.0318(6) Uani 1 1 d . . . . .
H11M H 0.6377 0.5429 0.1999 0.048 Uiso 1 1 calc GR . . . .
H11N H 0.5855 0.6029 0.1401 0.048 Uiso 1 1 calc GR . . . .
H11O H 0.6466 0.4972 0.1296 0.048 Uiso 1 1 calc GR . . . .
C116 C 0.4073(3) 0.4750(2) 0.10294(13) 0.0309(6) Uani 1 1 d . . . . .
H11P H 0.4632 0.4427 0.0730 0.046 Uiso 1 1 calc GR . . . .
H11Q H 0.3840 0.5396 0.0860 0.046 Uiso 1 1 calc GR . . . .
H11R H 0.3340 0.4345 0.1084 0.046 Uiso 1 1 calc GR . . . .
C117 C 0.7864(3) 0.5048(2) 0.41835(14) 0.0265(6) Uani 1 1 d . . . . .
H11S H 0.7707 0.5356 0.4604 0.032 Uiso 1 1 calc R . . . .
H11T H 0.8653 0.4694 0.4212 0.032 Uiso 1 1 calc R . . . .
C118 C 0.7980(3) 0.5866(2) 0.36770(14) 0.0280(6) Uani 1 1 d . . . . .
H11U H 0.7186 0.5946 0.3456 0.034 Uiso 1 1 calc R . . . .
H11V H 0.8176 0.6495 0.3892 0.034 Uiso 1 1 calc R . . . .
C119 C 0.8969(3) 0.56374(19) 0.31850(13) 0.0273(6) Uani 1 1 d . . . . .
H11W H 0.9771 0.5618 0.3403 0.033 Uiso 1 1 calc R . . . .
H11X H 0.8814 0.4976 0.3004 0.033 Uiso 1 1 calc R . . . .
C120 C 0.9034(3) 0.63756(19) 0.26421(14) 0.0293(6) Uani 1 1 d . . . . .
H12A H 0.9215 0.7033 0.2822 0.035 Uiso 1 1 calc R . . . .
H12B H 0.8224 0.6411 0.2433 0.035 Uiso 1 1 calc R . . . .
C121 C 1.0000(3) 0.6130(2) 0.21363(14) 0.0309(6) Uani 1 1 d . . . . .
H12C H 0.9988 0.6645 0.1802 0.037 Uiso 1 1 calc R . . . .
H12D H 1.0818 0.6138 0.2339 0.037 Uiso 1 1 calc R . . . .
C122 C 0.9799(3) 0.5132(2) 0.18232(14) 0.0290(6) Uani 1 1 d . . . . .
H12E H 0.9980 0.4608 0.2138 0.035 Uiso 1 1 calc R . . . .
H12F H 0.8928 0.5071 0.1701 0.035 Uiso 1 1 calc R . . . .
C123 C 1.0586(3) 0.4972(2) 0.12356(14) 0.0274(6) Uani 1 1 d . . . . .
H12G H 1.1441 0.5152 0.1339 0.033 Uiso 1 1 calc R . . . .
H12H H 1.0302 0.5417 0.0892 0.033 Uiso 1 1 calc R . . . .
C124 C 1.0562(2) 0.3911(2) 0.09867(15) 0.0314(6) Uani 1 1 d . . . . .
H12I H 1.1110 0.3862 0.0612 0.038 Uiso 1 1 calc R . . . .
H12J H 1.0889 0.3470 0.1322 0.038 Uiso 1 1 calc R . . . .
C125 C 0.9302(3) 0.3558(2) 0.07973(14) 0.0275(6) Uani 1 1 d . . . . .
H12K H 0.9009 0.3965 0.0436 0.033 Uiso 1 1 calc R . . . .
H12L H 0.8739 0.3668 0.1161 0.033 Uiso 1 1 calc R . . . .
C126 C 0.9228(3) 0.2485(2) 0.06045(17) 0.0361(7) Uani 1 1 d . . . . .
H12M H 0.9401 0.2077 0.0986 0.043 Uiso 1 1 calc R . . . .
H12N H 0.9881 0.2353 0.0288 0.043 Uiso 1 1 calc R . . . .
C127 C 0.8007(3) 0.2151(2) 0.03192(15) 0.0329(7) Uani 1 1 d . . . . .
H12O H 0.8142 0.1521 0.0092 0.040 Uiso 1 1 calc R . . . .
H12P H 0.7750 0.2642 -0.0003 0.040 Uiso 1 1 calc R . . . .
C128 C 0.6952(3) 0.2008(2) 0.07928(15) 0.0327(6) Uani 1 1 d . . . . .
H12Q H 0.6272 0.1676 0.0567 0.039 Uiso 1 1 calc R . . . .
H12R H 0.7232 0.1561 0.1136 0.039 Uiso 1 1 calc R . . . .
C129 C 0.6457(3) 0.2937(2) 0.11001(13) 0.0252(6) Uani 1 1 d . . . . .
H12S H 0.6310 0.3436 0.0764 0.030 Uiso 1 1 calc R . . . .
H12T H 0.7078 0.3204 0.1397 0.030 Uiso 1 1 calc R . . . .
C130 C 0.5262(3) 0.2760(2) 0.14688(13) 0.0251(6) Uani 1 1 d . . . . .
H13A H 0.5301 0.2101 0.1670 0.030 Uiso 1 1 calc R . . . .
H13B H 0.4576 0.2754 0.1160 0.030 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 P2 2.2844(6) . ?
Rh1 P3 2.2731(6) . ?
Rh1 C4 1.865(3) . ?
Rh1 C101 2.083(3) . ?
P2 C107 1.839(3) . ?
P2 C109 1.863(3) . ?
P2 C117 1.844(3) . ?
P3 C108 1.835(3) . ?
P3 C113 1.873(3) . ?
P3 C130 1.832(3) . ?
O5 C4 1.150(3) . ?
C101 C102 1.418(4) . ?
C101 C106 1.415(4) . ?
C102 C103 1.391(4) . ?
C102 C107 1.506(4) . ?
C103 C104 1.387(4) . ?
C104 C105 1.386(4) . ?
C105 C106 1.395(4) . ?
C106 C108 1.514(4) . ?
C109 C110 1.531(4) . ?
C109 C111 1.535(4) . ?
C109 C112 1.536(4) . ?
C113 C114 1.541(4) . ?
C113 C115 1.540(4) . ?
C113 C116 1.532(4) . ?
C117 C118 1.541(4) . ?
C118 C119 1.526(4) . ?
C119 C120 1.518(4) . ?
C120 C121 1.533(4) . ?
C121 C122 1.523(4) . ?
C122 C123 1.517(4) . ?
C123 C124 1.533(4) . ?
C124 C125 1.513(4) . ?
C125 C126 1.515(4) . ?
C126 C127 1.532(4) . ?
C127 C128 1.534(4) . ?
C128 C129 1.517(4) . ?
C129 C130 1.536(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P3 Rh1 P2 160.83(2) . . ?
C4 Rh1 P2 99.15(8) . . ?
C4 Rh1 P3 99.53(8) . . ?
C4 Rh1 C101 171.38(10) . . ?
C101 Rh1 P2 82.03(8) . . ?
C101 Rh1 P3 80.15(8) . . ?
C107 P2 Rh1 103.00(9) . . ?
C107 P2 C109 105.56(12) . . ?
C107 P2 C117 102.78(13) . . ?
C109 P2 Rh1 117.61(9) . . ?
C117 P2 Rh1 121.62(10) . . ?
C117 P2 C109 104.19(13) . . ?
C108 P3 Rh1 103.94(9) . . ?
C108 P3 C113 106.03(13) . . ?
C113 P3 Rh1 113.83(9) . . ?
C130 P3 Rh1 121.73(10) . . ?
C130 P3 C108 102.70(13) . . ?
C130 P3 C113 106.91(13) . . ?
O5 C4 Rh1 175.5(2) . . ?
C102 C101 Rh1 121.52(19) . . ?
C106 C101 Rh1 121.61(19) . . ?
C106 C101 C102 116.8(2) . . ?
C101 C102 C107 117.6(2) . . ?
C103 C102 C101 121.2(3) . . ?
C103 C102 C107 121.2(2) . . ?
C104 C103 C102 120.5(3) . . ?
C105 C104 C103 119.8(3) . . ?
C104 C105 C106 120.2(3) . . ?
C101 C106 C108 117.9(2) . . ?
C105 C106 C101 121.4(2) . . ?
C105 C106 C108 120.7(2) . . ?
C102 C107 P2 109.13(17) . . ?
C106 C108 P3 107.34(18) . . ?
C110 C109 P2 107.65(18) . . ?
C110 C109 C111 109.2(2) . . ?
C110 C109 C112 109.8(2) . . ?
C111 C109 P2 107.66(19) . . ?
C111 C109 C112 109.6(2) . . ?
C112 C109 P2 112.88(19) . . ?
C114 C113 P3 108.90(19) . . ?
C115 C113 P3 108.79(19) . . ?
C115 C113 C114 107.4(2) . . ?
C116 C113 P3 111.49(19) . . ?
C116 C113 C114 109.9(2) . . ?
C116 C113 C115 110.3(2) . . ?
C118 C117 P2 114.0(2) . . ?
C119 C118 C117 112.1(2) . . ?
C120 C119 C118 113.9(2) . . ?
C119 C120 C121 113.9(2) . . ?
C122 C121 C120 113.1(2) . . ?
C123 C122 C121 113.3(2) . . ?
C122 C123 C124 113.6(2) . . ?
C125 C124 C123 113.8(2) . . ?
C124 C125 C126 115.1(2) . . ?
C125 C126 C127 115.8(3) . . ?
C126 C127 C128 116.2(3) . . ?
C129 C128 C127 115.9(2) . . ?
C128 C129 C130 112.7(2) . . ?
C129 C130 P3 114.70(18) . . ?

_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 7.330
_oxdiff_exptl_absorpt_empirical_full_min 0.708
####################################################################### 
# 
# 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_0423abc18s
_database_code_depnum_ccdc_archive 'CCDC 1972815'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# [Rh(PCP-14)Cl2(CO)]
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT301_0423abc18s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        16% Note 
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C31 H53 Cl2 O P2 Rh'
_chemical_formula_sum            'C31 H53 Cl2 O P2 Rh'
_chemical_formula_weight         677.48
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Cl Cl 0.3639 0.7018 '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'
Rh Rh 0.0927 3.6045 '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                   11.62738(6)
_cell_length_b                   11.80036(5)
_cell_length_c                   24.50061(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3361.66(3)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    22868
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4460
_cell_measurement_theta_min      3.5650
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    6.624
_exptl_absorpt_correction_T_max  0.876
_exptl_absorpt_correction_T_min  0.564
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.339
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
7 0 -3 0.0230
-2 2 15 0.0583
-7 -1 -4 0.0209
2 0 -15 0.0613
-2 7 6 0.0451
-2 -2 15 0.0650
0 -7 7 0.0561

_exptl_crystal_recrystallization_method 
'Crystals grown from CH2Cl2-hexane at 293 K'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.147
_exptl_crystal_size_min          0.069
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
7.4159 -0.3085 -2.8755 -0.2999 -0.8155 0.4951
-1.6364 2.0197 14.9477 -0.0481 -0.1024 -0.9936
-7.2370 -0.6676 -4.2980 0.3493 0.9360 -0.0442
2.3898 0.2700 -15.0739 -0.2651 0.0900 0.9600
-1.7242 6.8161 6.2801 -0.7071 0.2705 -0.6533
-2.1979 -1.6859 14.8055 0.4281 -0.1515 -0.8910
-0.3653 -6.9128 6.8082 0.9211 -0.3425 -0.1853

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            29314
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.065
_diffrn_reflns_theta_max         70.065
_diffrn_reflns_theta_min         6.451
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -116.00 -17.00   1.00    2.00    --  -41.82 -37.00-180.00   99
  2  ω    -92.00  -2.00   1.00    2.00    --  -41.82 125.00 -90.00   90
  3  ω     23.00  98.00   1.00    2.00    --   41.82-125.00-150.00   75
  4  ω     34.00 118.00   1.00    8.00    --  107.00-125.00-180.00   84
  5  ω     78.00 178.00   1.00    8.00    --  107.00  61.00   0.00  100
  6  ω     78.00 178.00   1.00    8.00    --  107.00  61.00  90.00  100
  7  ω     24.00 110.00   1.00    8.00    --  107.00 -94.00 120.00   86
  8  ω     34.00 118.00   1.00    8.00    --  107.00-125.00  60.00   84
  9  ω     24.00 110.00   1.00    8.00    --  107.00 -94.00 -90.00   86
 10  ω    -70.00  31.00   1.00    2.00    --  -41.82  57.00  90.00  101
 11  ω   -118.00  -9.00   1.00    2.00    --  -41.82 -77.00 -30.00  109
 12  ω   -118.00  -9.00   1.00    2.00    --  -41.82 -77.00  90.00  109
 13  ω     74.00 178.00   1.00    8.00    --  107.00  77.00 120.00  104
 14  ω     79.00 178.00   1.00    8.00    --  107.00  30.00 -60.00   99
 15  ω     81.00 136.00   1.00    8.00    --  107.00  45.00  60.00   55
 16  ω     79.00 178.00   1.00    8.00    --  107.00  30.00-150.00   99
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0421514000
_diffrn_orient_matrix_UB_12      -0.1224347000
_diffrn_orient_matrix_UB_13      0.0087135000
_diffrn_orient_matrix_UB_21      -0.1179732000
_diffrn_orient_matrix_UB_22      0.0320405000
_diffrn_orient_matrix_UB_23      -0.0240977000
_diffrn_orient_matrix_UB_31      0.0431591000
_diffrn_orient_matrix_UB_32      -0.0320293000
_diffrn_orient_matrix_UB_33      -0.0574179000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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         0.778
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                6268
_reflns_number_total             6376
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.338
_refine_diff_density_min         -0.212
_refine_diff_density_rms         0.038
_refine_ls_abs_structure_details 
;
 Flack x determined using 2700 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.021(2)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         6376
_refine_ls_number_restraints     354
_refine_ls_R_factor_all          0.0181
_refine_ls_R_factor_gt           0.0170
_refine_ls_restrained_S_all      1.061
_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)+(0.0189P)²+0.8202P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0404
_refine_ls_wR_factor_ref         0.0408
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C125-C124 \\sim C124-C123 \\sim C123-C122
 with sigma of 0.01
 C119-C118 \\sim C219-C118 \\sim C220-C219 \\sim C120-C119 \\sim C222-C221
\\sim C221-C220 \\sim C122-
 C121 \\sim C223-C222 \\sim C123-C122 \\sim C224-C223 \\sim C124-C123 \\sim
C125-C124 \\sim C224-C125
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim
C125 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223 \\sim C224: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C125) \\sim Ueq, Uanis(C223) \\sim Ueq,
Uanis(C224) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C219) \\sim Ueq, Uanis(C220) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
4. Others
 Sof(H11W)=Sof(H11X)=Sof(H12M)=Sof(H12N)=Sof(C219)=Sof(H21A)=Sof(H21B)=
 Sof(C220)=Sof(H22A)=Sof(H22B)=Sof(C221)=Sof(H22C)=Sof(H22D)=Sof(C222)=
 Sof(H22E)=Sof(H22F)=Sof(C223)=Sof(H22G)=Sof(H22H)=Sof(C224)=Sof(H22I)=
 Sof(H22J)=1-FVAR(1)
 Sof(H11U)=Sof(H11V)=Sof(C119)=Sof(H11Y)=Sof(H)=Sof(C120)=Sof(H12A)=Sof(H12B)=
 Sof(C121)=Sof(H12C)=Sof(H12D)=Sof(C122)=Sof(H12E)=Sof(H12F)=Sof(C123)=
 Sof(H12G)=Sof(H12H)=Sof(C124)=Sof(H12I)=Sof(H12J)=Sof(H12K)=Sof(H12L)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11S,H11T), C118(H11U,H11V), C118(H11W,
 H11X), C119(H11Y,H), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F),
 C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L), C125(H12M,H12N), C126(H12O,
 H12P), C127(H12Q,H12R), C128(H12S,H12T), C129(H12U,H12V), C130(H13A,H13B),
 C219(H21A,H21B), C220(H22A,H22B), C221(H22C,H22D), C222(H22E,H22F), C223(H22G,
 H22H), C224(H22I,H22J)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
5.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Rh1 Rh -0.47766(2) -0.32545(2) -0.63689(2) 0.01962(5) Uani 1 1 d . . . . .
Cl6 Cl -0.60989(5) -0.32332(6) -0.71026(2) 0.02730(11) Uani 1 1 d . . . . .
Cl7 Cl -0.33999(5) -0.33493(6) -0.56631(2) 0.03091(13) Uani 1 1 d . . . . .
P2 P -0.60563(6) -0.39540(6) -0.57006(3) 0.02523(13) Uani 1 1 d . . . . .
P3 P -0.36771(5) -0.19976(5) -0.69309(2) 0.02132(12) Uani 1 1 d . . . . .
O5 O -0.4028(2) -0.56301(19) -0.67872(10) 0.0461(5) Uani 1 1 d . . . . .
C4 C -0.4253(2) -0.4771(2) -0.66420(11) 0.0303(6) Uani 1 1 d . . . . .
C101 C -0.53837(19) -0.1734(2) -0.60723(9) 0.0238(4) Uani 1 1 d . . . . .
C102 C -0.5915(2) -0.1677(3) -0.55592(10) 0.0283(5) Uani 1 1 d . . . . .
C103 C -0.6307(3) -0.0639(3) -0.53596(12) 0.0372(7) Uani 1 1 d . . . . .
H103 H -0.6679 -0.0604 -0.5015 0.045 Uiso 1 1 calc R . . . .
C104 C -0.6156(3) 0.0334(3) -0.56607(13) 0.0391(7) Uani 1 1 d . . . . .
H104 H -0.6423 0.1038 -0.5522 0.047 Uiso 1 1 calc R . . . .
C105 C -0.5618(2) 0.0294(2) -0.61648(12) 0.0333(6) Uani 1 1 d . . . . .
H105 H -0.5504 0.0972 -0.6367 0.040 Uiso 1 1 calc R . . . .
C106 C -0.5245(2) -0.0738(2) -0.63764(11) 0.0260(5) Uani 1 1 d . . . . .
C107 C -0.6058(3) -0.2748(2) -0.52319(11) 0.0310(6) Uani 1 1 d . . . . .
H10A H -0.6791 -0.2725 -0.5027 0.037 Uiso 1 1 calc R . . . .
H10B H -0.5419 -0.2823 -0.4967 0.037 Uiso 1 1 calc R . . . .
C108 C -0.4692(2) -0.0806(2) -0.69302(10) 0.0270(5) Uani 1 1 d . . . . .
H10C H -0.4281 -0.0090 -0.7011 0.032 Uiso 1 1 calc R . . . .
H10D H -0.5287 -0.0922 -0.7214 0.032 Uiso 1 1 calc R . . . .
C109 C -0.7604(2) -0.4259(3) -0.58523(11) 0.0324(6) Uani 1 1 d . . . . .
C110 C -0.8189(2) -0.3169(3) -0.60409(12) 0.0409(7) Uani 1 1 d . . . . .
H11A H -0.8154 -0.2604 -0.5748 0.061 Uiso 1 1 calc GR . . . .
H11B H -0.8995 -0.3327 -0.6131 0.061 Uiso 1 1 calc GR . . . .
H11C H -0.7794 -0.2876 -0.6365 0.061 Uiso 1 1 calc GR . . . .
C111 C -0.7671(3) -0.5161(3) -0.63005(12) 0.0383(6) Uani 1 1 d . . . . .
H11D H -0.7269 -0.4888 -0.6627 0.057 Uiso 1 1 calc GR . . . .
H11E H -0.8478 -0.5310 -0.6390 0.057 Uiso 1 1 calc GR . . . .
H11F H -0.7307 -0.5861 -0.6172 0.057 Uiso 1 1 calc GR . . . .
C112 C -0.8223(3) -0.4699(3) -0.53405(12) 0.0458(8) Uani 1 1 d . . . . .
H11G H -0.7894 -0.5431 -0.5234 0.069 Uiso 1 1 calc GR . . . .
H11H H -0.9044 -0.4793 -0.5419 0.069 Uiso 1 1 calc GR . . . .
H11I H -0.8125 -0.4155 -0.5042 0.069 Uiso 1 1 calc GR . . . .
C113 C -0.2273(2) -0.1372(2) -0.67021(11) 0.0273(5) Uani 1 1 d . . . . .
C114 C -0.2471(3) -0.0740(3) -0.61633(11) 0.0333(6) Uani 1 1 d . . . . .
H11J H -0.3002 -0.0108 -0.6224 0.050 Uiso 1 1 calc GR . . . .
H11K H -0.1736 -0.0448 -0.6027 0.050 Uiso 1 1 calc GR . . . .
H11L H -0.2801 -0.1261 -0.5894 0.050 Uiso 1 1 calc GR . . . .
C115 C -0.1374(2) -0.2308(3) -0.66127(12) 0.0345(6) Uani 1 1 d . . . . .
H11M H -0.1670 -0.2861 -0.6350 0.052 Uiso 1 1 calc GR . . . .
H11N H -0.0664 -0.1971 -0.6471 0.052 Uiso 1 1 calc GR . . . .
H11O H -0.1214 -0.2687 -0.6960 0.052 Uiso 1 1 calc GR . . . .
C116 C -0.1840(3) -0.0512(3) -0.71251(12) 0.0347(6) Uani 1 1 d . . . . .
H11P H -0.1683 -0.0902 -0.7470 0.052 Uiso 1 1 calc GR . . . .
H11Q H -0.1132 -0.0156 -0.6991 0.052 Uiso 1 1 calc GR . . . .
H11R H -0.2427 0.0071 -0.7184 0.052 Uiso 1 1 calc GR . . . .
C117 C -0.5513(3) -0.5116(3) -0.52720(11) 0.0365(6) Uani 1 1 d . . . . .
H11S H -0.4745 -0.4889 -0.5136 0.044 Uiso 1 1 calc R . . . .
H11T H -0.6025 -0.5174 -0.4950 0.044 Uiso 1 1 calc R . . . .
C118 C -0.5397(3) -0.6311(3) -0.55177(14) 0.0469(8) Uani 1 1 d D U . . .
H11U H -0.5152 -0.6247 -0.5904 0.056 Uiso 0.812(5) 1 calc R . P A 1
H11V H -0.6157 -0.6690 -0.5511 0.056 Uiso 0.812(5) 1 calc R . P A 1
H11W H -0.6156 -0.6635 -0.5614 0.056 Uiso 0.188(5) 1 calc R . P A 2
H11X H -0.4895 -0.6312 -0.5844 0.056 Uiso 0.188(5) 1 calc R . P A 2
C119 C -0.4511(4) -0.7052(4) -0.5201(2) 0.0433(11) Uani 0.812(5) 1 d D U P A 1
H11Y H -0.4681 -0.6993 -0.4806 0.052 Uiso 0.812(5) 1 calc R . P A 1
H H -0.4622 -0.7853 -0.5308 0.052 Uiso 0.812(5) 1 calc R . P A 1
C120 C -0.3260(4) -0.6741(5) -0.5291(2) 0.0433(10) Uani 0.812(5) 1 d D U P A 1
H12A H -0.2813 -0.6979 -0.4967 0.052 Uiso 0.812(5) 1 calc R . P A 1
H12B H -0.3200 -0.5906 -0.5319 0.052 Uiso 0.812(5) 1 calc R . P A 1
C121 C -0.2716(5) -0.7265(4) -0.5796(2) 0.0421(10) Uani 0.812(5) 1 d D U P A 1
H12C H -0.3200 -0.7096 -0.6118 0.051 Uiso 0.812(5) 1 calc R . P A 1
H12D H -0.2684 -0.8098 -0.5752 0.051 Uiso 0.812(5) 1 calc R . P A 1
C122 C -0.1505(4) -0.6810(4) -0.58909(18) 0.0475(10) Uani 0.812(5) 1 d D U P A
1
H12E H -0.1082 -0.6834 -0.5540 0.057 Uiso 0.812(5) 1 calc R . P A 1
H12F H -0.1564 -0.6005 -0.6001 0.057 Uiso 0.812(5) 1 calc R . P A 1
C123 C -0.0796(4) -0.7438(4) -0.63202(19) 0.0545(11) Uani 0.812(5) 1 d D U P A
1
H12G H 0.0004 -0.7154 -0.6305 0.065 Uiso 0.812(5) 1 calc R . P A 1
H12H H -0.0779 -0.8253 -0.6223 0.065 Uiso 0.812(5) 1 calc R . P A 1
C124 C -0.1229(4) -0.7325(3) -0.69035(19) 0.0486(11) Uani 0.812(5) 1 d D U P A
1
H12I H -0.2043 -0.7570 -0.6920 0.058 Uiso 0.812(5) 1 calc R . P A 1
H12J H -0.0778 -0.7834 -0.7143 0.058 Uiso 0.812(5) 1 calc R . P A 1
C125 C -0.1135(3) -0.6104(3) -0.71172(18) 0.0572(10) Uani 1 1 d D U . . .
H12K H -0.1624 -0.5599 -0.6893 0.069 Uiso 0.812(5) 1 calc R . P A 1
H12L H -0.0329 -0.5841 -0.7085 0.069 Uiso 0.812(5) 1 calc R . P A 1
H12M H -0.1824 -0.5813 -0.6926 0.069 Uiso 0.188(5) 1 calc R . P A 2
H12N H -0.0571 -0.5477 -0.7097 0.069 Uiso 0.188(5) 1 calc R . P A 2
C126 C -0.1503(3) -0.6041(3) -0.76968(17) 0.0534(9) Uani 1 1 d . . . . .
H12O H -0.2272 -0.6396 -0.7731 0.064 Uiso 1 1 calc R . . . .
H12P H -0.0961 -0.6491 -0.7921 0.064 Uiso 1 1 calc R . . . .
C127 C -0.1563(3) -0.4857(3) -0.79272(15) 0.0454(8) Uani 1 1 d . . . . .
H12Q H -0.1679 -0.4903 -0.8327 0.054 Uiso 1 1 calc R . . . .
H12R H -0.0819 -0.4471 -0.7862 0.054 Uiso 1 1 calc R . . . .
C128 C -0.2529(2) -0.4145(2) -0.76782(12) 0.0338(6) Uani 1 1 d . . . . .
H12S H -0.3274 -0.4523 -0.7750 0.041 Uiso 1 1 calc R . . . .
H12T H -0.2422 -0.4110 -0.7278 0.041 Uiso 1 1 calc R . . . .
C129 C -0.2572(2) -0.2952(2) -0.79025(11) 0.0330(6) Uani 1 1 d . . . . .
H12U H -0.2648 -0.2990 -0.8305 0.040 Uiso 1 1 calc R . . . .
H12V H -0.1835 -0.2568 -0.7819 0.040 Uiso 1 1 calc R . . . .
C130 C -0.3558(2) -0.2238(2) -0.76743(10) 0.0290(5) Uani 1 1 d . . . . .
H13A H -0.4286 -0.2594 -0.7796 0.035 Uiso 1 1 calc R . . . .
H13B H -0.3516 -0.1485 -0.7851 0.035 Uiso 1 1 calc R . . . .
C219 C -0.4843(17) -0.695(2) -0.5040(7) 0.048(4) Uani 0.188(5) 1 d D U P A 2
H21A H -0.5049 -0.6597 -0.4686 0.058 Uiso 0.188(5) 1 calc R . P A 2
H21B H -0.5068 -0.7754 -0.5037 0.058 Uiso 0.188(5) 1 calc R . P A 2
C220 C -0.357(2) -0.680(3) -0.5164(10) 0.049(3) Uani 0.188(5) 1 d D U P A 2
H22A H -0.3108 -0.7064 -0.4848 0.059 Uiso 0.188(5) 1 calc R . P A 2
H22B H -0.3395 -0.5992 -0.5227 0.059 Uiso 0.188(5) 1 calc R . P A 2
C221 C -0.3246(19) -0.7495(18) -0.5673(8) 0.050(3) Uani 0.188(5) 1 d D U P A 2
H22C H -0.3108 -0.8298 -0.5576 0.060 Uiso 0.188(5) 1 calc R . P A 2
H22D H -0.3866 -0.7459 -0.5949 0.060 Uiso 0.188(5) 1 calc R . P A 2
C222 C -0.214(2) -0.6945(16) -0.5889(7) 0.046(3) Uani 0.188(5) 1 d D U P A 2
H22E H -0.2312 -0.6146 -0.5984 0.055 Uiso 0.188(5) 1 calc R . P A 2
H22F H -0.1562 -0.6943 -0.5595 0.055 Uiso 0.188(5) 1 calc R . P A 2
C223 C -0.1637(14) -0.7532(12) -0.6388(7) 0.046(3) Uani 0.188(5) 1 d D U P A 2
H22G H -0.2266 -0.7649 -0.6654 0.055 Uiso 0.188(5) 1 calc R . P A 2
H22H H -0.1367 -0.8291 -0.6273 0.055 Uiso 0.188(5) 1 calc R . P A 2
C224 C -0.0642(13) -0.6946(16) -0.6688(7) 0.057(3) Uani 0.188(5) 1 d D U P A 2
H22I H -0.0158 -0.7520 -0.6872 0.069 Uiso 0.188(5) 1 calc R . P A 2
H22J H -0.0157 -0.6531 -0.6422 0.069 Uiso 0.188(5) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 Cl6 2.3656(5) . ?
Rh1 Cl7 2.3591(6) . ?
Rh1 P2 2.3615(7) . ?
Rh1 P3 2.3938(6) . ?
Rh1 C4 2.005(3) . ?
Rh1 C101 2.061(3) . ?
P2 C107 1.828(3) . ?
P2 C109 1.873(3) . ?
P2 C117 1.838(3) . ?
P3 C108 1.836(3) . ?
P3 C113 1.877(3) . ?
P3 C130 1.849(3) . ?
O5 C4 1.106(4) . ?
C101 C102 1.402(3) . ?
C101 C106 1.400(4) . ?
C102 C103 1.395(4) . ?
C102 C107 1.506(4) . ?
C103 C104 1.376(5) . ?
C104 C105 1.385(4) . ?
C105 C106 1.393(4) . ?
C106 C108 1.503(3) . ?
C109 C110 1.527(5) . ?
C109 C111 1.531(4) . ?
C109 C112 1.536(4) . ?
C113 C114 1.533(4) . ?
C113 C115 1.536(4) . ?
C113 C116 1.536(4) . ?
C117 C118 1.540(4) . ?
C118 C119 1.558(5) . ?
C118 C219 1.531(10) . ?
C119 C120 1.517(5) . ?
C120 C121 1.520(7) . ?
C121 C122 1.526(5) . ?
C122 C123 1.528(5) . ?
C123 C124 1.521(6) . ?
C124 C125 1.537(5) . ?
C125 C126 1.485(6) . ?
C125 C224 1.556(10) . ?
C126 C127 1.509(5) . ?
C127 C128 1.530(4) . ?
C128 C129 1.513(4) . ?
C129 C130 1.528(4) . ?
C219 C220 1.521(10) . ?
C220 C221 1.537(10) . ?
C221 C222 1.530(10) . ?
C222 C223 1.523(10) . ?
C223 C224 1.535(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl6 Rh1 P3 84.46(2) . . ?
Cl7 Rh1 Cl6 176.92(2) . . ?
Cl7 Rh1 P2 84.42(2) . . ?
Cl7 Rh1 P3 95.09(2) . . ?
P2 Rh1 Cl6 96.96(2) . . ?
P2 Rh1 P3 162.17(2) . . ?
C4 Rh1 Cl6 87.31(8) . . ?
C4 Rh1 Cl7 89.80(8) . . ?
C4 Rh1 P2 96.36(8) . . ?
C4 Rh1 P3 101.47(8) . . ?
C4 Rh1 C101 177.22(11) . . ?
C101 Rh1 Cl6 92.07(6) . . ?
C101 Rh1 Cl7 90.87(6) . . ?
C101 Rh1 P2 81.03(7) . . ?
C101 Rh1 P3 81.15(7) . . ?
C107 P2 Rh1 99.44(9) . . ?
C107 P2 C109 105.88(13) . . ?
C107 P2 C117 102.81(14) . . ?
C109 P2 Rh1 122.35(9) . . ?
C117 P2 Rh1 116.12(10) . . ?
C117 P2 C109 107.46(14) . . ?
C108 P3 Rh1 97.51(9) . . ?
C108 P3 C113 104.93(12) . . ?
C108 P3 C130 99.60(12) . . ?
C113 P3 Rh1 122.42(8) . . ?
C130 P3 Rh1 120.77(9) . . ?
C130 P3 C113 106.84(12) . . ?
O5 C4 Rh1 175.9(3) . . ?
C102 C101 Rh1 120.6(2) . . ?
C106 C101 Rh1 120.22(17) . . ?
C106 C101 C102 119.2(2) . . ?
C101 C102 C107 119.1(2) . . ?
C103 C102 C101 120.0(3) . . ?
C103 C102 C107 120.9(2) . . ?
C104 C103 C102 120.2(3) . . ?
C103 C104 C105 120.5(3) . . ?
C104 C105 C106 120.1(3) . . ?
C101 C106 C108 119.0(2) . . ?
C105 C106 C101 120.0(2) . . ?
C105 C106 C108 121.0(2) . . ?
C102 C107 P2 108.58(17) . . ?
C106 C108 P3 108.43(17) . . ?
C110 C109 P2 109.0(2) . . ?
C110 C109 C111 110.2(2) . . ?
C110 C109 C112 108.9(3) . . ?
C111 C109 P2 109.0(2) . . ?
C111 C109 C112 109.1(2) . . ?
C112 C109 P2 110.7(2) . . ?
C114 C113 P3 108.56(18) . . ?
C114 C113 C115 109.2(2) . . ?
C114 C113 C116 108.0(2) . . ?
C115 C113 P3 110.63(19) . . ?
C116 C113 P3 110.11(18) . . ?
C116 C113 C115 110.3(2) . . ?
C118 C117 P2 119.3(2) . . ?
C117 C118 C119 112.1(3) . . ?
C219 C118 C117 100.7(10) . . ?
C120 C119 C118 115.2(4) . . ?
C119 C120 C121 114.8(4) . . ?
C120 C121 C122 111.4(4) . . ?
C121 C122 C123 115.6(4) . . ?
C124 C123 C122 115.2(3) . . ?
C123 C124 C125 112.2(4) . . ?
C126 C125 C124 110.6(3) . . ?
C126 C125 C224 141.7(9) . . ?
C125 C126 C127 114.7(3) . . ?
C126 C127 C128 113.1(3) . . ?
C129 C128 C127 113.0(3) . . ?
C128 C129 C130 113.9(2) . . ?
C129 C130 P3 120.08(19) . . ?
C220 C219 C118 101.7(17) . . ?
C219 C220 C221 110.0(18) . . ?
C222 C221 C220 105.1(15) . . ?
C223 C222 C221 114.2(16) . . ?
C222 C223 C224 118.1(16) . . ?
C223 C224 C125 109.5(11) . . ?

