# Electronic Supplementary Material (ESI) for Dalton Transactions.
# This journal is © The Royal Society of Chemistry 2018

####################################################################### 
# 
# 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_bp1ccd
_database_code_depnum_ccdc_archive 'CCDC 1833915'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
chloroform[[(1,2,5,6-n)-1,5-cyclooctadiene][(2-(9-borabicyclo[3.3.1]non-9-yl)ethyl]diphenylphosphine]rhodium
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C30 H40 B Cl P Rh'
_chemical_formula_weight         580.76

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'
B B 0.0013 0.0007 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           triclinic
_symmetry_space_group_name_H-M   'P -1'

loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'

_cell_length_a                   11.0741(10)
_cell_length_b                   11.6900(10)
_cell_length_c                   13.0735(11)
_cell_angle_alpha                65.811(2)
_cell_angle_beta                 75.634(1)
_cell_angle_gamma                62.642(1)
_cell_volume                     1367.4(2)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7357
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      27.59

_exptl_crystal_description       paralellopiped
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.58
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.06
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.410
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             604
_exptl_absorpt_coefficient_mu    0.798
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.655
_exptl_absorpt_correction_T_max  0.954
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Siemens
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            9378
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0730
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_theta_min         1.71
_diffrn_reflns_theta_max         27.59
_reflns_number_total             5969
_reflns_number_gt                5318
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
; 
 Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. 
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0395P)²+4.5030P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         5969
_refine_ls_number_parameters     307
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0604
_refine_ls_R_factor_gt           0.0547
_refine_ls_wR_factor_ref         0.1632
_refine_ls_wR_factor_gt          0.1591
_refine_ls_goodness_of_fit_ref   1.098
_refine_ls_restrained_S_all      1.098
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000

loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.65637(4) 0.21783(4) 0.63787(3) 0.03372(13) Uani 1 1 d . . .
Cl1 Cl 0.44933(13) 0.38765(14) 0.68649(10) 0.0443(3) Uani 1 1 d . . .
P1 P 0.77010(12) 0.24777(13) 0.74321(10) 0.0350(3) Uani 1 1 d . . .
C1 C 0.6914(5) 0.2654(6) 0.8799(4) 0.0446(12) Uani 1 1 d . . .
H1A H 0.6858 0.1793 0.9297 0.054 Uiso 1 1 calc R . .
H1B H 0.7513 0.2801 0.9116 0.054 Uiso 1 1 calc R . .
C2 C 0.5492(6) 0.3807(6) 0.8792(4) 0.0439(11) Uani 1 1 d . . .
H2A H 0.5512 0.4629 0.8184 0.053 Uiso 1 1 calc R . .
H2B H 0.5317 0.3985 0.9489 0.053 Uiso 1 1 calc R . .
C3 C 0.8023(5) 0.4023(5) 0.6663(4) 0.0373(10) Uani 1 1 d . . .
C4 C 0.7798(5) 0.4694(5) 0.5528(4) 0.0419(11) Uani 1 1 d . . .
H4 H 0.7472 0.4358 0.5171 0.050 Uiso 1 1 calc R . .
C5 C 0.8056(6) 0.5866(6) 0.4920(5) 0.0513(13) Uani 1 1 d . . .
H5 H 0.7907 0.6304 0.4159 0.062 Uiso 1 1 calc R . .
C6 C 0.8523(6) 0.6369(6) 0.5437(6) 0.0541(14) Uani 1 1 d . . .
H6 H 0.8689 0.7153 0.5028 0.065 Uiso 1 1 calc R . .
C7 C 0.8755(7) 0.5716(6) 0.6577(6) 0.0566(14) Uani 1 1 d . . .
H7 H 0.9086 0.6055 0.6926 0.068 Uiso 1 1 calc R . .
C8 C 0.8490(6) 0.4558(6) 0.7185(5) 0.0470(12) Uani 1 1 d . . .
H8 H 0.8624 0.4133 0.7948 0.056 Uiso 1 1 calc R . .
C9 C 0.9397(5) 0.1109(5) 0.7832(4) 0.0394(10) Uani 1 1 d . . .
C10 C 1.0597(5) 0.1285(6) 0.7411(5) 0.0444(11) Uani 1 1 d . . .
H10 H 1.0566 0.2138 0.6916 0.053 Uiso 1 1 calc R . .
C11 C 1.1850(6) 0.0204(7) 0.7715(5) 0.0572(15) Uani 1 1 d . . .
H11 H 1.2651 0.0337 0.7432 0.069 Uiso 1 1 calc R . .
C12 C 1.1901(6) -0.1073(7) 0.8443(5) 0.0572(15) Uani 1 1 d . . .
H12 H 1.2739 -0.1801 0.8644 0.069 Uiso 1 1 calc R . .
C13 C 1.0721(7) -0.1263(7) 0.8867(5) 0.0613(17) Uani 1 1 d . . .
H13 H 1.0759 -0.2120 0.9355 0.074 Uiso 1 1 calc R . .
C14 C 0.9463(6) -0.0178(6) 0.8571(5) 0.0536(14) Uani 1 1 d . . .
H14 H 0.8664 -0.0313 0.8866 0.064 Uiso 1 1 calc R . .
C15 C 0.4193(6) 0.2087(5) 0.9307(4) 0.0432(11) Uani 1 1 d . . .
H15 H 0.5078 0.1394 0.9157 0.052 Uiso 1 1 calc R . .
C16 C 0.4015(7) 0.1903(6) 1.0569(5) 0.0543(14) Uani 1 1 d . . .
H16A H 0.3930 0.1040 1.1003 0.065 Uiso 1 1 calc R . .
H16B H 0.4836 0.1838 1.0771 0.065 Uiso 1 1 calc R . .
C17 C 0.2781(8) 0.3053(6) 1.0913(5) 0.0625(17) Uani 1 1 d . . .
H17A H 0.1973 0.2887 1.1001 0.075 Uiso 1 1 calc R . .
H17B H 0.2916 0.2995 1.1640 0.075 Uiso 1 1 calc R . .
C18 C 0.2514(6) 0.4512(6) 1.0092(5) 0.0518(13) Uani 1 1 d . . .
H18A H 0.3111 0.4820 1.0238 0.062 Uiso 1 1 calc R . .
H18B H 0.1583 0.5108 1.0248 0.062 Uiso 1 1 calc R . .
C19 C 0.2721(6) 0.4694(5) 0.8824(4) 0.0442(11) Uani 1 1 d . . .
H19 H 0.2702 0.5611 0.8384 0.053 Uiso 1 1 calc R . .
C20 C 0.3082(6) 0.1934(6) 0.8947(6) 0.0555(14) Uani 1 1 d . . .
H20A H 0.3039 0.1067 0.9442 0.067 Uiso 1 1 calc R . .
H20B H 0.3343 0.1894 0.8193 0.067 Uiso 1 1 calc R . .
C21 C 0.1653(6) 0.3079(7) 0.8954(7) 0.0644(17) Uani 1 1 d . . .
H21A H 0.1257 0.2925 0.9724 0.077 Uiso 1 1 calc R . .
H21B H 0.1084 0.3025 0.8533 0.077