_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 2.079
_oxdiff_exptl_absorpt_empirical_full_min 0.825
####################################################################### 
# 
# 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_0463abc19s
_database_code_depnum_ccdc_archive 'CCDC 1972812'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# trans-POCOP-14.2BH3
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT301_0463abc19s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        24% Note  
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C28 H56 B2 O2 P2'
_chemical_formula_sum            'C28 H56 B2 O2 P2'
_chemical_formula_weight         508.28
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
B B 0.0090 0.0039 '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      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                   15.09343(9)
_cell_length_b                   12.86467(7)
_cell_length_c                   32.65837(16)
_cell_angle_alpha                90
_cell_angle_beta                 90.5535(5)
_cell_angle_gamma                90
_cell_volume                     6341.04(6)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    32841
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.4190
_cell_measurement_theta_min      3.1940
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    1.388
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.351
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.45a (Rigaku Oxford Diffraction, 2019)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.065
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             2240
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
-10 0 -1 0.3572
-1 -4 -19 0.0764
10 -1 -3 0.2868
1 4 19 0.0020
-9 -2 -3 0.3416
0 7 -10 0.1017
0 -7 10 0.1321

_exptl_crystal_recrystallization_method 'Crystals grown from an oil at 293 K'
_exptl_crystal_size_max          0.653
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.087
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
-9.7724 0.0421 -1.3556 -0.1302 -0.1200 0.9842
-0.5320 -4.0180 -18.5296 0.6688 0.6844 0.2903
9.6548 -0.9631 -2.8910 0.2835 0.2770 -0.9181
0.7843 4.0034 18.5025 -0.6632 -0.6790 -0.3149
-9.4227 -1.9069 -3.0080 -0.1178 0.1282 0.9847
0.1304 7.2804 -10.3840 0.7131 -0.7001 0.0360
-0.3485 -7.2993 10.2782 -0.7134 0.7007 -0.0130

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0395
_diffrn_reflns_av_unetI/netI     0.0215
_diffrn_reflns_Laue_measured_fraction_full 0.990
_diffrn_reflns_Laue_measured_fraction_max 0.990
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            68205
_diffrn_reflns_point_group_measured_fraction_full 0.990
_diffrn_reflns_point_group_measured_fraction_max 0.990
_diffrn_reflns_theta_full        73.612
_diffrn_reflns_theta_max         73.612
_diffrn_reflns_theta_min         2.706
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -66.00  32.00   1.00    6.00    --  -42.07  37.00-150.00   98
  2  ω    -66.00  32.00   1.00    6.00    --  -42.07  37.00 120.00   98
  3  ω      1.00  83.00   1.00    6.00    --   42.07 -99.00 -30.00   82
  4  ω     31.00 140.00   1.00   24.00    --  107.00 -77.00 150.00  109
  5  ω     94.00 178.00   1.00   24.00    --  107.00 125.00 120.00   84
  6  ω     94.00 178.00   1.00   24.00    --  107.00 125.00-180.00   84
  7  ω     81.00 178.00   1.00   24.00    --  107.00  45.00 -60.00   97
  8  ω   -114.00 -14.00   1.00    6.00    --  -42.07 -57.00 -60.00  100
  9  ω   -114.00 -14.00   1.00    6.00    --  -42.07 -57.00-180.00  100
 10  ω   -114.00 -14.00   1.00    6.00    --  -42.07 -57.00  60.00  100
 11  ω     78.00 178.00   1.00   24.00    --  107.00  61.00-120.00  100
 12  ω     81.00 178.00   1.00   24.00    --  107.00  45.00 150.00   97
 13  ω     74.00 178.00   1.00   24.00    --  107.00  77.00-180.00  104
 14  ω   -118.00  -9.00   1.00    6.00    --  -42.07 -77.00 -90.00  109
 15  ω     30.00 112.00   1.00   24.00    --  107.00-109.00 147.00   82
 16  ω     74.00 178.00   1.00   24.00    --  107.00  77.00-150.00  104
 17  ω     74.00 178.00   1.00   24.00    --  107.00  77.00 150.00  104
 18  ω     34.00 118.00   1.00   24.00    --  107.00-125.00   0.00   84
 19  ω   -118.00 -77.00   1.00    6.00    --  -42.07 -77.00-180.00   41
 20  ω     23.00  98.00   1.00    6.00    --   42.07-125.00-120.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0195959000
_diffrn_orient_matrix_UB_12      0.0346100000
_diffrn_orient_matrix_UB_13      -0.0441611000
_diffrn_orient_matrix_UB_21      0.0135290000
_diffrn_orient_matrix_UB_22      -0.1142965000
_diffrn_orient_matrix_UB_23      -0.0125404000
_diffrn_orient_matrix_UB_31      -0.0992381000
_diffrn_orient_matrix_UB_32      -0.0088301000
_diffrn_orient_matrix_UB_33      -0.0109036000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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                11183
_reflns_number_total             12666
_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 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.45a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.464
_refine_diff_density_min         -0.355
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         12666
_refine_ls_number_restraints     573
_refine_ls_R_factor_all          0.0442
_refine_ls_R_factor_gt           0.0388
_refine_ls_restrained_S_all      1.109
_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)+(0.0544P)²+2.3195P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1031
_refine_ls_wR_factor_ref         0.1082
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All B(H,H,H) groups, All C(H,H,H) groups
2. Restrained distances
 C218-C217 \\sim C318-C217 \\sim C219-C218 \\sim C319-C318 \\sim C320-C319
\\sim C220-C219 \\sim C321-
 C320 \\sim C221-C220 \\sim C322-C321 \\sim C222-C221 \\sim C223-C222 \\sim
C323-C322 \\sim C324-C323 ~
 C224-C223 \\sim C325-C324 \\sim C225-C224 \\sim C226-C225 \\sim C325-C226
 with sigma of 0.01
 B12-H12B \\sim B12-H12A \\sim B12-H12C \\sim B13-H13A \\sim B13-H13B \\sim
B13-H13C \\sim B3-H3B \\sim B3-
 H3A \\sim B3-H3C \\sim B2-H2C \\sim B2-H2A \\sim B2-H2B
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C217 \\sim C218 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223 \\sim
C224 \\sim C225 \\sim C226 \\sim C318 \\sim C319 \\sim C320 \\sim C321 \\sim
C322 \\sim C323 \\sim C324 \\sim C325: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C222) \\sim Ueq, Uanis(C217) \\sim Ueq, Uanis(C221) \\sim Ueq,
Uanis(C220) \\sim Ueq, Uanis(C219) \\sim Ueq, Uanis(C218) \\sim Ueq,
Uanis(C318) \\sim Ueq, Uanis(C321) \\sim Ueq, Uanis(C319) \\sim Ueq,
Uanis(C322) \\sim Ueq, Uanis(C320) \\sim Ueq, Uanis(C323) \\sim Ueq,
Uanis(C226) \\sim Ueq, Uanis(C225) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C223) \\sim Ueq, Uanis(C324) \\sim Ueq, Uanis(C325) \\sim Ueq: with sigma
of 0.007 and sigma for terminal atoms of 0.014
4. Others
 Sof(H21U)=Sof(H21V)=Sof(H22I)=Sof(H22J)=Sof(C318)=Sof(H31A)=Sof(H31B)=
 Sof(C319)=Sof(H31C)=Sof(H31D)=Sof(C320)=Sof(H32I)=Sof(H32J)=Sof(C321)=
 Sof(H32A)=Sof(H32B)=Sof(C322)=Sof(H32E)=Sof(H32F)=Sof(C323)=Sof(H32K)=
 Sof(H32L)=Sof(C324)=Sof(H32C)=Sof(H32D)=Sof(C325)=Sof(H32G)=Sof(H32H)=1-FVAR(1)
 Sof(H21S)=Sof(H21T)=Sof(C218)=Sof(H)=Sof(H21Y)=Sof(C219)=Sof(H21W)=Sof(H21X)=
 Sof(C220)=Sof(H22U)=Sof(H22V)=Sof(C221)=Sof(H22S)=Sof(H22T)=Sof(C222)=
 Sof(H22K)=Sof(H22L)=Sof(C223)=Sof(H22Q)=Sof(H22R)=Sof(C224)=Sof(H22O)=
 Sof(H22P)=Sof(C225)=Sof(H22M)=Sof(H22N)=Sof(H22G)=Sof(H22H)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11F,H11G), C118(H11D,H11E), C119(H11Q,H11R), C120(H12V,H12W), C121(H12T,
 H12U), C122(H12N,H12O), C123(H12F,H12G), C124(H12L,H12M), C125(H12R,H12S),
 C126(H12D,H12E), C127(H12H,H12I), C128(H12P,H12Q), C129(H12J,H12K), C130(H13D,
 H13E), C217(H21S,H21T), C217(H21U,H21V), C218(H,H21Y), C219(H21W,H21X),
 C220(H22U,H22V), C221(H22S,H22T), C222(H22K,H22L), C223(H22Q,H22R), C224(H22O,
 H22P), C225(H22M,H22N), C226(H22G,H22H), C226(H22I,H22J), C227(H22E,H22F),
 C228(H22C,H22D), C229(H22A,H22B), C230(H23A,H23B), C318(H31A,H31B), C319(H31C,
 H31D), C320(H32I,H32J), C321(H32A,H32B), C322(H32E,H32F), C323(H32K,H32L),
 C324(H32C,H32D), C325(H32G,H32H)
5.b Aromatic/amide H refined with riding coordinates:
 C101(H101), C103(H103), C104(H104), C105(H105), C201(H201), C203(H203),
 C204(H204), C205(H205)
5.c Idealised Me refined as rotating group:
 C110(H11H,H11I,H11J), C111(H11S,H11T,H11U), C112(H11K,H11L,H11M), C114(H11N,
 H11O,H11P), C115(H11V,H11W,H11X), C116(H11A,H11B,H11C), C210(H21D,H21E,H21F),
 C211(H21G,H21H,H21I), C212(H21J,H21K,H21L), C214(H21P,H21Q,H21R), C215(H21M,
 H21N,H21O), C216(H21A,H21B,H21C)
5.d Idealised Me refined as rotating group with stretchable bonds:
 B2(H2A,H2B,H2C), B3(H3A,H3B,H3C), B12(H12A,H12B,H12C), B13(H13A,H13B,H13C)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
P2 P 1.05812(2) 0.85760(2) 0.69200(2) 0.02060(8) Uani 1 1 d . . . . .
P3 P 0.75292(2) 0.79907(2) 0.53974(2) 0.01911(8) Uani 1 1 d . . . . .
O107 O 1.07416(6) 0.88031(7) 0.64346(3) 0.02221(19) Uani 1 1 d . . . . .
O108 O 0.78861(6) 0.87153(8) 0.57725(3) 0.0257(2) Uani 1 1 d . . . . .
C101 C 0.92901(8) 0.87505(10) 0.61055(4) 0.0205(2) Uani 1 1 d . . . . .
H101 H 0.9097 0.8215 0.6284 0.025 Uiso 1 1 calc R . . . .
C102 C 1.01284(8) 0.91784(10) 0.61462(4) 0.0192(2) Uani 1 1 d . . . . .
C103 C 1.04235(9) 0.99482(10) 0.58844(4) 0.0244(3) Uani 1 1 d . . . . .
H103 H 1.1004 1.0225 0.5914 0.029 Uiso 1 1 calc R . . . .
C104 C 0.98580(10) 1.03097(11) 0.55779(4) 0.0295(3) Uani 1 1 d . . . . .
H104 H 1.0055 1.0837 0.5397 0.035 Uiso 1 1 calc R . . . .
C105 C 0.90070(9) 0.99079(11) 0.55331(4) 0.0290(3) Uani 1 1 d . . . . .
H105 H 0.8617 1.0163 0.5326 0.035 Uiso 1 1 calc R . . . .
C106 C 0.87410(8) 0.91278(10) 0.57964(4) 0.0221(3) Uani 1 1 d . . . . .
C109 C 1.07410(10) 0.98425(10) 0.71709(4) 0.0267(3) Uani 1 1 d . . . . .
C110 C 0.99905(11) 1.05622(11) 0.70293(4) 0.0353(3) Uani 1 1 d . . . . .
H11H H 1.0019 1.0655 0.6732 0.053 Uiso 1 1 calc GR . . . .
H11I H 1.0053 1.1239 0.7165 0.053 Uiso 1 1 calc GR . . . .
H11J H 0.9419 1.0253 0.7101 0.053 Uiso 1 1 calc GR . . . .
C111 C 1.06902(13) 0.96953(13) 0.76376(4) 0.0415(4) Uani 1 1 d . . . . .
H11S H 1.0119 0.9384 0.7707 0.062 Uiso 1 1 calc GR . . . .
H11T H 1.0749 1.0372 0.7773 0.062 Uiso 1 1 calc GR . . . .
H11U H 1.1171 0.9237 0.7729 0.062 Uiso 1 1 calc GR . . . .
C112 C 1.16390(11) 1.03122(12) 0.70559(5) 0.0372(3) Uani 1 1 d . . . . .
H11K H 1.2117 0.9860 0.7156 0.056 Uiso 1 1 calc GR . . . .
H11L H 1.1699 1.1002 0.7181 0.056 Uiso 1 1 calc GR . . . .
H11M H 1.1675 1.0375 0.6757 0.056 Uiso 1 1 calc GR . . . .
C113 C 0.64253(8) 0.85361(11) 0.52966(4) 0.0240(3) Uani 1 1 d . . . . .
C114 C 0.65409(10) 0.96870(13) 0.51839(5) 0.0393(4) Uani 1 1 d . . . . .
H11N H 0.6776 1.0068 0.5421 0.059 Uiso 1 1 calc GR . . . .
H11O H 0.5966 0.9980 0.5103 0.059 Uiso 1 1 calc GR . . . .
H11P H 0.6955 0.9747 0.4956 0.059 Uiso 1 1 calc GR . . . .
C115 C 0.60189(11) 0.79392(16) 0.49342(5) 0.0449(4) Uani 1 1 d . . . . .
H11V H 0.6413 0.7989 0.4698 0.067 Uiso 1 1 calc GR . . . .
H11W H 0.5441 0.8240 0.4863 0.067 Uiso 1 1 calc GR . . . .
H11X H 0.5944 0.7207 0.5010 0.067 Uiso 1 1 calc GR . . . .
C116 C 0.58251(9) 0.84537(12) 0.56694(4) 0.0319(3) Uani 1 1 d . . . . .
H11A H 0.5719 0.7720 0.5732 0.048 Uiso 1 1 calc GR . . . .
H11B H 0.5259 0.8798 0.5610 0.048 Uiso 1 1 calc GR . . . .
H11C H 0.6112 0.8791 0.5905 0.048 Uiso 1 1 calc GR . . . .
C117 C 1.15564(9) 0.77975(11) 0.70207(4) 0.0291(3) Uani 1 1 d . . . . .
H11F H 1.2043 0.8047 0.6845 0.035 Uiso 1 1 calc R . . . .
H11G H 1.1742 0.7899 0.7309 0.035 Uiso 1 1 calc R . . . .
C118 C 1.14159(9) 0.66314(11) 0.69433(4) 0.0284(3) Uani 1 1 d . . . . .
H11D H 1.0988 0.6357 0.7144 0.034 Uiso 1 1 calc R . . . .
H11E H 1.1159 0.6532 0.6666 0.034 Uiso 1 1 calc R . . . .
C119 C 1.22759(10) 0.60252(12) 0.69780(6) 0.0420(4) Uani 1 1 d . . . . .
H11Q H 1.2594 0.6248 0.7230 0.050 Uiso 1 1 calc R . . . .
H11R H 1.2653 0.6201 0.6741 0.050 Uiso 1 1 calc R . . . .
C120 C 1.21505(10) 0.48434(12) 0.69919(5) 0.0364(3) Uani 1 1 d . . . . .
H12V H 1.2727 0.4517 0.7061 0.044 Uiso 1 1 calc R . . . .
H12W H 1.1734 0.4675 0.7214 0.044 Uiso 1 1 calc R . . . .
C121 C 1.18033(11) 0.43666(12) 0.65967(5) 0.0353(3) Uani 1 1 d . . . . .
H12T H 1.2212 0.4538 0.6371 0.042 Uiso 1 1 calc R . . . .
H12U H 1.1218 0.4672 0.6529 0.042 Uiso 1 1 calc R . . . .
C122 C 1.17135(11) 0.31872(11) 0.66300(5) 0.0344(3) Uani 1 1 d . . . . .
H12N H 1.2298 0.2892 0.6706 0.041 Uiso 1 1 calc R . . . .
H12O H 1.1298 0.3025 0.6854 0.041 Uiso 1 1 calc R . . . .
C123 C 1.13848(12) 0.26542(13) 0.62396(5) 0.0402(4) Uani 1 1 d . . . . .
H12F H 1.1312 0.1903 0.6296 0.048 Uiso 1 1 calc R . . . .
H12G H 1.1845 0.2725 0.6028 0.048 Uiso 1 1 calc R . . . .
C124 C 1.05085(11) 0.30766(12) 0.60662(4) 0.0361(3) Uani 1 1 d . . . . .
H12L H 1.0600 0.3803 0.5976 0.043 Uiso 1 1 calc R . . . .
H12M H 1.0339 0.2663 0.5822 0.043 Uiso 1 1 calc R . . . .
C125 C 0.97495(11) 0.30512(12) 0.63690(5) 0.0365(3) Uani 1 1 d . . . . .
H12R H 0.9929 0.3442 0.6617 0.044 Uiso 1 1 calc R . . . .
H12S H 0.9646 0.2321 0.6451 0.044 Uiso 1 1 calc R . . . .
C126 C 0.88804(11) 0.35041(11) 0.62064(5) 0.0338(3) Uani 1 1 d . . . . .
H12D H 0.8665 0.3071 0.5975 0.041 Uiso 1 1 calc R . . . .
H12E H 0.8432 0.3473 0.6425 0.041 Uiso 1 1 calc R . . . .
C127 C 0.89682(10) 0.46237(11) 0.60618(5) 0.0306(3) Uani 1 1 d . . . . .
H12H H 0.9354 0.4639 0.5818 0.037 Uiso 1 1 calc R . . . .
H12I H 0.9263 0.5035 0.6280 0.037 Uiso 1 1 calc R . . . .
C128 C 0.80880(9) 0.51389(11) 0.59527(4) 0.0281(3) Uani 1 1 d . . . . .
H12P H 0.7727 0.5207 0.6203 0.034 Uiso 1 1 calc R . . . .
H12Q H 0.7759 0.4694 0.5756 0.034 Uiso 1 1 calc R . . . .
C129 C 0.82266(9) 0.62104(10) 0.57645(4) 0.0276(3) Uani 1 1 d . . . . .
H12J H 0.8602 0.6140 0.5519 0.033 Uiso 1 1 calc R . . . .
H12K H 0.8548 0.6655 0.5964 0.033 Uiso 1 1 calc R . . . .
C130 C 0.73592(9) 0.67457(11) 0.56419(4) 0.0270(3) Uani 1 1 d . . . . .
H13D H 0.6996 0.6847 0.5889 0.032 Uiso 1 1 calc R . . . .
H13E H 0.7024 0.6287 0.5453 0.032 Uiso 1 1 calc R . . . .
B2 B 0.95103(11) 0.78983(14) 0.70732(5) 0.0330(4) Uani 1 1 d D . . . .
H2A H 0.8959(4) 0.8431(5) 0.7037(3) 0.049 Uiso 1 1 calc DGR . . . .
H2B H 0.9559(3) 0.7654(8) 0.7390(2) 0.049 Uiso 1 1 calc DGR . . . .
H2C H 0.9404(4) 0.7225(7) 0.6880(3) 0.049 Uiso 1 1 calc DGR . . . .
B3 B 0.82789(11) 0.78955(13) 0.49331(5) 0.0305(3) Uani 1 1 d D . . . .
H3A H 0.8255(6) 0.8618(6) 0.4765(2) 0.046 Uiso 1 1 calc DGR . . . .
H3B H 0.8056(5) 0.7268(7) 0.4738(2) 0.046 Uiso 1 1 calc DGR . . . .
H3C H 0.8951(5) 0.7747(9) 0.50335(8) 0.046 Uiso 1 1 calc DGR . . . .
P12 P 0.57307(2) 0.63338(3) 0.69116(2) 0.02467(9) Uani 1 1 d . . . . .
P13 P 0.25686(2) 0.70293(3) 0.54559(2) 0.02110(8) Uani 1 1 d . . . . .
O207 O 0.58558(6) 0.60437(9) 0.64302(3) 0.0323(2) Uani 1 1 d . . . . .
O208 O 0.29474(6) 0.62863(8) 0.58209(3) 0.0300(2) Uani 1 1 d . . . . .
C201 C 0.43767(9) 0.61886(11) 0.61263(4) 0.0261(3) Uani 1 1 d . . . . .
H201 H 0.4210 0.6716 0.6314 0.031 Uiso 1 1 calc R . . . .
C202 C 0.52102(9) 0.57333(11) 0.61467(4) 0.0253(3) Uani 1 1 d . . . . .
C203 C 0.54642(9) 0.49755(11) 0.58705(4) 0.0304(3) Uani 1 1 d . . . . .
H203 H 0.6039 0.4677 0.5886 0.036 Uiso 1 1 calc R . . . .
C204 C 0.48684(10) 0.46587(12) 0.55711(5) 0.0366(3) Uani 1 1 d . . . . .
H204 H 0.5039 0.4142 0.5380 0.044 Uiso 1 1 calc R . . . .
C205 C 0.40242(10) 0.50867(13) 0.55467(5) 0.0355(3) Uani 1 1 d . . . . .
H205 H 0.3613 0.4859 0.5344 0.043 Uiso 1 1 calc R . . . .
C206 C 0.37947(9) 0.58501(11) 0.58237(4) 0.0272(3) Uani 1 1 d . . . . .
C209 C 0.56098(10) 0.50842(11) 0.71749(4) 0.0303(3) Uani 1 1 d . . . . .
C210 C 0.47245(12) 0.45983(14) 0.70385(5) 0.0448(4) Uani 1 1 d . . . . .
H21D H 0.4740 0.4451 0.6744 0.067 Uiso 1 1 calc GR . . . .
H21E H 0.4241 0.5084 0.7095 0.067 Uiso 1 1 calc GR . . . .
H21F H 0.4628 0.3950 0.7189 0.067 Uiso 1 1 calc GR . . . .
C211 C 0.55877(14) 0.52909(17) 0.76379(5) 0.0533(5) Uani 1 1 d . . . . .
H21G H 0.5090 0.5753 0.7700 0.080 Uiso 1 1 calc GR . . . .
H21H H 0.6144 0.5620 0.7725 0.080 Uiso 1 1 calc GR . . . .
H21I H 0.5515 0.4632 0.7784 0.080 Uiso 1 1 calc GR . . . .
C212 C 0.63664(13) 0.43439(13) 0.70753(6) 0.0459(4) Uani 1 1 d . . . . .
H21J H 0.6929 0.4648 0.7168 0.069 Uiso 1 1 calc GR . . . .
H21K H 0.6384 0.4228 0.6779 0.069 Uiso 1 1 calc GR . . . .
H21L H 0.6272 0.3680 0.7215 0.069 Uiso 1 1 calc GR . . . .
C213 C 0.14599(9) 0.64879(11) 0.53628(4) 0.0269(3) Uani 1 1 d . . . . .
C214 C 0.15683(11) 0.53552(14) 0.52235(6) 0.0445(4) Uani 1 1 d . . . . .
H21P H 0.1835 0.4947 0.5446 0.067 Uiso 1 1 calc GR . . . .
H21Q H 0.1953 0.5330 0.4984 0.067 Uiso 1 1 calc GR . . . .
H21R H 0.0986 0.5066 0.5152 0.067 Uiso 1 1 calc GR . . . .
C215 C 0.10154(12) 0.71347(18) 0.50255(6) 0.0554(5) Uani 1 1 d . . . . .
H21M H 0.1390 0.7136 0.4782 0.083 Uiso 1 1 calc GR . . . .
H21N H 0.0935 0.7849 0.5122 0.083 Uiso 1 1 calc GR . . . .
H21O H 0.0437 0.6832 0.4956 0.083 Uiso 1 1 calc GR . . . .
C216 C 0.09006(10) 0.65046(12) 0.57500(5) 0.0345(3) Uani 1 1 d . . . . .
H21A H 0.0813 0.7225 0.5838 0.052 Uiso 1 1 calc GR . . . .
H21B H 0.1206 0.6116 0.5968 0.052 Uiso 1 1 calc GR . . . .
H21C H 0.0324 0.6183 0.5693 0.052 Uiso 1 1 calc GR . . . .
C217 C 0.68589(10) 0.67624(13) 0.70214(6) 0.0445(4) Uani 1 1 d D U . . .
H21S H 0.7109 0.6309 0.7238 0.053 Uiso 0.596(2) 1 calc R . P A 1
H21T H 0.7217 0.6654 0.6772 0.053 Uiso 0.596(2) 1 calc R . P A 1
H21U H 0.6914 0.6966 0.7313 0.053 Uiso 0.404(2) 1 calc R . P A 2
H21V H 0.7279 0.6187 0.6970 0.053 Uiso 0.404(2) 1 calc R . P A 2
C218 C 0.69745(17) 0.79106(19) 0.71594(8) 0.0347(6) Uani 0.596(2) 1 d D U P A 1
H H 0.6501 0.8103 0.7353 0.042 Uiso 0.596(2) 1 calc R . P A 1
H21Y H 0.7554 0.8002 0.7299 0.042 Uiso 0.596(2) 1 calc R . P A 1
C219 C 0.69249(19) 0.8588(2) 0.67862(10) 0.0362(6) Uani 0.596(2) 1 d D U P A 1
H21W H 0.6341 0.8488 0.6651 0.043 Uiso 0.596(2) 1 calc R . P A 1
H21X H 0.7387 0.8366 0.6592 0.043 Uiso 0.596(2) 1 calc R . P A 1
C220 C 0.7051(2) 0.9761(3) 0.68820(10) 0.0409(8) Uani 0.596(2) 1 d D U P A 1
H22U H 0.6665 0.9960 0.7112 0.049 Uiso 0.596(2) 1 calc R . P A 1
H22V H 0.7673 0.9889 0.6967 0.049 Uiso 0.596(2) 1 calc R . P A 1
C221 C 0.68275(18) 1.04276(19) 0.65107(8) 0.0349(6) Uani 0.596(2) 1 d D U P A 1
H22S H 0.6225 1.0240 0.6413 0.042 Uiso 0.596(2) 1 calc R . P A 1
H22T H 0.7245 1.0252 0.6289 0.042 Uiso 0.596(2) 1 calc R . P A 1
C222 C 0.6859(2) 1.1596(2) 0.65803(10) 0.0342(6) Uani 0.596(2) 1 d D U P A 1
H22K H 0.7477 1.1801 0.6644 0.041 Uiso 0.596(2) 1 calc R . P A 1
H22L H 0.6495 1.1767 0.6822 0.041 Uiso 0.596(2) 1 calc R . P A 1
C223 C 0.6526(2) 1.2235(2) 0.62143(9) 0.0376(7) Uani 0.596(2) 1 d D U P A 1
H22Q H 0.6521 1.2978 0.6292 0.045 Uiso 0.596(2) 1 calc R . P A 1
H22R H 0.6949 1.2153 0.5987 0.045 Uiso 0.596(2) 1 calc R . P A 1
C224 C 0.56001(18) 1.19344(19) 0.60604(7) 0.0329(6) Uani 0.596(2) 1 d D U P A 1
H22O H 0.5627 1.1230 0.5939 0.039 Uiso 0.596(2) 1 calc R . P A 1
H22P H 0.5420 1.2423 0.5841 0.039 Uiso 0.596(2) 1 calc R . P A 1
C225 C 0.4891(2) 1.1942(2) 0.63932(9) 0.0356(7) Uani 0.596(2) 1 d D U P A 1
H22M H 0.5100 1.1521 0.6629 0.043 Uiso 0.596(2) 1 calc R . P A 1
H22N H 0.4804 1.2663 0.6490 0.043 Uiso 0.596(2) 1 calc R . P A 1
C226 C 0.40227(11) 1.15158(12) 0.62404(5) 0.0367(3) Uani 1 1 d D U . . .
H22G H 0.3805 1.1961 0.6014 0.044 Uiso 0.596(2) 1 calc R . P A 1
H22H H 0.3586 1.1557 0.6464 0.044 Uiso 0.596(2) 1 calc R . P A 1
H22I H 0.3838 1.1529 0.6530 0.044 Uiso 0.404(2) 1 calc R . P A 2
H22J H 0.3579 1.1907 0.6077 0.044 Uiso 0.404(2) 1 calc R . P A 2
C227 C 0.40666(10) 1.03951(11) 0.60897(5) 0.0340(3) Uani 1 1 d . . . . .
H22E H 0.4405 1.0381 0.5832 0.041 Uiso 1 1 calc R . . . .
H22F H 0.4401 0.9980 0.6294 0.041 Uiso 1 1 calc R . . . .
C228 C 0.31742(10) 0.98722(12) 0.60138(5) 0.0328(3) Uani 1 1 d . . . . .
H22C H 0.2810 1.0312 0.5829 0.039 Uiso 1 1 calc R . . . .
H22D H 0.2858 0.9803 0.6277 0.039 Uiso 1 1 calc R . . . .
C229 C 0.32895(9) 0.87976(11) 0.58219(5) 0.0296(3) Uani 1 1 d . . . . .
H22A H 0.3628 0.8352 0.6015 0.035 Uiso 1 1 calc R . . . .
H22B H 0.3642 0.8868 0.5569 0.035 Uiso 1 1 calc R . . . .
C230 C 0.24138(9) 0.82596(11) 0.57154(5) 0.0301(3) Uani 1 1 d . . . . .
H23A H 0.2055 0.8724 0.5538 0.036 Uiso 1 1 calc R . . . .
H23B H 0.2079 0.8140 0.5970 0.036 Uiso 1 1 calc R . . . .
C318 C 0.7094(2) 0.7744(2) 0.67313(9) 0.0259(7) Uani 0.404(2) 1 d D U P A 2
H31A H 0.7704 0.7672 0.6626 0.031 Uiso 0.404(2) 1 calc R . P A 2
H31B H 0.6680 0.7768 0.6495 0.031 Uiso 0.404(2) 1 calc R . P A 2
C319 C 0.7017(3) 0.8755(3) 0.69844(13) 0.0308(8) Uani 0.404(2) 1 d D U P A 2
H31C H 0.6412 0.8815 0.7096 0.037 Uiso 0.404(2) 1 calc R . P A 2
H31D H 0.7442 0.8734 0.7217 0.037 Uiso 0.404(2) 1 calc R . P A 2
C320 C 0.7214(3) 0.9697(3) 0.67152(13) 0.0326(10) Uani 0.404(2) 1 d D U P A 2
H32I H 0.7805 0.9616 0.6591 0.039 Uiso 0.404(2) 1 calc R . P A 2
H32J H 0.6769 0.9739 0.6491 0.039 Uiso 0.404(2) 1 calc R . P A 2
C321 C 0.7193(3) 1.0680(3) 0.69629(11) 0.0348(8) Uani 0.404(2) 1 d D U P A 2
H32A H 0.7668 1.0646 0.7173 0.042 Uiso 0.404(2) 1 calc R . P A 2
H32B H 0.6620 1.0715 0.7107 0.042 Uiso 0.404(2) 1 calc R . P A 2
C322 C 0.7309(3) 1.1685(3) 0.67146(14) 0.0397(9) Uani 0.404(2) 1 d D U P A 2
H32E H 0.7906 1.1676 0.6592 0.048 Uiso 0.404(2) 1 calc R . P A 2
H32F H 0.7289 1.2280 0.6906 0.048 Uiso 0.404(2) 1 calc R . P A 2
C323 C 0.6626(3) 1.1881(4) 0.63704(16) 0.0360(9) Uani 0.404(2) 1 d D U P A 2
H32K H 0.6686 1.2605 0.6272 0.043 Uiso 0.404(2) 1 calc R . P A 2
H32L H 0.6754 1.1412 0.6138 0.043 Uiso 0.404(2) 1 calc R . P A 2
C324 C 0.5671(2) 1.1701(3) 0.65099(11) 0.0357(8) Uani 0.404(2) 1 d D U P A 2
H32C H 0.5589 1.0952 0.6567 0.043 Uiso 0.404(2) 1 calc R . P A 2
H32D H 0.5577 1.2084 0.6769 0.043 Uiso 0.404(2) 1 calc R . P A 2
C325 C 0.4970(3) 1.2046(3) 0.61976(16) 0.0376(10) Uani 0.404(2) 1 d D U P A 2
H32G H 0.5195 1.1899 0.5920 0.045 Uiso 0.404(2) 1 calc R . P A 2
H32H H 0.4896 1.2808 0.6221 0.045 Uiso 0.404(2) 1 calc R . P A 2
B12 B 0.48475(13) 0.73303(16) 0.70423(8) 0.0499(5) Uani 1 1 d D . . . .
H12A H 0.4202(4) 0.6972(4) 0.7023(4) 0.075 Uiso 1 1 calc DGR . . . .
H12B H 0.4879(6) 0.7970(7) 0.6829(3) 0.075 Uiso 1 1 calc DGR . . . .
H12C H 0.4960(6) 0.7615(9) 0.7349(3) 0.075 Uiso 1 1 calc DGR . . . .
B13 B 0.32904(11) 0.71505(14) 0.49832(5) 0.0326(3) Uani 1 1 d D . . . .
H13A H 0.3270(6) 0.6432(6) 0.4813(2) 0.049 Uiso 1 1 calc DGR . . . .
H13B H 0.3964(5) 0.7314(9) 0.50760(8) 0.049 Uiso 1 1 calc DGR . . . .
H13C H 0.3046(5) 0.7774(7) 0.4793(2) 0.049 Uiso 1 1 calc DGR . . . .


_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
P2 O107 1.6323(9) . ?
P2 C109 1.8386(14) . ?
P2 C117 1.8079(14) . ?
P2 B2 1.9076(16) . ?
P3 O108 1.6270(9) . ?
P3 C113 1.8348(13) . ?
P3 C130 1.8090(14) . ?
P3 B3 1.9046(15) . ?
O107 C102 1.4001(15) . ?
O108 C106 1.3967(15) . ?
C101 C102 1.3850(17) . ?
C101 C106 1.3876(18) . ?
C102 C103 1.3848(18) . ?
C103 C104 1.3892(19) . ?
C104 C105 1.391(2) . ?
C105 C106 1.3835(19) . ?
C109 C110 1.531(2) . ?
C109 C111 1.5385(18) . ?
C109 C112 1.534(2) . ?
C113 C114 1.536(2) . ?
C113 C115 1.5337(19) . ?
C113 C116 1.5284(18) . ?
C117 C118 1.5356(19) . ?
C118 C119 1.518(2) . ?
C119 C120 1.533(2) . ?
C120 C121 1.518(2) . ?
C121 C122 1.527(2) . ?
C122 C123 1.526(2) . ?
C123 C124 1.533(2) . ?
C124 C125 1.521(2) . ?
C125 C126 1.526(2) . ?
C126 C127 1.5219(19) . ?
C127 C128 1.5238(19) . ?
C128 C129 1.5246(18) . ?
C129 C130 1.5291(18) . ?
P12 O207 1.6284(10) . ?
P12 C209 1.8331(15) . ?
P12 C217 1.8223(16) . ?
P12 B12 1.9010(18) . ?
P13 O208 1.6274(10) . ?
P13 C213 1.8353(14) . ?
P13 C230 1.8114(14) . ?
P13 B13 1.9043(15) . ?
O207 C202 1.3961(17) . ?
O208 C206 1.3965(16) . ?
C201 C202 1.3887(19) . ?
C201 C206 1.386(2) . ?
C202 C203 1.385(2) . ?
C203 C204 1.383(2) . ?
C204 C205 1.390(2) . ?
C205 C206 1.382(2) . ?
C209 C210 1.537(2) . ?
C209 C211 1.536(2) . ?
C209 C212 1.524(2) . ?
C213 C214 1.536(2) . ?
C213 C215 1.530(2) . ?
C213 C216 1.5272(18) . ?
C217 C218 1.554(3) . ?
C217 C318 1.620(3) . ?
C218 C219 1.499(3) . ?
C219 C220 1.553(4) . ?
C220 C221 1.521(4) . ?
C221 C222 1.521(3) . ?
C222 C223 1.531(4) . ?
C223 C224 1.530(4) . ?
C224 C225 1.532(3) . ?
C225 C226 1.502(3) . ?
C226 C227 1.525(2) . ?
C226 C325 1.592(4) . ?
C227 C228 1.524(2) . ?
C228 C229 1.5285(19) . ?
C229 C230 1.5291(19) . ?
C318 C319 1.546(4) . ?
C319 C320 1.527(5) . ?
C320 C321 1.502(5) . ?
C321 C322 1.537(4) . ?
C322 C323 1.538(5) . ?
C323 C324 1.534(5) . ?
C324 C325 1.528(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O107 P2 C109 104.72(5) . . ?
O107 P2 C117 98.49(6) . . ?
O107 P2 B2 118.07(6) . . ?
C109 P2 B2 113.33(7) . . ?
C117 P2 C109 107.86(7) . . ?
C117 P2 B2 112.92(7) . . ?
O108 P3 C113 102.09(6) . . ?
O108 P3 C130 102.84(6) . . ?
O108 P3 B3 116.19(6) . . ?
C113 P3 B3 115.28(7) . . ?
C130 P3 C113 106.58(6) . . ?
C130 P3 B3 112.48(7) . . ?
C102 O107 P2 127.71(8) . . ?
C106 O108 P3 123.96(8) . . ?
C102 C101 C106 118.00(11) . . ?
C101 C102 O107 121.67(11) . . ?
C103 C102 O107 116.58(11) . . ?
C103 C102 C101 121.60(12) . . ?
C102 C103 C104 119.03(12) . . ?
C103 C104 C105 120.77(13) . . ?
C106 C105 C104 118.52(12) . . ?
C101 C106 O108 116.91(11) . . ?
C105 C106 O108 120.96(12) . . ?
C105 C106 C101 122.07(12) . . ?
C110 C109 P2 107.93(10) . . ?
C110 C109 C111 109.25(12) . . ?
C110 C109 C112 109.93(12) . . ?
C111 C109 P2 108.96(10) . . ?
C112 C109 P2 110.64(10) . . ?
C112 C109 C111 110.10(13) . . ?
C114 C113 P3 107.85(9) . . ?
C115 C113 P3 107.62(10) . . ?
C115 C113 C114 110.08(13) . . ?
C116 C113 P3 112.01(9) . . ?
C116 C113 C114 109.10(12) . . ?
C116 C113 C115 110.13(12) . . ?
C118 C117 P2 113.60(10) . . ?
C119 C118 C117 111.90(12) . . ?
C118 C119 C120 113.96(13) . . ?
C121 C120 C119 114.68(14) . . ?
C120 C121 C122 111.79(12) . . ?
C123 C122 C121 114.53(13) . . ?
C122 C123 C124 114.94(12) . . ?
C125 C124 C123 113.88(13) . . ?
C124 C125 C126 114.58(12) . . ?
C127 C126 C125 113.09(13) . . ?
C126 C127 C128 113.94(12) . . ?
C127 C128 C129 111.39(11) . . ?
C128 C129 C130 113.10(11) . . ?
C129 C130 P3 112.93(9) . . ?
O207 P12 C209 105.36(6) . . ?
O207 P12 C217 98.19(8) . . ?
O207 P12 B12 117.36(9) . . ?
C209 P12 B12 114.39(9) . . ?
C217 P12 C209 105.67(7) . . ?
C217 P12 B12 114.06(8) . . ?
O208 P13 C213 102.22(6) . . ?
O208 P13 C230 102.50(6) . . ?
O208 P13 B13 116.25(7) . . ?
C213 P13 B13 115.13(7) . . ?
C230 P13 C213 106.71(6) . . ?
C230 P13 B13 112.65(7) . . ?
C202 O207 P12 128.25(8) . . ?
C206 O208 P13 123.77(8) . . ?
C206 C201 C202 117.98(13) . . ?
C201 C202 O207 122.50(13) . . ?
C203 C202 O207 115.95(12) . . ?
C203 C202 C201 121.47(13) . . ?
C204 C203 C202 119.05(13) . . ?
C203 C204 C205 120.88(14) . . ?
C206 C205 C204 118.66(14) . . ?
C201 C206 O208 116.89(12) . . ?
C205 C206 O208 121.12(13) . . ?
C205 C206 C201 121.94(13) . . ?
C210 C209 P12 108.11(10) . . ?
C211 C209 P12 108.25(12) . . ?
C211 C209 C210 109.18(14) . . ?
C212 C209 P12 111.70(11) . . ?
C212 C209 C210 109.57(14) . . ?
C212 C209 C211 109.97(14) . . ?
C214 C213 P13 108.04(10) . . ?
C215 C213 P13 107.79(11) . . ?
C215 C213 C214 110.48(14) . . ?
C216 C213 P13 111.59(10) . . ?
C216 C213 C214 108.66(12) . . ?
C216 C213 C215 110.26(13) . . ?
C218 C217 P12 116.54(14) . . ?
C318 C217 P12 109.31(15) . . ?
C219 C218 C217 108.2(2) . . ?
C218 C219 C220 113.3(3) . . ?
C221 C220 C219 111.2(3) . . ?
C220 C221 C222 115.6(2) . . ?
C221 C222 C223 113.8(2) . . ?
C224 C223 C222 114.4(2) . . ?
C223 C224 C225 114.0(2) . . ?
C226 C225 C224 112.0(2) . . ?
C225 C226 C227 114.30(16) . . ?
C227 C226 C325 109.6(2) . . ?
C228 C227 C226 115.39(13) . . ?
C227 C228 C229 111.22(12) . . ?
C228 C229 C230 113.65(12) . . ?
C229 C230 P13 112.76(9) . . ?
C319 C318 C217 109.0(2) . . ?
C320 C319 C318 110.1(3) . . ?
C321 C320 C319 110.6(4) . . ?
C320 C321 C322 114.9(3) . . ?
C321 C322 C323 116.4(4) . . ?
C324 C323 C322 112.5(4) . . ?
C325 C324 C323 113.9(4) . . ?
C324 C325 C226 115.7(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 7.402
_oxdiff_exptl_absorpt_empirical_full_min 0.544
####################################################################### 
# 
# 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_0555abc19s
_database_code_depnum_ccdc_archive 'CCDC 1972814'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
#====================================================================

_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C29 H49 O3 P2 Rh'
_chemical_formula_sum            'C29 H49 O3 P2 Rh'
_chemical_formula_weight         610.53
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Rh Rh 0.0927 3.6045 '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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   20.85015(15)
_cell_length_b                   10.67243(11)
_cell_length_c                   13.58703(12)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3023.41(5)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    14138
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.6650
_cell_measurement_theta_min      4.1080
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    5.770
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.02682
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   .
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.341
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1288
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
1 -7 -1 0.0326
-1 7 1 0.0242
-3 1 -9 0.1739
3 -1 9 0.1804
-14 0 0 0.0932
14 0 0 0.0932
9 1 -7 0.1382
-1 -1 9 0.1717

_exptl_crystal_recrystallization_method 'Crystals grown from TMS at 293 K'
_exptl_crystal_size_max          0.356
_exptl_crystal_size_mid          0.186
_exptl_crystal_size_min          0.064
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
0.6485 -6.8905 -0.8555 0.3667 -0.9303 -0.0013
-0.7646 6.9078 0.5259 -0.3661 0.9297 0.0397
-3.0338 0.5828 -8.5593 0.0091 0.0022 1.0000
3.0338 -0.5828 8.5593 -0.0091 -0.0022 -1.0000
-13.5154 -0.3434 0.0049 0.9102 0.3567 0.2104
13.5154 0.3434 -0.0049 -0.9102 -0.3567 -0.2104
8.8390 0.6925 -6.6190 -0.7436 -0.2989 0.5981
-0.6701 -0.7572 8.7528 0.2488 0.0888 -0.9645

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0556
_diffrn_reflns_av_unetI/netI     0.0360
_diffrn_reflns_Laue_measured_fraction_full 0.980
_diffrn_reflns_Laue_measured_fraction_max 0.980
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            19287
_diffrn_reflns_point_group_measured_fraction_full 0.843
_diffrn_reflns_point_group_measured_fraction_max 0.843
_diffrn_reflns_theta_full        70.071
_diffrn_reflns_theta_max         70.071
_diffrn_reflns_theta_min         6.516
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.980
_diffrn_measured_fraction_theta_max 0.980
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω   -126.00 -37.00   1.00    3.00    --  -37.40 178.00 -30.00   89
  2  ω    -71.00  44.00   1.00    3.00    --  -37.40  37.00 120.00  115
  3  ω   -117.00  -4.00   1.00    3.00    --  -37.40 -57.00 -60.00  113
  4  ω     61.00 131.00   1.00    3.00    --   37.40 178.00 -90.00   70
  5  ω     24.00 106.00   1.00   12.00    --  112.00 -94.00-120.00   82
  6  ω     98.00 178.00   1.00   12.00    --  112.00 124.00 -24.00   80
  7  ω     31.00 147.00   1.00   12.00    --  112.00 -61.00 -90.00  116
  8  ω   -126.00 -37.00   1.00    3.00    --  -37.40 178.00-120.00   89
  9  ω   -117.00  -4.00   1.00    3.00    --  -37.40 -57.00  90.00  113
 10  ω   -117.00  -4.00   1.00    3.00    --  -37.40 -57.00-180.00  113
 11  ω    -43.00  71.00   1.00    3.00    --   37.40 -57.00-150.00  114
 12  ω     79.00 178.00   1.00   12.00    --  112.00  45.00 150.00   99
 13  ω     77.00 178.00   1.00   12.00    --  112.00  61.00-150.00  101
 14  ω     79.00 178.00   1.00   12.00    --  112.00  45.00   0.00   99
 15  ω   -117.00 -37.00   1.00    3.00    --  -37.40 -57.00-150.00   80
 16  ω   -117.00  -4.00   1.00    3.00    --  -37.40 -57.00   0.00  113
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0657735000
_diffrn_orient_matrix_UB_12      -0.0616462000
_diffrn_orient_matrix_UB_13      0.0180528000
_diffrn_orient_matrix_UB_21      -0.0296836000
_diffrn_orient_matrix_UB_22      0.1298531000
_diffrn_orient_matrix_UB_23      0.0191074000
_diffrn_orient_matrix_UB_31      -0.0159255000
_diffrn_orient_matrix_UB_32      0.0123890000
_diffrn_orient_matrix_UB_33      -0.1103384000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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         0.645
_reflns_Friedel_fraction_full    0.694
_reflns_Friedel_fraction_max     0.694
_reflns_number_gt                4704
_reflns_number_total             4830
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         1.536
_refine_diff_density_min         -1.363
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 
;
 Classical Flack method preferred over Parsons because s.u. lower.
;
_refine_ls_abs_structure_Flack   -0.016(13)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         4830
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0474
_refine_ls_restrained_S_all      1.063
_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)+(0.1035P)²+0.4951P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1283
_refine_ls_wR_factor_ref         0.1297
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C119(H11W,H11X), C120(H12A,H12B), C121(H12C,
 H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L),
 C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,H12R), C129(H12S,H12T), C130(H13A,
 H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
2.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Rh1 Rh -1.34766(2) -1.62375(3) -1.47893(6) 0.01280(17) Uani 1 1 d . . . . .
P2 P -1.45519(7) -1.63375(13) -1.45379(12) 0.0160(4) Uani 1 1 d . . . . .
P3 P -1.25227(6) -1.52951(13) -1.51621(12) 0.0135(3) Uani 1 1 d . . . . .
O5 O -1.3154(3) -1.8936(5) -1.4367(5) 0.0366(14) Uani 1 1 d . . . . .
O107 O -1.48042(17) -1.4875(4) -1.4415(4) 0.0225(9) Uani 1 1 d . . . . .
O108 O -1.2583(2) -1.3838(4) -1.4721(5) 0.0190(10) Uani 1 1 d . . . . .
C4 C -1.3267(2) -1.7936(5) -1.4618(5) 0.0182(13) Uani 1 1 d . . . . .
C101 C -1.3692(2) -1.4393(6) -1.4591(4) 0.0151(11) Uani 1 1 d . . . . .
C102 C -1.4313(3) -1.3982(6) -1.4412(5) 0.0186(12) Uani 1 1 d . . . . .
C103 C -1.4465(3) -1.2742(6) -1.4185(6) 0.0263(14) Uani 1 1 d . . . . .
H103 H -1.4894 -1.2494 -1.4055 0.032 Uiso 1 1 calc R . . . .
C104 C -1.3970(3) -1.1891(6) -1.4157(6) 0.0276(14) Uani 1 1 d . . . . .
H104 H -1.4065 -1.1043 -1.4000 0.033 Uiso 1 1 calc R . . . .
C105 C -1.3342(3) -1.2216(6) -1.4345(5) 0.0236(13) Uani 1 1 d . . . . .
H105 H -1.3009 -1.1608 -1.4331 0.028 Uiso 1 1 calc R . . . .
C106 C -1.3212(3) -1.3472(6) -1.4557(5) 0.0170(13) Uani 1 1 d . . . . .
C109 C -1.4890(3) -1.7059(6) -1.3411(5) 0.0218(13) Uani 1 1 d . . . . .
C110 C -1.4517(3) -1.6498(9) -1.2547(6) 0.0335(17) Uani 1 1 d . . . . .
H11A H -1.4562 -1.5584 -1.2554 0.050 Uiso 1 1 calc GR . . . .
H11B H -1.4063 -1.6720 -1.2606 0.050 Uiso 1 1 calc GR . . . .
H11C H -1.4688 -1.6830 -1.1928 0.050 Uiso 1 1 calc GR . . . .
C111 C -1.4777(4) -1.8469(7) -1.3443(8) 0.042(2) Uani 1 1 d . . . . .
H11D H -1.4324 -1.8636 -1.3585 0.063 Uiso 1 1 calc GR . . . .
H11E H -1.5044 -1.8842 -1.3960 0.063 Uiso 1 1 calc GR . . . .
H11F H -1.4890 -1.8837 -1.2806 0.063 Uiso 1 1 calc GR . . . .
C112 C -1.5603(3) -1.6774(7) -1.3295(7) 0.0327(16) Uani 1 1 d . . . . .
H11G H -1.5842 -1.7169 -1.3832 0.049 Uiso 1 1 calc GR . . . .
H11H H -1.5670 -1.5866 -1.3313 0.049 Uiso 1 1 calc GR . . . .
H11I H -1.5754 -1.7105 -1.2663 0.049 Uiso 1 1 calc GR . . . .
C113 C -1.2361(2) -1.4964(6) -1.6486(5) 0.0169(11) Uani 1 1 d . . . . .
C114 C -1.2932(3) -1.4229(7) -1.6894(5) 0.0272(13) Uani 1 1 d . . . . .
H11J H -1.2985 -1.3452 -1.6519 0.041 Uiso 1 1 calc GR . . . .
H11K H -1.3322 -1.4737 -1.6836 0.041 Uiso 1 1 calc GR . . . .
H11L H -1.2855 -1.4028 -1.7588 0.041 Uiso 1 1 calc GR . . . .
C115 C -1.2312(3) -1.6201(5) -1.7062(5) 0.0182(13) Uani 1 1 d . . . . .
H11M H -1.2720 -1.6653 -1.7016 0.027 Uiso 1 1 calc GR . . . .
H11N H -1.1969 -1.6717 -1.6782 0.027 Uiso 1 1 calc GR . . . .
H11O H -1.2217 -1.6021 -1.7754 0.027 Uiso 1 1 calc GR . . . .
C116 C -1.1748(3) -1.4180(6) -1.6609(5) 0.0243(13) Uani 1 1 d . . . . .
H11P H -1.1375 -1.4678 -1.6407 0.036 Uiso 1 1 calc GR . . . .
H11Q H -1.1777 -1.3427 -1.6198 0.036 Uiso 1 1 calc GR . . . .
H11R H -1.1701 -1.3935 -1.7300 0.036 Uiso 1 1 calc GR . . . .
C117 C -1.5076(3) -1.6886(7) -1.5514(5) 0.0279(14) Uani 1 1 d . . . . .
H11S H -1.5123 -1.7805 -1.5450 0.033 Uiso 1 1 calc R . . . .
H11T H -1.5506 -1.6512 -1.5413 0.033 Uiso 1 1 calc R . . . .
C118 C -1.4860(4) -1.6593(8) -1.6561(6) 0.0347(16) Uani 1 1 d . . . . .
H11U H -1.4743 -1.5695 -1.6597 0.042 Uiso 1 1 calc R . . . .
H11V H -1.5227 -1.6729 -1.7011 0.042 Uiso 1 1 calc R . . . .
C119 C -1.4289(3) -1.7369(8) -1.6932(5) 0.0330(17) Uani 1 1 d . . . . .
H11W H -1.3911 -1.7188 -1.6514 0.040 Uiso 1 1 calc R . . . .
H11X H -1.4185 -1.7105 -1.7611 0.040 Uiso 1 1 calc R . . . .
C120 C -1.4413(5) -1.8789(8) -1.6925(10) 0.049(3) Uani 1 1 d . . . . .
H12A H -1.4441 -1.9068 -1.6231 0.058 Uiso 1 1 calc R . . . .
H12B H -1.4837 -1.8944 -1.7232 0.058 Uiso 1 1 calc R . . . .
C121 C -1.3921(4) -1.9600(9) -1.7445(7) 0.050(2) Uani 1 1 d . . . . .
H12C H -1.4075 -2.0477 -1.7458 0.059 Uiso 1 1 calc R . . . .
H12D H -1.3876 -1.9312 -1.8134 0.059 Uiso 1 1 calc R . . . .
C122 C -1.3286(4) -1.9557(10) -1.6960(8) 0.050(2) Uani 1 1 d . . . . .
H12E H -1.3337 -1.9815 -1.6265 0.060 Uiso 1 1 calc R . . . .
H12F H -1.3130 -1.8681 -1.6964 0.060 Uiso 1 1 calc R . . . .
C123 C -1.2766(4) -2.0416(8) -1.7457(7) 0.0414(19) Uani 1 1 d . . . . .
H12G H -1.2886 -2.1306 -1.7367 0.050 Uiso 1 1 calc R . . . .
H12H H -1.2752 -2.0242 -1.8172 0.050 Uiso 1 1 calc R . . . .
C124 C -1.2107(4) -2.0195(8) -1.7018(6) 0.0381(19) Uani 1 1 d . . . . .
H12I H -1.1993 -1.9300 -1.7096 0.046 Uiso 1 1 calc R . . . .
H12J H -1.1788 -2.0695 -1.7388 0.046 Uiso 1 1 calc R . . . .
C125 C -1.2067(4) -2.0544(7) -1.5926(6) 0.0349(16) Uani 1 1 d . . . . .
H12K H -1.2183 -2.1438 -1.5850 0.042 Uiso 1 1 calc R . . . .
H12L H -1.2386 -2.0042 -1.5557 0.042 Uiso 1 1 calc R . . . .
C126 C -1.1400(4) -2.0331(8) -1.5465(7) 0.0407(19) Uani 1 1 d . . . . .
H12M H -1.1411 -2.0620 -1.4773 0.049 Uiso 1 1 calc R . . . .
H12N H -1.1084 -2.0856 -1.5820 0.049 Uiso 1 1 calc R . . . .
C127 C -1.1168(4) -1.8976(7) -1.5483(7) 0.0358(18) Uani 1 1 d . . . . .
H12O H -1.0753 -1.8931 -1.5131 0.043 Uiso 1 1 calc R . . . .
H12P H -1.1088 -1.8735 -1.6176 0.043 Uiso 1 1 calc R . . . .
C128 C -1.1622(3) -1.8016(7) -1.5030(5) 0.0279(16) Uani 1 1 d . . . . .
H12Q H -1.2024 -1.7990 -1.5419 0.034 Uiso 1 1 calc R . . . .
H12R H -1.1733 -1.8281 -1.4353 0.034 Uiso 1 1 calc R . . . .
C129 C -1.1331(3) -1.6718(7) -1.4998(5) 0.0273(15) Uani 1 1 d . . . . .
H12S H -1.1207 -1.6482 -1.5676 0.033 Uiso 1 1 calc R . . . .
H12T H -1.0933 -1.6760 -1.4603 0.033 Uiso 1 1 calc R . . . .
C130 C -1.1751(3) -1.5675(6) -1.4579(4) 0.0208(13) Uani 1 1 d . . . . .
H13A H -1.1490 -1.4900 -1.4576 0.025 Uiso 1 1 calc R . . . .
H13B H -1.1840 -1.5888 -1.3883 0.025 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Rh1 P2 2.2704(15) . ?
Rh1 P3 2.2856(13) . ?
Rh1 C4 1.879(6) . ?
Rh1 C101 2.037(6) . ?
P2 O107 1.656(4) . ?
P2 C109 1.852(7) . ?
P2 C117 1.816(7) . ?
P3 O108 1.671(4) . ?
P3 C113 1.864(6) . ?
P3 C130 1.839(6) . ?
O5 C4 1.145(7) . ?
O107 C102 1.399(8) . ?
O108 C106 1.385(7) . ?
C101 C102 1.389(8) . ?
C101 C106 1.404(8) . ?
C102 C103 1.396(9) . ?
C103 C104 1.375(9) . ?
C104 C105 1.378(9) . ?
C105 C106 1.397(9) . ?
C109 C110 1.530(10) . ?
C109 C111 1.525(9) . ?
C109 C112 1.525(7) . ?
C113 C114 1.531(8) . ?
C113 C115 1.538(8) . ?
C113 C116 1.536(8) . ?
C117 C118 1.525(11) . ?
C118 C119 1.534(11) . ?
C119 C120 1.537(12) . ?
C120 C121 1.517(12) . ?
C121 C122 1.479(12) . ?
C122 C123 1.573(12) . ?
C123 C124 1.516(12) . ?
C124 C125 1.532(12) . ?
C125 C126 1.542(11) . ?
C126 C127 1.525(12) . ?
C127 C128 1.525(9) . ?
C128 C129 1.512(10) . ?
C129 C130 1.526(9) . ?

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 Rh1 P3 155.98(5) . . ?
C4 Rh1 P2 99.53(16) . . ?
C4 Rh1 P3 104.46(16) . . ?
C4 Rh1 C101 165.3(3) . . ?
C101 Rh1 P2 78.93(15) . . ?
C101 Rh1 P3 78.22(15) . . ?
O107 P2 Rh1 106.54(14) . . ?
O107 P2 C109 100.8(3) . . ?
O107 P2 C117 100.7(3) . . ?
C109 P2 Rh1 121.29(19) . . ?
C117 P2 Rh1 120.0(2) . . ?
C117 P2 C109 103.9(3) . . ?
O108 P3 Rh1 105.32(17) . . ?
O108 P3 C113 100.6(3) . . ?
O108 P3 C130 96.7(3) . . ?
C113 P3 Rh1 117.07(18) . . ?
C130 P3 Rh1 124.7(2) . . ?
C130 P3 C113 107.4(3) . . ?
C102 O107 P2 114.2(4) . . ?
C106 O108 P3 113.1(4) . . ?
O5 C4 Rh1 169.7(6) . . ?
C102 C101 Rh1 122.3(4) . . ?
C102 C101 C106 116.0(5) . . ?
C106 C101 Rh1 121.6(4) . . ?
C101 C102 O107 117.8(5) . . ?
C101 C102 C103 123.3(6) . . ?
C103 C102 O107 118.7(5) . . ?
C104 C103 C102 117.5(6) . . ?
C103 C104 C105 122.7(6) . . ?
C104 C105 C106 117.7(6) . . ?
O108 C106 C101 118.2(5) . . ?
O108 C106 C105 119.2(5) . . ?
C105 C106 C101 122.6(5) . . ?
C110 C109 P2 106.2(5) . . ?
C111 C109 P2 109.2(5) . . ?
C111 C109 C110 109.2(7) . . ?
C111 C109 C112 110.5(5) . . ?
C112 C109 P2 112.0(5) . . ?
C112 C109 C110 109.7(6) . . ?
C114 C113 P3 107.8(4) . . ?
C114 C113 C115 107.9(5) . . ?
C114 C113 C116 109.2(5) . . ?
C115 C113 P3 109.9(4) . . ?
C116 C113 P3 111.0(4) . . ?
C116 C113 C115 111.0(5) . . ?
C118 C117 P2 115.9(5) . . ?
C117 C118 C119 115.2(6) . . ?
C118 C119 C120 113.6(7) . . ?
C121 C120 C119 116.4(9) . . ?
C122 C121 C120 112.4(8) . . ?
C121 C122 C123 114.1(8) . . ?
C124 C123 C122 111.5(7) . . ?
C123 C124 C125 113.1(7) . . ?
C124 C125 C126 114.0(7) . . ?
C127 C126 C125 114.7(6) . . ?
C128 C127 C126 115.7(7) . . ?
C129 C128 C127 112.2(6) . . ?
C128 C129 C130 116.7(5) . . ?
C129 C130 P3 120.1(4) . . ?

_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 17.977
_oxdiff_exptl_absorpt_empirical_full_min 0.349
####################################################################### 
# 
# 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_0317abc17s
_database_code_depnum_ccdc_archive 'CCDC 1972817'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C31 H53 Ir O P2'
_chemical_formula_sum            'C31 H53 Ir O P2'
_chemical_formula_weight         695.87
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

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

_cell_length_a                   10.91013(11)
_cell_length_b                   13.58277(17)
_cell_length_c                   20.9292(2)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3101.49(6)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    49625
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      33.3560
_cell_measurement_theta_min      3.5750
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    4.429
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.73805
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_absorpt_special_details   .
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    1.490
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1416
_exptl_crystal_recrystallization_method 'Crystals grown from neohexane at 243 K'
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0529
_diffrn_reflns_av_unetI/netI     0.0209
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            120512
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.573
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         3.086
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -17.00 104.00   1.00    2.00    --   24.25  19.00-150.00  121
  2  ω     -8.00 100.00   1.00    2.00    --   24.25  77.00 -90.00  108
  3  ω     35.00 113.00   1.00    2.00    --   24.25 178.00 -60.00   78
  4  ω   -110.00 -55.00   1.00    2.00    --  -23.31 178.00-120.00   55
  5  ω   -112.00 -57.00   1.00    2.00    --  -23.31-178.00 -30.00   55
  6  ω    -64.00  57.00   1.00    2.00    --  -23.31  19.00 150.00  121
  7  ω     -4.00  97.00   1.00    2.00    --   24.25  57.00-150.00  101
  8  ω    -20.00  65.00   1.00    2.00    --   24.25 -99.00 -90.00   85
  9  ω     -4.00  97.00   1.00    2.00    --   24.25  57.00  60.00  101
 10  ω    -87.00 -31.00   1.00    2.00    --  -23.31 138.00  51.00   56
 11  ω    -99.00   9.00   1.00    2.00    --  -23.31 -77.00-120.00  108
 12  ω    -98.00   1.00   1.00    2.00    --  -23.31 -37.00  30.00   99
 13  ω    -99.00   9.00   1.00    2.00    --  -23.31 -77.00   0.00  108
 14  ω     13.00  94.00   1.00    2.00    --   24.25-147.00  86.00   81
 15  ω     10.00  88.00   1.00    2.00    --   24.25-138.00 -10.00   78
 16  ω      1.00  80.00   1.00    2.00    --   24.25-124.00-108.00   79
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0005043000
_diffrn_orient_matrix_UB_12      -0.0184614000
_diffrn_orient_matrix_UB_13      -0.0317024000
_diffrn_orient_matrix_UB_21      -0.0056307000
_diffrn_orient_matrix_UB_22      0.0486502000
_diffrn_orient_matrix_UB_23      -0.0119535000
_diffrn_orient_matrix_UB_31      0.0647708000
_diffrn_orient_matrix_UB_32      0.0043659000
_diffrn_orient_matrix_UB_33      -0.0007968000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.800
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                8426
_reflns_number_total             8680
_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 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.801
_refine_diff_density_min         -0.364
_refine_diff_density_rms         0.059
_refine_ls_abs_structure_details 
;
 Flack x determined using 3663 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0172(19)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.070
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     322
_refine_ls_number_reflns         8680
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0166
_refine_ls_R_factor_gt           0.0154
_refine_ls_restrained_S_all      1.070
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0147P)²+0.4882P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0338
_refine_ls_wR_factor_ref         0.0343
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11S,H11T), C118(H11U,H11V), C119(H11W,
 H11X), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F), C123(H12G,H12H),
 C124(H12I,H12J), C125(H12K,H12L), C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,
 H12R), C129(H12S,H12T), C130(H13A,H13B)
2.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
2.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Ir1 Ir -0.89377(2) -0.12167(2) -0.69974(2) 0.01571(3) Uani 1 1 d . . . . .
P2 P -0.83591(6) -0.08488(5) -0.59773(3) 0.01687(13) Uani 1 1 d . . . . .
P3 P -1.00765(6) -0.13209(6) -0.79060(3) 0.01801(13) Uani 1 1 d . . . . .
O5 O -0.6491(2) -0.18917(17) -0.75046(12) 0.0320(5) Uani 1 1 d . . . . .
C4 C -0.7418(3) -0.1597(2) -0.73178(13) 0.0197(6) Uani 1 1 d . . . . .
C101 C -1.0682(2) -0.1002(2) -0.66143(14) 0.0195(6) Uani 1 1 d . . . . .
C102 C -1.0846(3) -0.0611(2) -0.59946(14) 0.0208(6) Uani 1 1 d . . . . .
C103 C -1.2005(3) -0.0532(2) -0.57228(15) 0.0247(6) Uani 1 1 d . . . . .
H103 H -1.2093 -0.0282 -0.5302 0.030 Uiso 1 1 calc R . . . .
C104 C -1.3028(3) -0.0818(2) -0.60642(16) 0.0281(7) Uani 1 1 d . . . . .
H104 H -1.3818 -0.0761 -0.5877 0.034 Uiso 1 1 calc R . . . .
C105 C -1.2910(2) -0.1189(3) -0.66790(15) 0.0279(6) Uani 1 1 d . . . . .
H105 H -1.3619 -0.1376 -0.6913 0.033 Uiso 1 1 calc R . . . .
C106 C -1.1751(2) -0.1286(2) -0.69530(13) 0.0223(5) Uani 1 1 d . . . . .
C107 C -0.9727(3) -0.0243(2) -0.56476(14) 0.0213(6) Uani 1 1 d . . . . .
H10A H -0.9798 -0.0390 -0.5186 0.026 Uiso 1 1 calc R . . . .
H10B H -0.9656 0.0480 -0.5699 0.026 Uiso 1 1 calc R . . . .
C108 C -1.1599(3) -0.1692(2) -0.76202(15) 0.0252(7) Uani 1 1 d . . . . .
H10C H -1.2243 -0.1426 -0.7905 0.030 Uiso 1 1 calc R . . . .
H10D H -1.1668 -0.2419 -0.7615 0.030 Uiso 1 1 calc R . . . .
C109 C -0.8017(3) -0.1893(2) -0.54290(14) 0.0202(6) Uani 1 1 d . . . . .
C110 C -0.9186(3) -0.2506(2) -0.53662(16) 0.0293(7) Uani 1 1 d . . . . .
H11A H -0.9828 -0.2109 -0.5164 0.044 Uiso 1 1 calc GR . . . .
H11B H -0.9021 -0.3088 -0.5103 0.044 Uiso 1 1 calc GR . . . .
H11C H -0.9459 -0.2715 -0.5791 0.044 Uiso 1 1 calc GR . . . .
C111 C -0.7015(3) -0.2521(2) -0.57414(16) 0.0263(7) Uani 1 1 d . . . . .
H11D H -0.7306 -0.2762 -0.6156 0.039 Uiso 1 1 calc GR . . . .
H11E H -0.6823 -0.3082 -0.5465 0.039 Uiso 1 1 calc GR . . . .
H11F H -0.6278 -0.2121 -0.5803 0.039 Uiso 1 1 calc GR . . . .
C112 C -0.7597(3) -0.1555(3) -0.47665(15) 0.0304(7) Uani 1 1 d . . . . .
H11G H -0.6818 -0.1201 -0.4804 0.046 Uiso 1 1 calc GR . . . .
H11H H -0.7487 -0.2130 -0.4490 0.046 Uiso 1 1 calc GR . . . .
H11I H -0.8218 -0.1118 -0.4581 0.046 Uiso 1 1 calc GR . . . .
C113 C -1.0296(3) -0.0119(2) -0.83285(14) 0.0224(6) Uani 1 1 d . . . . .
C114 C -1.1060(3) 0.0561(2) -0.78964(14) 0.0311(7) Uani 1 1 d . . . . .
H11J H -1.1890 0.0294 -0.7853 0.047 Uiso 1 1 calc GR . . . .
H11K H -1.1101 0.1219 -0.8087 0.047 Uiso 1 1 calc GR . . . .
H11L H -1.0676 0.0602 -0.7474 0.047 Uiso 1 1 calc GR . . . .
C115 C -0.9032(3) 0.0369(2) -0.84197(16) 0.0302(7) Uani 1 1 d . . . . .
H11M H -0.8616 0.0418 -0.8006 0.045 Uiso 1 1 calc GR . . . .
H11N H -0.9141 0.1030 -0.8599 0.045 Uiso 1 1 calc GR . . . .
H11O H -0.8536 -0.0029 -0.8712 0.045 Uiso 1 1 calc GR . . . .
C116 C -1.0933(3) -0.0259(2) -0.89720(14) 0.0293(7) Uani 1 1 d . . . . .
H11P H -1.0375 -0.0590 -0.9269 0.044 Uiso 1 1 calc GR . . . .
H11Q H -1.1164 0.0385 -0.9146 0.044 Uiso 1 1 calc GR . . . .
H11R H -1.1670 -0.0661 -0.8914 0.044 Uiso 1 1 calc GR . . . .
C117 C -0.7128(3) 0.0046(2) -0.58192(15) 0.0244(6) Uani 1 1 d . . . . .
H11S H -0.7274 0.0353 -0.5397 0.029 Uiso 1 1 calc R . . . .
H11T H -0.6338 -0.0310 -0.5796 0.029 Uiso 1 1 calc R . . . .
C118 C -0.7021(3) 0.0866(2) -0.63240(15) 0.0257(6) Uani 1 1 d . . . . .
H11U H -0.7816 0.0938 -0.6547 0.031 Uiso 1 1 calc R . . . .
H11V H -0.6838 0.1498 -0.6108 0.031 Uiso 1 1 calc R . . . .
C119 C -0.6020(3) 0.0650(2) -0.68136(14) 0.0255(6) Uani 1 1 d . . . . .
H11W H -0.5218 0.0639 -0.6592 0.031 Uiso 1 1 calc R . . . .
H11X H -0.6161 -0.0013 -0.6995 0.031 Uiso 1 1 calc R . . . .
C120 C -0.5959(3) 0.1387(2) -0.73553(15) 0.0278(6) Uani 1 1 d . . . . .
H12A H -0.5774 0.2045 -0.7176 0.033 Uiso 1 1 calc R . . . .
H12B H -0.6773 0.1423 -0.7562 0.033 Uiso 1 1 calc R . . . .
C121 C -0.4999(3) 0.1140(2) -0.78628(14) 0.0286(6) Uani 1 1 d . . . . .
H12C H -0.5014 0.1657 -0.8196 0.034 Uiso 1 1 calc R . . . .
H12D H -0.4177 0.1151 -0.7662 0.034 Uiso 1 1 calc R . . . .
C122 C -0.5192(3) 0.0148(2) -0.81767(15) 0.0276(7) Uani 1 1 d . . . . .
H12E H -0.5001 -0.0375 -0.7863 0.033 Uiso 1 1 calc R . . . .
H12F H -0.6068 0.0083 -0.8294 0.033 Uiso 1 1 calc R . . . .
C123 C -0.4420(3) -0.0010(2) -0.87671(15) 0.0252(7) Uani 1 1 d . . . . .
H12G H -0.3562 0.0174 -0.8669 0.030 Uiso 1 1 calc R . . . .
H12H H -0.4716 0.0434 -0.9109 0.030 Uiso 1 1 calc R . . . .
C124 C -0.4441(3) -0.1068(3) -0.90153(16) 0.0296(7) Uani 1 1 d . . . . .
H12I H -0.3900 -0.1113 -0.9394 0.035 Uiso 1 1 calc R . . . .
H12J H -0.4101 -0.1507 -0.8682 0.035 Uiso 1 1 calc R . . . .
C125 C -0.5708(3) -0.1433(2) -0.91978(15) 0.0264(7) Uani 1 1 d . . . . .
H12K H -0.6263 -0.1333 -0.8830 0.032 Uiso 1 1 calc R . . . .
H12L H -0.6017 -0.1024 -0.9554 0.032 Uiso 1 1 calc R . . . .
C126 C -0.5770(3) -0.2498(3) -0.9395(2) 0.0367(8) Uani 1 1 d . . . . .
H12M H -0.5577 -0.2910 -0.9018 0.044 Uiso 1 1 calc R . . . .
H12N H -0.5125 -0.2619 -0.9718 0.044 Uiso 1 1 calc R . . . .
C127 C -0.6996(3) -0.2843(3) -0.96704(17) 0.0328(8) Uani 1 1 d . . . . .
H12O H -0.7264 -0.2356 -0.9993 0.039 Uiso 1 1 calc R . . . .
H12P H -0.6858 -0.3474 -0.9896 0.039 Uiso 1 1 calc R . . . .
C128 C -0.8043(3) -0.2990(3) -0.91949(17) 0.0331(7) Uani 1 1 d . . . . .
H12Q H -0.8727 -0.3321 -0.9420 0.040 Uiso 1 1 calc R . . . .
H12R H -0.7757 -0.3441 -0.8855 0.040 Uiso 1 1 calc R . . . .
C129 C -0.8538(3) -0.2072(2) -0.88824(15) 0.0253(6) Uani 1 1 d . . . . .
H12S H -0.8679 -0.1566 -0.9215 0.030 Uiso 1 1 calc R . . . .
H12T H -0.7915 -0.1811 -0.8583 0.030 Uiso 1 1 calc R . . . .
C130 C -0.9737(3) -0.2245(2) -0.85166(15) 0.0236(6) Uani 1 1 d . . . . .
H13A H -0.9697 -0.2900 -0.8309 0.028 Uiso 1 1 calc R . . . .
H13B H -1.0421 -0.2260 -0.8827 0.028 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 P2 2.2817(7) . ?
Ir1 P3 2.2760(7) . ?
Ir1 C4 1.862(3) . ?
Ir1 C101 2.085(3) . ?
P2 C107 1.838(3) . ?
P2 C109 1.863(3) . ?
P2 C117 1.842(3) . ?
P3 C108 1.836(3) . ?
P3 C113 1.872(3) . ?
P3 C130 1.829(3) . ?
O5 C4 1.156(3) . ?
C101 C102 1.413(4) . ?
C101 C106 1.418(4) . ?
C102 C103 1.391(4) . ?
C102 C107 1.506(4) . ?
C103 C104 1.381(5) . ?
C104 C105 1.387(5) . ?
C105 C106 1.395(4) . ?
C106 C108 1.511(4) . ?
C109 C110 1.529(4) . ?
C109 C111 1.532(4) . ?
C109 C112 1.531(4) . ?
C113 C114 1.538(4) . ?
C113 C115 1.542(4) . ?
C113 C116 1.528(4) . ?
C117 C118 1.540(4) . ?
C118 C119 1.526(4) . ?
C119 C120 1.514(4) . ?
C120 C121 1.529(4) . ?
C121 C122 1.514(4) . ?
C122 C123 1.511(4) . ?
C123 C124 1.528(5) . ?
C124 C125 1.517(4) . ?
C125 C126 1.506(5) . ?
C126 C127 1.529(5) . ?
C127 C128 1.528(5) . ?
C128 C129 1.508(4) . ?
C129 C130 1.534(4) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
P3 Ir1 P2 161.16(2) . . ?
C4 Ir1 P2 98.70(9) . . ?
C4 Ir1 P3 99.67(9) . . ?
C4 Ir1 C101 171.91(12) . . ?
C101 Ir1 P2 82.07(8) . . ?
C101 Ir1 P3 80.32(8) . . ?
C107 P2 Ir1 102.99(10) . . ?
C107 P2 C109 105.82(14) . . ?
C107 P2 C117 103.22(14) . . ?
C109 P2 Ir1 117.72(10) . . ?
C117 P2 Ir1 120.97(10) . . ?
C117 P2 C109 104.24(14) . . ?
C108 P3 Ir1 103.81(10) . . ?
C108 P3 C113 106.13(14) . . ?
C113 P3 Ir1 114.22(10) . . ?
C130 P3 Ir1 121.04(11) . . ?
C130 P3 C108 102.86(14) . . ?
C130 P3 C113 107.12(14) . . ?
O5 C4 Ir1 175.7(3) . . ?
C102 C101 Ir1 121.4(2) . . ?
C102 C101 C106 117.2(2) . . ?
C106 C101 Ir1 121.3(2) . . ?
C101 C102 C107 117.7(2) . . ?
C103 C102 C101 121.3(3) . . ?
C103 C102 C107 121.0(3) . . ?
C104 C103 C102 120.1(3) . . ?
C103 C104 C105 120.5(3) . . ?
C104 C105 C106 120.0(3) . . ?
C101 C106 C108 118.1(2) . . ?
C105 C106 C101 121.0(3) . . ?
C105 C106 C108 120.9(3) . . ?
C102 C107 P2 109.2(2) . . ?
C106 C108 P3 107.46(19) . . ?
C110 C109 P2 107.5(2) . . ?
C110 C109 C111 109.2(3) . . ?
C110 C109 C112 109.6(3) . . ?
C111 C109 P2 107.7(2) . . ?
C112 C109 P2 112.9(2) . . ?
C112 C109 C111 109.9(2) . . ?
C114 C113 P3 108.4(2) . . ?
C114 C113 C115 107.4(3) . . ?
C115 C113 P3 108.6(2) . . ?
C116 C113 P3 111.5(2) . . ?
C116 C113 C114 110.2(3) . . ?
C116 C113 C115 110.6(3) . . ?
C118 C117 P2 114.2(2) . . ?
C119 C118 C117 112.1(3) . . ?
C120 C119 C118 114.0(2) . . ?
C119 C120 C121 113.9(3) . . ?
C122 C121 C120 113.6(3) . . ?
C123 C122 C121 113.8(3) . . ?
C122 C123 C124 113.8(3) . . ?
C125 C124 C123 114.0(3) . . ?
C126 C125 C124 115.1(3) . . ?
C125 C126 C127 115.9(3) . . ?
C128 C127 C126 116.6(3) . . ?
C129 C128 C127 116.2(3) . . ?
C128 C129 C130 113.2(3) . . ?
C129 C130 P3 114.6(2) . . ?

_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 1.336
_oxdiff_exptl_absorpt_empirical_full_min 0.755
####################################################################### 
# 
# 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_0554abc19s
_database_code_depnum_ccdc_archive 'CCDC 1972818'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;
#====================================================================

_audit_creation_date             2019-10-01
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C29 H49 Ir O3 P2'
_chemical_formula_sum            'C29 H49 Ir O3 P2'
_chemical_formula_weight         699.82
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Ir Ir -4.7710 6.5667 '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           29
_space_group_name_H-M_alt        'P c a 21'
_space_group_name_Hall           'P 2c -2ac'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, z+1/2'
'x+1/2, -y, z'
'-x+1/2, y, z+1/2'

_cell_length_a                   20.8772(2)
_cell_length_b                   10.65296(8)
_cell_length_c                   13.56659(11)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3017.26(4)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    18690
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      73.5080
_cell_measurement_theta_min      3.8720
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    9.772
_exptl_absorpt_correction_T_max  0.848
_exptl_absorpt_correction_T_min  0.190
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.40.57a (Rigaku Oxford Diffraction, 2019)
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            'dark yellow'
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1416
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
2 -7 2 0.0484
-12 -1 -3 0.1107
-2 7 -1 0.0372
13 1 -2 0.0990
-1 1 9 0.1236
-4 1 8 0.1222
-12 -1 4 0.1171
-10 -2 -5 0.0985
5 -1 -8 0.1479
8 5 0 0.0619
-4 -6 1 0.0682
0 -7 3 0.0599
0 7 -3 0.0542
0 7 3 0.0698
10 -5 0 0.0803
4 -6 -2 0.0847
-8 -5 -4 0.0880
6 6 -1 0.0400

_exptl_crystal_recrystallization_method 'Crystals grown from TMS at 293 K'
_exptl_crystal_size_max          0.304
_exptl_crystal_size_mid          0.224
_exptl_crystal_size_min          0.088
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
2.3580 -6.6987 1.5607 0.0436 0.9988 -0.0204
-12.3261 -1.4768 -3.1307 0.0072 -0.0352 -0.9994
-1.9792 6.7439 -1.4644 -0.0438 -0.9977 0.0511
12.9530 0.9209 -2.3124 -0.5994 0.0333 0.7997
-0.8646 1.1907 8.6570 0.9406 -0.0378 0.3373
-4.3703 0.7933 8.2767 0.9963 -0.0426 0.0746
-11.8024 -0.5187 4.2825 0.7766 -0.0394 -0.6287
-10.0364 -1.7813 -5.4588 -0.3035 0.0046 -0.9528
5.3153 -0.6692 -8.0586 -0.9991 0.0434 0.0015
8.2470 5.4847 0.1614 -0.1714 -0.6371 0.7515
-4.4056 -6.4383 1.4598 0.2255 0.8563 -0.4646
0.0947 -6.5279 2.9062 0.2496 0.9621 -0.1100
-0.1669 6.5220 -2.9262 -0.2497 -0.9627 0.1042
0.1816 6.5591 2.7852 0.3390 -0.8688 0.3609
9.7907 -4.7810 -0.1241 -0.3268 0.8178 0.4738
4.1188 -6.4175 -1.8998 -0.3662 0.9299 -0.0340
-8.1263 -4.7717 -3.5618 -0.1825 0.4834 -0.8562
6.3591 6.0035 -1.4224 -0.2800 -0.7647 0.5803

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0356
_diffrn_reflns_av_unetI/netI     0.0261
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            25010
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        70.073
_diffrn_reflns_theta_max         70.073
_diffrn_reflns_theta_min         6.526
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -87.00  -6.00   1.00    1.00    --  -41.82 125.00 -90.00   81
  2  ω      6.00  83.00   1.00    1.00    --   41.82 -99.00   0.00   77
  3  ω     14.00 115.00   1.00    1.00    --   41.82  57.00-120.00  101
  4  ω     27.00  98.00   1.00    1.00    --   41.82-125.00  90.00   71
  5  ω     97.00 178.00   1.00    1.20    --  107.00 125.00 -90.00   81
  6  ω     97.00 178.00   1.00    1.20    --  107.00 125.00 -60.00   81
  7  ω     81.00 178.00   1.00    1.20    --  107.00  45.00 150.00   97
  8  ω    103.00 178.00   1.00    1.20    --  107.00  77.00  60.00   75
  9  ω     34.00 133.00   1.00    1.20    --  107.00 -45.00-120.00   99
 10  ω     35.00 136.00   1.00    1.20    --  107.00 -61.00-180.00  101
 11  ω   -116.00 -17.00   1.00    1.00    --  -41.82 -37.00 -90.00   99
 12  ω   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00   0.00  100
 13  ω   -114.00 -14.00   1.00    1.00    --  -41.82 -57.00  90.00  100
 14  ω     78.00 178.00   1.00    1.20    --  107.00  61.00 -90.00  100
 15  ω     81.00 178.00   1.00    1.20    --  107.00  45.00   0.00   97
 16  ω     34.00 105.00   1.00    1.20    --  107.00-125.00  90.00   71
 17  ω    103.00 178.00   1.00    1.20    --  107.00  77.00-150.00   75
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0281467000
_diffrn_orient_matrix_UB_12      0.0079892000
_diffrn_orient_matrix_UB_13      0.1047461000
_diffrn_orient_matrix_UB_21      0.0154403000
_diffrn_orient_matrix_UB_22      -0.1398513000
_diffrn_orient_matrix_UB_23      0.0164077000
_diffrn_orient_matrix_UB_31      0.0664460000
_diffrn_orient_matrix_UB_32      0.0359143000
_diffrn_orient_matrix_UB_33      0.0406613000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\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         0.913
_reflns_Friedel_fraction_full    0.999
_reflns_Friedel_fraction_max     0.999
_reflns_number_gt                5575
_reflns_number_total             5667
_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 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_collection       'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_data_reduction        'CrysAlisPro 1.171.40.57a (Rigaku OD, 2019)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.603
_refine_diff_density_min         -0.476
_refine_diff_density_rms         0.058
_refine_ls_abs_structure_details 
;
 Refined as an inversion twin.
;
_refine_ls_abs_structure_Flack   0.234(9)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.075
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     323
_refine_ls_number_reflns         5667
_refine_ls_number_restraints     1
_refine_ls_R_factor_all          0.0205
_refine_ls_R_factor_gt           0.0192
_refine_ls_restrained_S_all      1.075
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0260P)²+0.4746P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0464
_refine_ls_wR_factor_ref         0.0467
_refine_special_details          .
_olex2_refinement_description    
;
1. Twinned data refinement
 Scales: 0.766(9)
 0.234(9)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C119(H11W,H11X), C120(H12A,H12B), C121(H12C,
 H12D), C122(H12E,H12F), C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L),
 C126(H12M,H12N), C127(H12O,H12P), C128(H12Q,H12R), C129(H12S,H12T), C130(H13A,
 H13B)
3.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
3.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Ir1 Ir -0.65292(2) -0.62186(2) -0.47614(3) 0.01680(6) Uani 1 1 d . . . . .
P2 P -0.54555(5) -0.63246(8) -0.45139(7) 0.0200(3) Uani 1 1 d . . . . .
P3 P -0.74805(5) -0.52805(9) -0.51331(8) 0.01785(19) Uani 1 1 d . . . . .
O5 O -0.68544(18) -0.8931(3) -0.4364(3) 0.0345(8) Uani 1 1 d . . . . .
O107 O -0.52016(14) -0.4856(3) -0.4394(2) 0.0254(6) Uani 1 1 d . . . . .
O108 O -0.74196(13) -0.3821(2) -0.4707(5) 0.0231(6) Uani 1 1 d . . . . .
C4 C -0.6740(2) -0.7920(4) -0.4592(3) 0.0226(10) Uani 1 1 d . . . . .
C101 C -0.6311(2) -0.4361(3) -0.4568(3) 0.0201(9) Uani 1 1 d . . . . .
C102 C -0.5688(2) -0.3960(4) -0.4385(4) 0.0233(9) Uani 1 1 d . . . . .
C103 C -0.5535(2) -0.2717(4) -0.4176(4) 0.0291(10) Uani 1 1 d . . . . .
H103 H -0.5106 -0.2470 -0.4050 0.035 Uiso 1 1 calc R . . . .
C104 C -0.6034(2) -0.1849(4) -0.4157(4) 0.0318(11) Uani 1 1 d . . . . .
H104 H -0.5939 -0.0995 -0.4018 0.038 Uiso 1 1 calc R . . . .
C105 C -0.6660(2) -0.2192(4) -0.4332(4) 0.0272(9) Uani 1 1 d . . . . .
H105 H -0.6994 -0.1586 -0.4317 0.033 Uiso 1 1 calc R . . . .
C106 C -0.6791(2) -0.3444(4) -0.4532(3) 0.0209(10) Uani 1 1 d . . . . .
C109 C -0.5123(2) -0.7048(4) -0.3389(4) 0.0253(9) Uani 1 1 d . . . . .
C110 C -0.5488(3) -0.6487(5) -0.2523(4) 0.0365(12) Uani 1 1 d . . . . .
H11A H -0.5443 -0.5572 -0.2531 0.055 Uiso 1 1 calc GR . . . .
H11B H -0.5313 -0.6819 -0.1905 0.055 Uiso 1 1 calc GR . . . .
H11C H -0.5942 -0.6711 -0.2575 0.055 Uiso 1 1 calc GR . . . .
C111 C -0.5244(3) -0.8459(5) -0.3422(5) 0.0414(13) Uani 1 1 d . . . . .
H11D H -0.5701 -0.8615 -0.3534 0.062 Uiso 1 1 calc GR . . . .
H11E H -0.5115 -0.8836 -0.2793 0.062 Uiso 1 1 calc GR . . . .
H11F H -0.4994 -0.8833 -0.3958 0.062 Uiso 1 1 calc GR . . . .
C112 C -0.4405(2) -0.6771(4) -0.3264(4) 0.0327(10) Uani 1 1 d . . . . .
H11G H -0.4166 -0.7150 -0.3810 0.049 Uiso 1 1 calc GR . . . .
H11H H -0.4255 -0.7127 -0.2639 0.049 Uiso 1 1 calc GR . . . .
H11I H -0.4336 -0.5862 -0.3262 0.049 Uiso 1 1 calc GR . . . .
C113 C -0.7645(2) -0.4970(4) -0.6460(3) 0.0213(8) Uani 1 1 d . . . . .
C114 C -0.7072(2) -0.4231(4) -0.6874(4) 0.0284(9) Uani 1 1 d . . . . .
H11J H -0.7019 -0.3449 -0.6501 0.043 Uiso 1 1 calc GR . . . .
H11K H -0.7148 -0.4034 -0.7570 0.043 Uiso 1 1 calc GR . . . .
H11L H -0.6682 -0.4738 -0.6815 0.043 Uiso 1 1 calc GR . . . .
C115 C -0.7694(2) -0.6213(3) -0.7019(3) 0.0233(9) Uani 1 1 d . . . . .
H11M H -0.7295 -0.6685 -0.6940 0.035 Uiso 1 1 calc GR . . . .
H11N H -0.7768 -0.6045 -0.7720 0.035 Uiso 1 1 calc GR . . . .
H11O H -0.8052 -0.6705 -0.6755 0.035 Uiso 1 1 calc GR . . . .
C116 C -0.8259(2) -0.4189(4) -0.6583(3) 0.0272(9) Uani 1 1 d . . . . .
H11P H -0.8628 -0.4680 -0.6357 0.041 Uiso 1 1 calc GR . . . .
H11Q H -0.8315 -0.3972 -0.7280 0.041 Uiso 1 1 calc GR . . . .
H11R H -0.8225 -0.3419 -0.6192 0.041 Uiso 1 1 calc GR . . . .
C117 C -0.4931(2) -0.6874(5) -0.5497(4) 0.0302(10) Uani 1 1 d . . . . .
H11S H -0.4505 -0.6486 -0.5404 0.036 Uiso 1 1 calc R . . . .
H11T H -0.4878 -0.7793 -0.5425 0.036 Uiso 1 1 calc R . . . .
C118 C -0.5152(3) -0.6606(5) -0.6540(4) 0.0364(12) Uani 1 1 d . . . . .
H11U H -0.4782 -0.6722 -0.6989 0.044 Uiso 1 1 calc R . . . .
H11V H -0.5281 -0.5714 -0.6580 0.044 Uiso 1 1 calc R . . . .
C119 C -0.5704(2) -0.7408(5) -0.6917(3) 0.0339(11) Uani 1 1 d . . . . .
H11W H -0.6086 -0.7241 -0.6504 0.041 Uiso 1 1 calc R . . . .
H11X H -0.5807 -0.7146 -0.7599 0.041 Uiso 1 1 calc R . . . .
C120 C -0.5572(3) -0.8804(5) -0.6912(5) 0.0437(14) Uani 1 1 d . . . . .
H12A H -0.5535 -0.9086 -0.6219 0.052 Uiso 1 1 calc R . . . .
H12B H -0.5153 -0.8953 -0.7233 0.052 Uiso 1 1 calc R . . . .
C121 C -0.6077(3) -0.9615(5) -0.7428(4) 0.0434(13) Uani 1 1 d . . . . .
H12C H -0.6117 -0.9338 -0.8122 0.052 Uiso 1 1 calc R . . . .
H12D H -0.5930 -1.0498 -0.7431 0.052 Uiso 1 1 calc R . . . .
C122 C -0.6721(3) -0.9552(5) -0.6952(5) 0.0442(13) Uani 1 1 d . . . . .
H12E H -0.6874 -0.8673 -0.6972 0.053 Uiso 1 1 calc R . . . .
H12F H -0.6676 -0.9794 -0.6250 0.053 Uiso 1 1 calc R . . . .
C123 C -0.7229(3) -1.0398(6) -0.7432(4) 0.0389(14) Uani 1 1 d . . . . .
H12G H -0.7244 -1.0225 -0.8148 0.047 Uiso 1 1 calc R . . . .
H12H H -0.7106 -1.1288 -0.7341 0.047 Uiso 1 1 calc R . . . .
C124 C -0.7895(3) -1.0189(6) -0.6992(4) 0.0388(13) Uani 1 1 d . . . . .
H12I H -0.8013 -0.9295 -0.7073 0.047 Uiso 1 1 calc R . . . .
H12J H -0.8210 -1.0696 -0.7367 0.047 Uiso 1 1 calc R . . . .
C125 C -0.7941(3) -1.0535(4) -0.5904(4) 0.0352(11) Uani 1 1 d . . . . .
H12K H -0.7623 -1.0033 -0.5532 0.042 Uiso 1 1 calc R . . . .
H12L H -0.7826 -1.1431 -0.5826 0.042 Uiso 1 1 calc R . . . .
C126 C -0.8604(3) -1.0321(5) -0.5449(4) 0.0413(12) Uani 1 1 d . . . . .
H12M H -0.8918 -1.0844 -0.5809 0.050 Uiso 1 1 calc R . . . .
H12N H -0.8594 -1.0621 -0.4758 0.050 Uiso 1 1 calc R . . . .
C127 C -0.8838(3) -0.8972(5) -0.5454(4) 0.0355(11) Uani 1 1 d . . . . .
H12O H -0.9252 -0.8936 -0.5099 0.043 Uiso 1 1 calc R . . . .
H12P H -0.8920 -0.8721 -0.6145 0.043 Uiso 1 1 calc R . . . .
C128 C -0.8382(2) -0.8014(4) -0.4988(3) 0.0277(11) Uani 1 1 d . . . . .
H12Q H -0.8275 -0.8284 -0.4309 0.033 Uiso 1 1 calc R . . . .
H12R H -0.7979 -0.7989 -0.5372 0.033 Uiso 1 1 calc R . . . .
C129 C -0.8671(2) -0.6709(4) -0.4956(3) 0.0259(10) Uani 1 1 d . . . . .
H12S H -0.9068 -0.6747 -0.4558 0.031 Uiso 1 1 calc R . . . .
H12T H -0.8796 -0.6473 -0.5635 0.031 Uiso 1 1 calc R . . . .
C130 C -0.8245(2) -0.5657(4) -0.4537(3) 0.0234(9) Uani 1 1 d . . . . .
H13A H -0.8150 -0.5872 -0.3842 0.028 Uiso 1 1 calc R . . . .
H13B H -0.8504 -0.4878 -0.4527 0.028 Uiso 1 1 calc R . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 P2 2.2694(11) . ?
Ir1 P3 2.2798(10) . ?
Ir1 C4 1.879(4) . ?
Ir1 C101 2.048(4) . ?
P2 O107 1.660(3) . ?
P2 C109 1.845(5) . ?
P2 C117 1.822(5) . ?
P3 O108 1.664(3) . ?
P3 C113 1.863(4) . ?
P3 C130 1.833(4) . ?
O5 C4 1.147(5) . ?
O107 C102 1.393(5) . ?
O108 C106 1.393(5) . ?
C101 C102 1.392(6) . ?
C101 C106 1.400(6) . ?
C102 C103 1.391(6) . ?
C103 C104 1.393(6) . ?
C104 C105 1.380(7) . ?
C105 C106 1.388(6) . ?
C109 C110 1.523(7) . ?
C109 C111 1.525(6) . ?
C109 C112 1.537(6) . ?
C113 C114 1.539(6) . ?
C113 C115 1.529(5) . ?
C113 C116 1.537(6) . ?
C117 C118 1.515(7) . ?
C118 C119 1.523(7) . ?
C119 C120 1.513(7) . ?
C120 C121 1.532(8) . ?
C121 C122 1.492(8) . ?
C122 C123 1.537(8) . ?
C123 C124 1.529(8) . ?
C124 C125 1.525(8) . ?
C125 C126 1.531(8) . ?
C126 C127 1.518(7) . ?
C127 C128 1.534(6) . ?
C128 C129 1.516(6) . ?
C129 C130 1.541(6) . ?

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 Ir1 P3 156.21(3) . . ?
C4 Ir1 P2 99.50(13) . . ?
C4 Ir1 P3 104.25(13) . . ?
C4 Ir1 C101 165.60(18) . . ?
C101 Ir1 P2 79.01(12) . . ?
C101 Ir1 P3 78.37(12) . . ?
O107 P2 Ir1 106.44(11) . . ?
O107 P2 C109 101.08(18) . . ?
O107 P2 C117 100.55(19) . . ?
C109 P2 Ir1 121.00(15) . . ?
C117 P2 Ir1 120.06(16) . . ?
C117 P2 C109 104.2(2) . . ?
O108 P3 Ir1 105.45(12) . . ?
O108 P3 C113 100.6(2) . . ?
O108 P3 C130 96.75(19) . . ?
C113 P3 Ir1 116.90(13) . . ?
C130 P3 Ir1 124.37(14) . . ?
C130 P3 C113 107.76(19) . . ?
C102 O107 P2 114.5(3) . . ?
C106 O108 P3 113.6(2) . . ?
O5 C4 Ir1 171.3(4) . . ?
C102 C101 Ir1 121.8(3) . . ?
C102 C101 C106 116.7(4) . . ?
C106 C101 Ir1 121.3(3) . . ?
C101 C102 O107 118.0(3) . . ?
C103 C102 O107 119.1(4) . . ?
C103 C102 C101 122.8(4) . . ?
C102 C103 C104 117.7(4) . . ?
C105 C104 C103 122.0(4) . . ?
C104 C105 C106 118.3(4) . . ?
O108 C106 C101 117.9(4) . . ?
C105 C106 O108 119.7(4) . . ?
C105 C106 C101 122.4(4) . . ?
C110 C109 P2 106.6(3) . . ?
C110 C109 C111 109.0(4) . . ?
C110 C109 C112 109.1(4) . . ?
C111 C109 P2 109.0(3) . . ?
C111 C109 C112 110.7(4) . . ?
C112 C109 P2 112.3(3) . . ?
C114 C113 P3 107.5(3) . . ?
C115 C113 P3 109.7(3) . . ?
C115 C113 C114 108.3(4) . . ?
C115 C113 C116 111.0(4) . . ?
C116 C113 P3 110.8(3) . . ?
C116 C113 C114 109.4(4) . . ?
C118 C117 P2 116.2(4) . . ?
C117 C118 C119 115.9(4) . . ?
C120 C119 C118 114.4(5) . . ?
C119 C120 C121 115.3(5) . . ?
C122 C121 C120 113.4(5) . . ?
C121 C122 C123 114.4(5) . . ?
C124 C123 C122 112.2(5) . . ?
C125 C124 C123 113.6(5) . . ?
C124 C125 C126 114.3(5) . . ?
C127 C126 C125 115.5(4) . . ?
C126 C127 C128 115.3(4) . . ?
C129 C128 C127 112.0(4) . . ?
C128 C129 C130 116.6(4) . . ?
C129 C130 P3 119.9(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 1.195
_oxdiff_exptl_absorpt_empirical_full_min 0.882
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.766(9)
2 0.234(9)

####################################################################### 
# 
# 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_0388abc18s
_database_code_depnum_ccdc_archive 'CCDC 1972819'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# [Ir(PCP-14)Cl2(CO)]
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT301_0388abc18s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        16% Note
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C31 H53 Cl2 Ir O P2'
_chemical_formula_sum            'C31 H53 Cl2 Ir O P2'
_chemical_formula_weight         766.77
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ir Ir -1.4442 7.9887 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      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                   11.6548(2)
_cell_length_b                   11.78332(18)
_cell_length_c                   24.5327(4)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     3369.14(10)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    32179
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.8230
_cell_measurement_theta_min      3.4550
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    4.238
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.110
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018)
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            'pale yellow'
_exptl_crystal_density_diffrn    1.512
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       plate
_exptl_crystal_F_000             1552
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
12 8 -18 0.1779
-2 14 17 0.0177
-12 -7 19 0.1438
2 -14 -17 0.0625
6 -6 -29 0.1384
-10 4 -26 0.1479
-7 6 29 0.0644
13 -7 13 0.1377

_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 293 K'
_exptl_crystal_size_max          0.326
_exptl_crystal_size_mid          0.324
_exptl_crystal_size_min          0.08
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
11.8686 7.6297 -17.8981 0.2893 0.7878 0.5437
-1.8053 14.2767 17.2772 0.2133 0.5505 -0.8071
-12.0109 -6.6602 19.1129 -0.2751 -0.7512 -0.6000
1.7857 -14.2879 -17.2463 -0.2137 -0.5517 0.8062
6.1935 -6.1891 -29.3291 0.1844 -0.0594 0.9811
-9.7976 3.9947 -26.4773 0.9271 -0.3450 0.1463
-6.7565 6.4738 28.5007 -0.1427 0.0438 -0.9888
13.4220 -7.3387 12.8080 -0.8776 0.3313 0.3464

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0430
_diffrn_reflns_av_unetI/netI     0.0240
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -34
_diffrn_reflns_number            79384
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        29.573
_diffrn_reflns_theta_max         29.573
_diffrn_reflns_theta_min         2.967
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_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     34.00 111.00   1.00    4.00    --   24.25-178.00  60.00   77
  2  ω    -50.00  49.00   1.00    4.00    --   24.25 -37.00 150.00   99
  3  ω   -110.00 -55.00   1.00    4.00    --  -23.31 178.00 120.00   55
  4  ω     35.00 113.00   1.00    4.00    --   24.25 178.00-180.00   78
  5  ω      0.00  99.00   1.00    4.00    --   24.25  37.00  90.00   99
  6  ω      0.00  99.00   1.00    4.00    --   24.25  37.00-120.00   99
  7  ω     -4.00  97.00   1.00    4.00    --   24.25  57.00 150.00  101
  8  ω     -8.00 100.00   1.00    4.00    --   24.25  77.00 -90.00  108
  9  ω    -99.00   9.00   1.00    4.00    --  -23.31 -77.00 -60.00  108
 10  ω    -20.00  15.00   1.00    4.00    --   24.25 -99.00 -60.00   35
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  
'Rigaku Oxford Diffraction: SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0275944000
_diffrn_orient_matrix_UB_12      0.0350658000
_diffrn_orient_matrix_UB_13      -0.0195140000
_diffrn_orient_matrix_UB_21      0.0443416000
_diffrn_orient_matrix_UB_22      0.0408025000
_diffrn_orient_matrix_UB_23      0.0027793000
_diffrn_orient_matrix_UB_31      0.0312456000
_diffrn_orient_matrix_UB_32      -0.0269783000
_diffrn_orient_matrix_UB_33      -0.0211586000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.801
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     1.000
_reflns_number_gt                9078
_reflns_number_total             9431
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
_reflns_threshold_expression     'I > 2σ(I)'
_computing_cell_refinement       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         0.746
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.065
_refine_ls_abs_structure_details 
;
 Flack x determined using 3922 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   -0.0206(18)
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.058
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     395
_refine_ls_number_reflns         9431
_refine_ls_number_restraints     270
_refine_ls_R_factor_all          0.0200
_refine_ls_R_factor_gt           0.0180
_refine_ls_restrained_S_all      1.053
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0156P)²+0.8759P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0377
_refine_ls_wR_factor_ref         0.0384
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Uiso/Uaniso restraints and constraints
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim
C125 \\sim C219 \\sim C220 \\sim C221 \\sim C222 \\sim C223 \\sim C224: within
2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq,
Uanis(C121) \\sim Ueq, Uanis(C122) \\sim Ueq, Uanis(C123) \\sim Ueq,
Uanis(C124) \\sim Ueq, Uanis(C223) \\sim Ueq, Uanis(C224) \\sim Ueq,
Uanis(C220) \\sim Ueq, Uanis(C221) \\sim Ueq, Uanis(C219) \\sim Ueq,
Uanis(C222) \\sim Ueq, Uanis(C125) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
3. Others
 Sof(H11W)=Sof(H11X)=Sof(H12M)=Sof(H12N)=Sof(C219)=Sof(H21A)=Sof(H21B)=
 Sof(C220)=Sof(H22E)=Sof(H22F)=Sof(C221)=Sof(H22G)=Sof(H22H)=Sof(C222)=
 Sof(H22I)=Sof(H22J)=Sof(C223)=Sof(H22A)=Sof(H22B)=Sof(C224)=Sof(H22C)=
 Sof(H22D)=1-FVAR(1)
 Sof(H11U)=Sof(H11V)=Sof(C119)=Sof(H)=Sof(H11Y)=Sof(C120)=Sof(H12A)=Sof(H12B)=
 Sof(C121)=Sof(H12C)=Sof(H12D)=Sof(C122)=Sof(H12E)=Sof(H12F)=Sof(C123)=
 Sof(H12G)=Sof(H12H)=Sof(C124)=Sof(H12I)=Sof(H12J)=Sof(H12K)=Sof(H12L)=FVAR(1)
4.a Secondary CH2 refined with riding coordinates:
 C107(H10A,H10B), C108(H10C,H10D), C117(H11S,H11T), C118(H11U,H11V), C118(H11W,
 H11X), C119(H,H11Y), C120(H12A,H12B), C121(H12C,H12D), C122(H12E,H12F),
 C123(H12G,H12H), C124(H12I,H12J), C125(H12K,H12L), C125(H12M,H12N), C126(H12O,
 H12P), C127(H12Q,H12R), C128(H12S,H12T), C129(H12U,H12V), C130(H13A,H13B),
 C219(H21A,H21B), C220(H22E,H22F), C221(H22G,H22H), C222(H22I,H22J), C223(H22A,
 H22B), C224(H22C,H22D)
4.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
4.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Ir1 Ir 0.52362(2) 1.17143(2) 0.86277(2) 0.01830(3) Uani 1 1 d . . . . .
Cl6 Cl 0.38877(6) 1.17736(8) 0.78982(3) 0.02535(15) Uani 1 1 d . . . . .
Cl7 Cl 0.66132(7) 1.16448(8) 0.93429(3) 0.02908(17) Uani 1 1 d . . . . .
P2 P 0.39578(8) 1.10403(8) 0.93020(4) 0.02472(19) Uani 1 1 d . . . . .
P3 P 0.63215(7) 1.29866(7) 0.80696(3) 0.01997(16) Uani 1 1 d . . . . .
O5 O 0.5978(3) 0.9378(2) 0.82115(11) 0.0370(6) Uani 1 1 d . . . . .
C4 C 0.5735(3) 1.0245(3) 0.83608(13) 0.0248(7) Uani 1 1 d . . . . .
C101 C 0.4625(3) 1.3260(3) 0.89271(12) 0.0222(6) Uani 1 1 d . . . . .
C102 C 0.4092(3) 1.3327(3) 0.94376(13) 0.0277(7) Uani 1 1 d . . . . .
C103 C 0.3699(4) 1.4366(3) 0.96385(17) 0.0365(9) Uani 1 1 d . . . . .
H103 H 0.3321 1.4401 0.9981 0.044 Uiso 1 1 calc R . . . .
C104 C 0.3862(4) 1.5335(3) 0.93381(18) 0.0388(10) Uani 1 1 d . . . . .
H104 H 0.3600 1.6041 0.9477 0.047 Uiso 1 1 calc R . . . .
C105 C 0.4404(3) 1.5301(3) 0.88351(15) 0.0317(8) Uani 1 1 d . . . . .
H105 H 0.4523 1.5980 0.8634 0.038 Uiso 1 1 calc R . . . .
C106 C 0.4772(3) 1.4262(3) 0.86264(14) 0.0258(6) Uani 1 1 d . . . . .
C107 C 0.3945(4) 1.2248(3) 0.97656(14) 0.0318(8) Uani 1 1 d . . . . .
H10A H 0.3209 1.2271 0.9967 0.038 Uiso 1 1 calc R . . . .
H10B H 0.4576 1.2175 1.0033 0.038 Uiso 1 1 calc R . . . .
C108 C 0.5328(3) 1.4189(3) 0.80759(13) 0.0252(7) Uani 1 1 d . . . . .
H10C H 0.5749 1.4900 0.7998 0.030 Uiso 1 1 calc R . . . .
H10D H 0.4735 1.4085 0.7791 0.030 Uiso 1 1 calc R . . . .
C109 C 0.2426(3) 1.0723(3) 0.91452(15) 0.0299(8) Uani 1 1 d . . . . .
C110 C 0.1824(3) 1.1810(4) 0.89585(16) 0.0406(9) Uani 1 1 d . . . . .
H11A H 0.1834 1.2367 0.9255 0.061 Uiso 1 1 calc GR . . . .
H11B H 0.1028 1.1636 0.8860 0.061 Uiso 1 1 calc GR . . . .
H11C H 0.2225 1.2121 0.8641 0.061 Uiso 1 1 calc GR . . . .
C111 C 0.2363(3) 0.9823(3) 0.86971(16) 0.0370(9) Uani 1 1 d . . . . .
H11D H 0.2748 1.0105 0.8369 0.055 Uiso 1 1 calc GR . . . .
H11E H 0.1558 0.9659 0.8613 0.055 Uiso 1 1 calc GR . . . .
H11F H 0.2743 0.9128 0.8822 0.055 Uiso 1 1 calc GR . . . .
C112 C 0.1806(4) 1.0270(4) 0.96588(16) 0.0466(11) Uani 1 1 d . . . . .
H11G H 0.2142 0.9541 0.9765 0.070 Uiso 1 1 calc GR . . . .
H11H H 0.0989 1.0168 0.9579 0.070 Uiso 1 1 calc GR . . . .
H11I H 0.1895 1.0816 0.9957 0.070 Uiso 1 1 calc GR . . . .
C113 C 0.7723(3) 1.3590(3) 0.82986(14) 0.0256(7) Uani 1 1 d . . . . .
C114 C 0.7535(3) 1.4230(3) 0.88374(15) 0.0331(8) Uani 1 1 d . . . . .
H11J H 0.7042 1.4890 0.8773 0.050 Uiso 1 1 calc GR . . . .
H11K H 0.8276 1.4483 0.8981 0.050 Uiso 1 1 calc GR . . . .
H11L H 0.7167 1.3724 0.9102 0.050 Uiso 1 1 calc GR . . . .
C115 C 0.8619(3) 1.2651(3) 0.83844(17) 0.0333(8) Uani 1 1 d . . . . .
H11M H 0.8321 1.2090 0.8643 0.050 Uiso 1 1 calc GR . . . .
H11N H 0.9326 1.2984 0.8530 0.050 Uiso 1 1 calc GR . . . .
H11O H 0.8782 1.2280 0.8035 0.050 Uiso 1 1 calc GR . . . .
C116 C 0.8171(3) 1.4447(3) 0.78753(16) 0.0333(8) Uani 1 1 d . . . . .
H11P H 0.8359 1.4048 0.7536 0.050 Uiso 1 1 calc GR . . . .
H11Q H 0.8861 1.4821 0.8017 0.050 Uiso 1 1 calc GR . . . .
H11R H 0.7579 1.5018 0.7803 0.050 Uiso 1 1 calc GR . . . .
C117 C 0.4501(3) 0.9892(3) 0.97335(15) 0.0356(9) Uani 1 1 d . . . . .
H11S H 0.5265 1.0126 0.9870 0.043 Uiso 1 1 calc R . . . .
H11T H 0.3989 0.9837 1.0055 0.043 Uiso 1 1 calc R . . . .
C118 C 0.4626(4) 0.8686(3) 0.94933(18) 0.0446(10) Uani 1 1 d . U . . .
H11U H 0.4864 0.8748 0.9107 0.054 Uiso 0.787(7) 1 calc R . P A 1
H11V H 0.3869 0.8306 0.9503 0.054 Uiso 0.787(7) 1 calc R . P A 1
H11W H 0.3870 0.8333 0.9422 0.054 Uiso 0.213(7) 1 calc R . P A 2
H11X H 0.5086 0.8687 0.9154 0.054 Uiso 0.213(7) 1 calc R . P A 2
C119 C 0.5514(6) 0.7937(5) 0.9804(3) 0.0419(15) Uani 0.787(7) 1 d . U P A 1
H H 0.5355 0.7991 1.0200 0.050 Uiso 0.787(7) 1 calc R . P A 1
H11Y H 0.5400 0.7136 0.9695 0.050 Uiso 0.787(7) 1 calc R . P A 1
C120 C 0.6754(5) 0.8248(7) 0.9707(3) 0.0406(13) Uani 0.787(7) 1 d . U P A 1
H12A H 0.6811 0.9084 0.9680 0.049 Uiso 0.787(7) 1 calc R . P A 1
H12B H 0.7207 0.8010 1.0029 0.049 Uiso 0.787(7) 1 calc R . P A 1
C121 C 0.7293(6) 0.7736(5) 0.9205(3) 0.0395(13) Uani 0.787(7) 1 d . U P A 1
H12C H 0.6811 0.7915 0.8884 0.047 Uiso 0.787(7) 1 calc R . P A 1
H12D H 0.7319 0.6901 0.9245 0.047 Uiso 0.787(7) 1 calc R . P A 1
C122 C 0.8501(6) 0.8180(5) 0.9110(3) 0.0494(14) Uani 0.787(7) 1 d . U P A 1
H12E H 0.8923 0.8153 0.9459 0.059 Uiso 0.787(7) 1 calc R . P A 1
H12F H 0.8448 0.8986 0.8999 0.059 Uiso 0.787(7) 1 calc R . P A 1
C123 C 0.9201(6) 0.7545(5) 0.8681(3) 0.0531(15) Uani 0.787(7) 1 d . U P A 1
H12G H 1.0003 0.7820 0.8697 0.064 Uiso 0.787(7) 1 calc R . P A 1
H12H H 0.9209 0.6729 0.8777 0.064 Uiso 0.787(7) 1 calc R . P A 1
C124 C 0.8771(6) 0.7665(5) 0.8099(3) 0.0473(15) Uani 0.787(7) 1 d . U P A 1
H12I H 0.7955 0.7433 0.8083 0.057 Uiso 0.787(7) 1 calc R . P A 1
H12J H 0.9213 0.7150 0.7860 0.057 Uiso 0.787(7) 1 calc R . P A 1
C125 C 0.8887(5) 0.8894(4) 0.7887(2) 0.0575(13) Uani 1 1 d . U . . .
H12K H 0.8410 0.9410 0.8111 0.069 Uiso 0.787(7) 1 calc R . P A 1
H12L H 0.9695 0.9144 0.7915 0.069 Uiso 0.787(7) 1 calc R . P A 1
H12M H 0.8206 0.9194 0.8081 0.069 Uiso 0.213(7) 1 calc R . P A 2
H12N H 0.9455 0.9518 0.7902 0.069 Uiso 0.213(7) 1 calc R . P A 2
C126 C 0.8509(4) 0.8944(3) 0.7313(2) 0.0554(14) Uani 1 1 d . . . . .
H12O H 0.7744 0.8585 0.7285 0.066 Uiso 1 1 calc R . . . .
H12P H 0.9048 0.8490 0.7089 0.066 Uiso 1 1 calc R . . . .
C127 C 0.8440(4) 1.0128(4) 0.70768(19) 0.0445(10) Uani 1 1 d . . . . .
H12Q H 0.8331 1.0073 0.6678 0.053 Uiso 1 1 calc R . . . .
H12R H 0.9176 1.0524 0.7143 0.053 Uiso 1 1 calc R . . . .
C128 C 0.7468(3) 1.0829(3) 0.73186(17) 0.0328(8) Uani 1 1 d . . . . .
H12S H 0.6730 1.0446 0.7241 0.039 Uiso 1 1 calc R . . . .
H12T H 0.7563 1.0861 0.7719 0.039 Uiso 1 1 calc R . . . .
C129 C 0.7419(3) 1.2028(3) 0.70983(15) 0.0314(8) Uani 1 1 d . . . . .
H12U H 0.7341 1.1994 0.6697 0.038 Uiso 1 1 calc R . . . .
H12V H 0.8153 1.2413 0.7182 0.038 Uiso 1 1 calc R . . . .
C130 C 0.6435(3) 1.2737(3) 0.73287(13) 0.0265(7) Uani 1 1 d . . . . .
H13A H 0.5710 1.2374 0.7210 0.032 Uiso 1 1 calc R . . . .
H13B H 0.6469 1.3489 0.7150 0.032 Uiso 1 1 calc R . . . .
C219 C 0.525(3) 0.810(3) 0.9956(12) 0.049(4) Uani 0.213(7) 1 d . U P A 2
H21A H 0.5051 0.8461 1.0309 0.059 Uiso 0.213(7) 1 calc R . P A 2
H21B H 0.5045 0.7290 0.9972 0.059 Uiso 0.213(7) 1 calc R . P A 2
C220 C 0.640(3) 0.823(3) 0.9849(12) 0.048(3) Uani 0.213(7) 1 d . U P A 2
H22E H 0.6849 0.7972 1.0169 0.058 Uiso 0.213(7) 1 calc R . P A 2
H22F H 0.6571 0.9046 0.9791 0.058 Uiso 0.213(7) 1 calc R . P A 2
C221 C 0.679(2) 0.752(2) 0.9315(11) 0.046(3) Uani 0.213(7) 1 d . U P A 2
H22G H 0.6931 0.6715 0.9416 0.055 Uiso 0.213(7) 1 calc R . P A 2
H22H H 0.6180 0.7540 0.9037 0.055 Uiso 0.213(7) 1 calc R . P A 2
C222 C 0.789(2) 0.804(2) 0.9086(11) 0.045(3) Uani 0.213(7) 1 d . U P A 2
H22I H 0.7732 0.8837 0.8987 0.054 Uiso 0.213(7) 1 calc R . P A 2
H22J H 0.8479 0.8042 0.9377 0.054 Uiso 0.213(7) 1 calc R . P A 2
C223 C 0.8367(19) 0.7455(16) 0.8604(11) 0.047(3) Uani 0.213(7) 1 d . U P A 2
H22A H 0.7761 0.7419 0.8322 0.056 Uiso 0.213(7) 1 calc R . P A 2
H22B H 0.8551 0.6664 0.8710 0.056 Uiso 0.213(7) 1 calc R . P A 2
C224 C 0.943(2) 0.7971(19) 0.8349(11) 0.052(3) Uani 0.213(7) 1 d . U P A 2
H22C H 0.9901 0.7384 0.8170 0.063 Uiso 0.213(7) 1 calc R . P A 2
H22D H 0.9895 0.8370 0.8626 0.063 Uiso 0.213(7) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 Cl6 2.3828(7) . ?
Ir1 Cl7 2.3793(8) . ?
Ir1 P2 2.3637(9) . ?
Ir1 P3 2.3922(8) . ?
Ir1 C4 1.940(3) . ?
Ir1 C101 2.089(3) . ?
P2 C107 1.822(4) . ?
P2 C109 1.864(4) . ?
P2 C117 1.831(4) . ?
P3 C108 1.829(3) . ?
P3 C113 1.868(4) . ?
P3 C130 1.846(3) . ?
O5 C4 1.122(4) . ?
C101 C102 1.400(4) . ?
C101 C106 1.402(4) . ?
C102 C103 1.396(5) . ?
C102 C107 1.515(5) . ?
C103 C104 1.373(6) . ?
C104 C105 1.386(5) . ?
C105 C106 1.395(4) . ?
C106 C108 1.501(5) . ?
C109 C110 1.530(6) . ?
C109 C111 1.529(5) . ?
C109 C112 1.547(5) . ?
C113 C114 1.537(5) . ?
C113 C115 1.535(5) . ?
C113 C116 1.540(5) . ?
C117 C118 1.545(5) . ?
C118 C119 1.560(8) . ?
C118 C219 1.51(3) . ?
C119 C120 1.510(9) . ?
C120 C121 1.507(9) . ?
C121 C122 1.520(8) . ?
C122 C123 1.527(9) . ?
C123 C124 1.519(9) . ?
C124 C125 1.546(7) . ?
C125 C126 1.477(8) . ?
C125 C224 1.69(2) . ?
C126 C127 1.513(6) . ?
C127 C128 1.523(5) . ?
C128 C129 1.513(5) . ?
C129 C130 1.527(5) . ?
C219 C220 1.37(4) . ?
C220 C221 1.62(4) . ?
C221 C222 1.52(3) . ?
C222 C223 1.48(3) . ?
C223 C224 1.51(3) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl6 Ir1 P3 84.29(3) . . ?
Cl7 Ir1 Cl6 178.81(3) . . ?
Cl7 Ir1 P3 94.99(3) . . ?
P2 Ir1 Cl6 96.87(3) . . ?
P2 Ir1 Cl7 84.12(3) . . ?
P2 Ir1 P3 160.81(3) . . ?
C4 Ir1 Cl6 88.30(10) . . ?
C4 Ir1 Cl7 90.92(10) . . ?
C4 Ir1 P2 97.19(10) . . ?
C4 Ir1 P3 101.98(10) . . ?
C4 Ir1 C101 177.24(14) . . ?
C101 Ir1 Cl6 90.78(8) . . ?
C101 Ir1 Cl7 90.04(8) . . ?
C101 Ir1 P2 80.34(9) . . ?
C101 Ir1 P3 80.50(9) . . ?
C107 P2 Ir1 100.36(12) . . ?
C107 P2 C109 106.10(18) . . ?
C107 P2 C117 102.65(18) . . ?
C109 P2 Ir1 121.78(12) . . ?
C117 P2 Ir1 115.79(13) . . ?
C117 P2 C109 107.59(18) . . ?
C108 P3 Ir1 98.38(11) . . ?
C108 P3 C113 104.84(16) . . ?
C108 P3 C130 100.21(16) . . ?
C113 P3 Ir1 121.92(11) . . ?
C130 P3 Ir1 120.10(12) . . ?
C130 P3 C113 107.10(16) . . ?
O5 C4 Ir1 177.0(3) . . ?
C102 C101 Ir1 121.0(3) . . ?
C102 C101 C106 118.5(3) . . ?
C106 C101 Ir1 120.5(2) . . ?
C101 C102 C107 118.6(3) . . ?
C103 C102 C101 120.7(4) . . ?
C103 C102 C107 120.7(3) . . ?
C104 C103 C102 119.6(4) . . ?
C103 C104 C105 121.1(3) . . ?
C104 C105 C106 119.5(3) . . ?
C101 C106 C108 118.5(3) . . ?
C105 C106 C101 120.6(3) . . ?
C105 C106 C108 120.9(3) . . ?
C102 C107 P2 108.9(2) . . ?
C106 C108 P3 109.0(2) . . ?
C110 C109 P2 109.4(3) . . ?
C110 C109 C112 108.6(3) . . ?
C111 C109 P2 109.5(3) . . ?
C111 C109 C110 110.1(3) . . ?
C111 C109 C112 108.9(3) . . ?
C112 C109 P2 110.4(3) . . ?
C114 C113 P3 108.7(2) . . ?
C114 C113 C116 107.9(3) . . ?
C115 C113 P3 111.2(2) . . ?
C115 C113 C114 109.4(3) . . ?
C115 C113 C116 109.5(3) . . ?
C116 C113 P3 110.1(2) . . ?
C118 C117 P2 119.4(3) . . ?
C117 C118 C119 113.4(4) . . ?
C219 C118 C117 100.1(12) . . ?
C120 C119 C118 114.9(5) . . ?
C121 C120 C119 115.5(6) . . ?
C120 C121 C122 112.0(5) . . ?
C121 C122 C123 115.6(5) . . ?
C124 C123 C122 115.1(5) . . ?
C123 C124 C125 112.0(5) . . ?
C126 C125 C124 109.4(5) . . ?
C126 C125 C224 140.8(10) . . ?
C125 C126 C127 114.7(4) . . ?
C126 C127 C128 113.0(4) . . ?
C129 C128 C127 113.3(3) . . ?
C128 C129 C130 114.0(3) . . ?
C129 C130 P3 120.4(3) . . ?
C220 C219 C118 106(2) . . ?
C219 C220 C221 112(3) . . ?
C222 C221 C220 109(2) . . ?
C223 C222 C221 115(2) . . ?
C222 C223 C224 117(2) . . ?
C223 C224 C125 103.5(17) . . ?

_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 1.460
_oxdiff_exptl_absorpt_empirical_full_min 0.713
####################################################################### 
# 
# 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_0327abc17s
_database_code_depnum_ccdc_archive 'CCDC 1972820'
loop_
_audit_author_name
_audit_author_address
'Adrian Chaplin'
;University of Warwick
United Kingdom
;
_audit_update_record             
;
2019-12-18 deposited with the CCDC.	2020-01-27 downloaded from the CCDC.
;

#====================================================================
# [Ir(POCOP-14)Cl2(CO)]
#--------------------------------------------------------------------
# Collected and solved by Adrian Chaplin
#--------------------------------------------------------------------  
# Start Validation Reply Form 

_vrf_PLAT972_0327abc17s          
; 
PROBLEM: Check Calcd Resid. Dens.  1.44A   From Ir1            -4.95 eA-3 
PROBLEM: Check Calcd Resid. Dens.  1.00A   From C115           -2.65 eA-3 
RESPONSE: 
The solution contains large Fourier peaks and holes near the Ir atom 
that are attributed to Fourier truncation errors.  
;

_vrf_PLAT410_0327abc17s          
; 
PROBLEM: Short Intra H...H Contact  H12P     ..H22E     .       1.83 Ang.    
RESPONSE: 
The short contact occurs with a disordered component.
;

_vrf_PLAT971_0327abc17s          
; 
PROBLEM: Check Calcd Resid. Dens.  1.85A   From C128            3.11 eA-3  
PROBLEM: Check Calcd Resid. Dens.  1.78A   From P3              2.10 eA-3   
PROBLEM: Check Calcd Resid. Dens.  1.34A   From C4              1.90 eA-3  
RESPONSE: 
The solution contains large Fourier peaks and holes near the Ir atom 
that are attributed to Fourier truncation errors.  
;

_vrf_PLAT301_0327abc17s          
; 
PROBLEM: Main Residue  Disorder ..............(Resd  1  )        11% Note
RESPONSE: 
The structure contains a significant degree of disorder. 
See _publ_section_exptl_refinement.
;
#====================================================================

_audit_creation_date             2019-04-17
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3510 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2014/7
_chemical_name_common            .
_chemical_name_systematic        .
_chemical_formula_moiety         'C29 H49 Cl2 Ir O3 P2'
_chemical_formula_sum            'C29 H49 Cl2 Ir O3 P2'
_chemical_formula_weight         770.72
_chemical_absolute_configuration .
_chemical_melting_point          'not measured'
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'
Cl Cl 0.3639 0.7018 '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'
Ir Ir -4.7710 6.5667 '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                   12.4393(2)
_cell_length_b                   13.2278(2)
_cell_length_c                   39.2327(7)
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_volume                     6455.6(2)
_cell_formula_units_Z            8
_cell_measurement_reflns_used    25050
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      30.9570
_cell_measurement_theta_min      3.5210
_shelx_estimated_absorpt_T_max   .
_shelx_estimated_absorpt_T_min   .
_exptl_absorpt_coefficient_mu    10.681
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.653
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details   
;
CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015)
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            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.586
_exptl_crystal_density_meas      'not measured'
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             3104
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
0 2 -55 0.0114
-2 -18 7 0.0239
0 0 55 0.0104
7 17 -2 0.0625
-13 13 6 0.0525
1 -19 -2 0.0205
17 4 -6 0.0729

_exptl_crystal_recrystallization_method 'Crystals grown from hexane at 293 K'
_exptl_crystal_size_max          0.168
_exptl_crystal_size_mid          0.092
_exptl_crystal_size_min          0.024
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
-0.1170 1.5515 -55.0879 0.0618 -0.9947 0.0819
-2.3723 -18.3400 6.6748 -0.0165 0.1195 -0.9927
0.3197 -0.0177 55.2713 -0.0613 0.9981 0.0011
7.4463 16.8756 -1.5142 -0.2849 -0.0390 0.9578
-12.5362 12.9005 5.7970 0.8037 0.1399 0.5784
1.4747 -18.5717 -2.0227 -0.2283 -0.0471 -0.9725
16.9189 4.4624 -6.1040 -0.9131 -0.1496 0.3794

_exptl_special_details           .
_exptl_transmission_factor_max   .
_exptl_transmission_factor_min   .
_diffrn_reflns_av_R_equivalents  0.0731
_diffrn_reflns_av_unetI/netI     0.0357
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       47
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            68739
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        70.070
_diffrn_reflns_theta_max         70.070
_diffrn_reflns_theta_min         6.789
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.3046
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_details      
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -20.00  65.00   1.00   27.50    --   24.25 -99.00  60.00   85
  2  ω     -4.00  97.00   1.00   27.50    --   24.25  57.00 -90.00  101
  3  ω      0.00  99.00   1.00   27.50    --   24.25  37.00-150.00   99
  4  ω    -99.00 -14.00   1.00   27.50    --  -23.31 -77.00  90.00   85
  5  ω    -29.00  52.00   1.00   27.50    --   24.25 -57.00 -90.00   81
  6  ω    -48.00  52.00   1.00   27.50    --   24.25 -57.00 120.00  100
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at zero, AtlasS2'
_diffrn_measurement_method       'ω scans'
_diffrn_orient_matrix_type       
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0563343000
_diffrn_orient_matrix_UB_12      0.0079041000
_diffrn_orient_matrix_UB_13      -0.0007798000
_diffrn_orient_matrix_UB_21      -0.0024181000
_diffrn_orient_matrix_UB_22      0.0003756000
_diffrn_orient_matrix_UB_23      0.0180727000
_diffrn_orient_matrix_UB_31      0.0084305000
_diffrn_orient_matrix_UB_32      0.0530329000
_diffrn_orient_matrix_UB_33      -0.0000113000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                5406
_reflns_number_total             6116
_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 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_refine_diff_density_max         2.321
_refine_diff_density_min         -3.870
_refine_diff_density_rms         0.161
_refine_ls_extinction_coef       .
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.445
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         6116
_refine_ls_number_restraints     258
_refine_ls_R_factor_all          0.0748
_refine_ls_R_factor_gt           0.0677
_refine_ls_restrained_S_all      1.417
_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)+87.5375P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1260
_refine_special_details          .
_olex2_refinement_description    
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C219-C118 \\sim C119-C118 \\sim C220-C219 \\sim C120-C119 \\sim C220-C121
\\sim C121-C120 \\sim C122-
 C121 \\sim C222-C121 \\sim C123-C122 \\sim C223-C222 \\sim C223-C124 \\sim
C124-C123
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C118 \\sim C119 \\sim C120 \\sim C121 \\sim C122 \\sim C123 \\sim C124 \\sim
C219 \\sim C220 \\sim C222 \\sim C223: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
Uanis(C118) \\sim Ueq, Uanis(C121) \\sim Ueq, Uanis(C124) \\sim Ueq,
Uanis(C119) \\sim Ueq, Uanis(C120) \\sim Ueq, Uanis(C122) \\sim Ueq,
Uanis(C123) \\sim Ueq, Uanis(C220) \\sim Ueq, Uanis(C222) \\sim Ueq,
Uanis(C219) \\sim Ueq, Uanis(C223) \\sim Ueq: with sigma of 0.007 and sigma for
terminal atoms of 0.014
4. Others
 Sof(H11W)=Sof(H11X)=Sof(H12E)=Sof(H12F)=Sof(H12M)=Sof(H12N)=Sof(C219)=
 Sof(H21A)=Sof(H21B)=Sof(C220)=Sof(H22A)=Sof(H22B)=Sof(C222)=Sof(H22C)=
 Sof(H22D)=Sof(C223)=Sof(H22E)=Sof(H22F)=1-FVAR(1)
 Sof(H11U)=Sof(H11V)=Sof(C119)=Sof(H11Y)=Sof(H)=Sof(C120)=Sof(H12A)=Sof(H12B)=
 Sof(H12C)=Sof(H12D)=Sof(C122)=Sof(H12G)=Sof(H12H)=Sof(C123)=Sof(H12I)=
 Sof(H12J)=Sof(H12K)=Sof(H12L)=FVAR(1)
5.a Secondary CH2 refined with riding coordinates:
 C117(H11S,H11T), C118(H11U,H11V), C118(H11W,H11X), C119(H11Y,H), C120(H12A,
 H12B), C121(H12C,H12D), C121(H12E,H12F), C122(H12G,H12H), C123(H12I,H12J),
 C124(H12K,H12L), C124(H12M,H12N), C125(H12O,H12P), C126(H12Q,H12R), C127(H12S,
 H12T), C128(H12U,H12V), C129(H12W,H12X), C130(H13A,H13B), C219(H21A,H21B),
 C220(H22A,H22B), C222(H22C,H22D), C223(H22E,H22F)
5.b Aromatic/amide H refined with riding coordinates:
 C103(H103), C104(H104), C105(H105)
5.c Idealised Me refined as rotating group:
 C110(H11A,H11B,H11C), C111(H11D,H11E,H11F), C112(H11G,H11H,H11I), C114(H11J,
 H11K,H11L), C115(H11M,H11N,H11O), C116(H11P,H11Q,H11R)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   difmap
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
Ir1 Ir 0.54717(3) 0.72157(3) 0.39662(2) 0.01522(11) Uani 1 1 d . . . . .
Cl6 Cl 0.4445(2) 0.59874(19) 0.42672(6) 0.0327(6) Uani 1 1 d . . . . .
Cl7 Cl 0.6466(2) 0.84066(19) 0.36425(6) 0.0323(5) Uani 1 1 d . . . . .
P2 P 0.6461(2) 0.7783(2) 0.44346(6) 0.0283(5) Uani 1 1 d . . . . .
P3 P 0.40253(19) 0.7205(2) 0.35704(6) 0.0254(5) Uani 1 1 d . . . . .
O5 O 0.6993(6) 0.5489(6) 0.3767(2) 0.044(2) Uani 1 1 d . . . . .
O107 O 0.5840(6) 0.8827(5) 0.45512(19) 0.0359(18) Uani 1 1 d . . . . .
O108 O 0.3065(5) 0.7754(6) 0.37927(17) 0.0310(15) Uani 1 1 d . . . . .
C4 C 0.6420(8) 0.6138(7) 0.3830(2) 0.025(2) Uani 1 1 d . . . . .
C101 C 0.4479(8) 0.8305(8) 0.4153(2) 0.029(2) Uani 1 1 d . . . . .
C102 C 0.4807(8) 0.8962(8) 0.4415(3) 0.030(2) Uani 1 1 d . . . . .
C103 C 0.4169(10) 0.9735(8) 0.4539(3) 0.039(3) Uani 1 1 d . . . . .
H103 H 0.4429 1.0186 0.4708 0.046 Uiso 1 1 calc R . . . .
C104 C 0.3140(9) 0.9831(8) 0.4409(3) 0.037(3) Uani 1 1 d . . . . .
H104 H 0.2689 1.0357 0.4491 0.045 Uiso 1 1 calc R . . . .
C105 C 0.2750(8) 0.9174(8) 0.4161(3) 0.032(2) Uani 1 1 d . . . . .
H105 H 0.2039 0.9236 0.4075 0.039 Uiso 1 1 calc R . . . .
C106 C 0.3427(8) 0.8438(8) 0.4045(2) 0.030(2) Uani 1 1 d . . . . .
C109 C 0.6546(8) 0.7051(8) 0.4835(2) 0.029(2) Uani 1 1 d . . . . .
C110 C 0.5439(9) 0.7055(9) 0.5011(3) 0.041(3) Uani 1 1 d . . . . .
H11A H 0.5270 0.7741 0.5088 0.062 Uiso 1 1 calc GR . . . .
H11B H 0.5454 0.6597 0.5207 0.062 Uiso 1 1 calc GR . . . .
H11C H 0.4889 0.6829 0.4849 0.062 Uiso 1 1 calc GR . . . .
C111 C 0.6883(9) 0.5966(8) 0.4751(3) 0.036(3) Uani 1 1 d . . . . .
H11D H 0.6338 0.5651 0.4605 0.054 Uiso 1 1 calc GR . . . .
H11E H 0.6951 0.5578 0.4963 0.054 Uiso 1 1 calc GR . . . .
H11F H 0.7575 0.5972 0.4632 0.054 Uiso 1 1 calc GR . . . .
C112 C 0.7372(9) 0.7537(8) 0.5078(3) 0.038(3) Uani 1 1 d . . . . .
H11G H 0.8100 0.7410 0.4993 0.057 Uiso 1 1 calc GR . . . .
H11H H 0.7294 0.7243 0.5306 0.057 Uiso 1 1 calc GR . . . .
H11I H 0.7246 0.8268 0.5090 0.057 Uiso 1 1 calc GR . . . .
C113 C 0.3985(8) 0.8000(7) 0.3177(2) 0.027(2) Uani 1 1 d . . . . .
C114 C 0.4035(9) 0.9106(7) 0.3279(3) 0.033(2) Uani 1 1 d . . . . .
H11J H 0.3428 0.9265 0.3429 0.050 Uiso 1 1 calc GR . . . .
H11K H 0.3998 0.9529 0.3074 0.050 Uiso 1 1 calc GR . . . .
H11L H 0.4711 0.9238 0.3399 0.050 Uiso 1 1 calc GR . . . .
C115 C 0.4901(9) 0.7730(9) 0.2928(3) 0.042(3) Uani 1 1 d . . . . .
H11M H 0.5594 0.7802 0.3044 0.063 Uiso 1 1 calc GR . . . .
H11N H 0.4876 0.8186 0.2731 0.063 Uiso 1 1 calc GR . . . .
H11O H 0.4814 0.7030 0.2850 0.063 Uiso 1 1 calc GR . . . .
C116 C 0.2881(9) 0.7834(9) 0.3002(3) 0.040(3) Uani 1 1 d . . . . .
H11P H 0.2845 0.7146 0.2911 0.060 Uiso 1 1 calc GR . . . .
H11Q H 0.2794 0.8322 0.2817 0.060 Uiso 1 1 calc GR . . . .
H11R H 0.2305 0.7930 0.3170 0.060 Uiso 1 1 calc GR . . . .
C117 C 0.7786(8) 0.8278(8) 0.4346(3) 0.034(2) Uani 1 1 d . . . . .
H11S H 0.7716 0.8840 0.4181 0.040 Uiso 1 1 calc R . . . .
H11T H 0.8085 0.8562 0.4559 0.040 Uiso 1 1 calc R . . . .
C118 C 0.8586(8) 0.7509(8) 0.4203(3) 0.038(2) Uani 1 1 d D U . . .
H11U H 0.8208 0.7031 0.4051 0.045 Uiso 0.868(14) 1 calc R . P A 1
H11V H 0.8909 0.7118 0.4392 0.045 Uiso 0.868(14) 1 calc R . P A 1
H11W H 0.8199 0.7190 0.4011 0.045 Uiso 0.132(14) 1 calc R . P A 2
H11X H 0.8633 0.6983 0.4382 0.045 Uiso 0.132(14) 1 calc R . P A 2
C119 C 0.9470(10) 0.8059(10) 0.4005(4) 0.046(3) Uani 0.868(14) 1 d D U P A 1
H11Y H 0.9141 0.8450 0.3817 0.055 Uiso 0.868(14) 1 calc R . P A 1
H H 0.9839 0.8541 0.4158 0.055 Uiso 0.868(14) 1 calc R . P A 1
C120 C 1.0296(11) 0.7323(10) 0.3857(3) 0.052(3) Uani 0.868(14) 1 d D U P A 1
H12A H 1.0584 0.6907 0.4046 0.062 Uiso 0.868(14) 1 calc R . P A 1
H12B H 1.0902 0.7721 0.3764 0.062 Uiso 0.868(14) 1 calc R . P A 1
C121 C 0.9887(11) 0.6612(10) 0.3578(3) 0.058(3) Uani 1 1 d D U . . .
H12C H 1.0510 0.6242 0.3483 0.070 Uiso 0.868(14) 1 calc R . P A 1
H12D H 0.9406 0.6107 0.3685 0.070 Uiso 0.868(14) 1 calc R . P A 1
H12E H 0.9222 0.6269 0.3655 0.070 Uiso 0.132(14) 1 calc R . P A 2
H12F H 1.0522 0.6234 0.3661 0.070 Uiso 0.132(14) 1 calc R . P A 2
C122 C 0.9285(13) 0.7111(12) 0.3285(3) 0.060(3) Uani 0.868(14) 1 d D U P A 1
H12G H 0.9619 0.7775 0.3237 0.072 Uiso 0.868(14) 1 calc R . P A 1
H12H H 0.8534 0.7235 0.3357 0.072 Uiso 0.868(14) 1 calc R . P A 1
C123 C 0.9271(14) 0.6491(11) 0.2955(4) 0.064(3) Uani 0.868(14) 1 d D U P A 1
H12I H 0.9006 0.6930 0.2769 0.077 Uiso 0.868(14) 1 calc R . P A 1
H12J H 1.0021 0.6302 0.2899 0.077 Uiso 0.868(14) 1 calc R . P A 1
C124 C 0.8593(12) 0.5530(10) 0.2960(4) 0.068(3) Uani 1 1 d D U . . .
H12K H 0.8876 0.5065 0.2783 0.082 Uiso 0.868(14) 1 calc R . P A 1
H12L H 0.8692 0.5196 0.3183 0.082 Uiso 0.868(14) 1 calc R . P A 1
H12M H 0.8974 0.5260 0.2758 0.082 Uiso 0.132(14) 1 calc R . P A 2
H12N H 0.8752 0.5110 0.3162 0.082 Uiso 0.132(14) 1 calc R . P A 2
C125 C 0.7398(13) 0.5663(12) 0.2899(4) 0.071(5) Uani 1 1 d . . . . .
H12O H 0.7287 0.5989 0.2675 0.086 Uiso 1 1 calc R . . . .
H12P H 0.7102 0.6119 0.3076 0.086 Uiso 1 1 calc R . . . .
C126 C 0.6776(12) 0.4645(10) 0.2908(3) 0.057(4) Uani 1 1 d . . . . .
H12Q H 0.7030 0.4216 0.2717 0.069 Uiso 1 1 calc R . . . .
H12R H 0.6949 0.4290 0.3123 0.069 Uiso 1 1 calc R . . . .
C127 C 0.5551(11) 0.4762(9) 0.2881(3) 0.051(3) Uani 1 1 d . . . . .
H12S H 0.5384 0.5206 0.2685 0.062 Uiso 1 1 calc R . . . .
H12T H 0.5231 0.4091 0.2834 0.062 Uiso 1 1 calc R . . . .
C128 C 0.5028(10) 0.5198(9) 0.3197(3) 0.042(3) Uani 1 1 d . . . . .
H12U H 0.5152 0.4727 0.3389 0.051 Uiso 1 1 calc R . . . .
H12V H 0.5391 0.5843 0.3254 0.051 Uiso 1 1 calc R . . . .
C129 C 0.3849(10) 0.5393(9) 0.3169(3) 0.044(3) Uani 1 1 d . . . . .
H12W H 0.3470 0.4735 0.3155 0.052 Uiso 1 1 calc R . . . .
H12X H 0.3708 0.5762 0.2954 0.052 Uiso 1 1 calc R . . . .
C130 C 0.3372(8) 0.6001(8) 0.3466(3) 0.034(2) Uani 1 1 d . . . . .
H13A H 0.3388 0.5570 0.3673 0.040 Uiso 1 1 calc R . . . .
H13B H 0.2608 0.6141 0.3414 0.040 Uiso 1 1 calc R . . . .
C219 C 0.974(2) 0.762(8) 0.4075(17) 0.047(3) Uani 0.132(14) 1 d D U P A 2
H21A H 1.0055 0.8228 0.4185 0.056 Uiso 0.132(14) 1 calc R . P A 2
H21B H 1.0155 0.7030 0.4155 0.056 Uiso 0.132(14) 1 calc R . P A 2
C220 C 0.992(8) 0.7719(18) 0.3691(16) 0.053(3) Uani 0.132(14) 1 d D U P A 2
H22A H 1.0618 0.8035 0.3638 0.063 Uiso 0.132(14) 1 calc R . P A 2
H22B H 0.9335 0.8115 0.3582 0.063 Uiso 0.132(14) 1 calc R . P A 2
C222 C 0.991(7) 0.675(9) 0.3191(5) 0.062(4) Uani 0.132(14) 1 d D U P A 2
H22C H 1.0400 0.6236 0.3092 0.074 Uiso 0.132(14) 1 calc R . P A 2
H22D H 1.0212 0.7423 0.3138 0.074 Uiso 0.132(14) 1 calc R . P A 2
C223 C 0.881(7) 0.6653(19) 0.302(3) 0.064(4) Uani 0.132(14) 1 d D U P A 2
H22E H 0.8247 0.6947 0.3167 0.077 Uiso 0.132(14) 1 calc R . P A 2
H22F H 0.8812 0.7021 0.2799 0.077 Uiso 0.132(14) 1 calc R . P A 2


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Ir1 Cl6 2.380(2) . ?
Ir1 Cl7 2.371(2) . ?
Ir1 P2 2.336(2) . ?
Ir1 P3 2.377(2) . ?
Ir1 C4 1.926(9) . ?
Ir1 C101 2.034(10) . ?
P2 O107 1.647(7) . ?
P2 C109 1.847(10) . ?
P2 C117 1.807(10) . ?
P3 O108 1.647(7) . ?
P3 C113 1.867(10) . ?
P3 C130 1.834(10) . ?
O5 C4 1.143(11) . ?
O107 C102 1.402(12) . ?
O108 C106 1.415(12) . ?
C101 C102 1.407(13) . ?
C101 C106 1.387(14) . ?
C102 C103 1.382(14) . ?
C103 C104 1.384(15) . ?
C104 C105 1.393(15) . ?
C105 C106 1.365(14) . ?
C109 C110 1.540(14) . ?
C109 C111 1.532(14) . ?
C109 C112 1.542(14) . ?
C113 C114 1.518(13) . ?
C113 C115 1.543(14) . ?
C113 C116 1.551(14) . ?
C117 C118 1.529(15) . ?
C118 C119 1.531(9) . ?
C118 C219 1.530(10) . ?
C119 C120 1.529(9) . ?
C120 C121 1.530(9) . ?
C121 C122 1.524(9) . ?
C121 C220 1.529(10) . ?
C121 C222 1.530(10) . ?
C122 C123 1.530(9) . ?
C123 C124 1.527(9) . ?
C124 C125 1.51(2) . ?
C124 C223 1.529(10) . ?
C125 C126 1.55(2) . ?
C126 C127 1.536(19) . ?
C127 C128 1.515(16) . ?
C128 C129 1.494(17) . ?
C129 C130 1.535(16) . ?
C219 C220 1.529(10) . ?
C222 C223 1.530(10) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
Cl7 Ir1 Cl6 177.37(9) . . ?
Cl7 Ir1 P3 92.80(9) . . ?
P2 Ir1 Cl6 96.42(9) . . ?
P2 Ir1 Cl7 86.15(9) . . ?
P2 Ir1 P3 156.18(9) . . ?
P3 Ir1 Cl6 85.06(8) . . ?
C4 Ir1 Cl6 87.8(3) . . ?
C4 Ir1 Cl7 91.4(3) . . ?
C4 Ir1 P2 97.6(3) . . ?
C4 Ir1 P3 106.2(3) . . ?
C4 Ir1 C101 174.9(4) . . ?
C101 Ir1 Cl6 88.8(3) . . ?
C101 Ir1 Cl7 92.3(3) . . ?
C101 Ir1 P2 79.0(3) . . ?
C101 Ir1 P3 77.3(3) . . ?
O107 P2 Ir1 103.9(3) . . ?
O107 P2 C109 103.3(4) . . ?
O107 P2 C117 100.3(5) . . ?
C109 P2 Ir1 122.0(3) . . ?
C117 P2 Ir1 116.5(4) . . ?
C117 P2 C109 107.5(5) . . ?
O108 P3 Ir1 101.6(3) . . ?
O108 P3 C113 99.8(4) . . ?
O108 P3 C130 100.3(4) . . ?
C113 P3 Ir1 123.8(3) . . ?
C130 P3 Ir1 119.1(4) . . ?
C130 P3 C113 107.0(5) . . ?
C102 O107 P2 115.6(6) . . ?
C106 O108 P3 114.9(6) . . ?
O5 C4 Ir1 176.4(9) . . ?
C102 C101 Ir1 121.7(8) . . ?
C106 C101 Ir1 123.5(7) . . ?
C106 C101 C102 114.7(9) . . ?
O107 C102 C101 117.7(9) . . ?
C103 C102 O107 119.1(9) . . ?
C103 C102 C101 123.2(10) . . ?
C102 C103 C104 118.0(10) . . ?
C103 C104 C105 121.5(10) . . ?
C106 C105 C104 117.6(10) . . ?
C101 C106 O108 115.7(9) . . ?
C105 C106 O108 119.5(9) . . ?
C105 C106 C101 124.8(10) . . ?
C110 C109 P2 109.1(7) . . ?
C110 C109 C112 108.5(9) . . ?
C111 C109 P2 109.0(7) . . ?
C111 C109 C110 110.0(9) . . ?
C111 C109 C112 109.9(8) . . ?
C112 C109 P2 110.2(7) . . ?
C114 C113 P3 108.9(7) . . ?
C114 C113 C115 111.1(9) . . ?
C114 C113 C116 106.8(9) . . ?
C115 C113 P3 111.9(7) . . ?
C115 C113 C116 110.0(8) . . ?
C116 C113 P3 108.0(7) . . ?
C118 C117 P2 115.0(7) . . ?
C117 C118 C119 109.8(9) . . ?
C117 C118 C219 132(4) . . ?
C120 C119 C118 111.9(11) . . ?
C119 C120 C121 116.0(11) . . ?
C122 C121 C120 116.0(11) . . ?
C220 C121 C222 100(5) . . ?
C121 C122 C123 114.3(13) . . ?
C124 C123 C122 116.3(13) . . ?
C125 C124 C123 116.3(14) . . ?
C125 C124 C223 95(3) . . ?
C124 C125 C126 112.6(11) . . ?
C127 C126 C125 113.9(11) . . ?
C128 C127 C126 114.1(11) . . ?
C129 C128 C127 115.3(10) . . ?
C128 C129 C130 114.5(9) . . ?
C129 C130 P3 117.0(8) . . ?
C220 C219 C118 118(6) . . ?
C219 C220 C121 102(5) . . ?
C121 C222 C223 114(7) . . ?
C124 C223 C222 108(6) . . ?

_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 1.800
_oxdiff_exptl_absorpt_empirical_full_min 0.561
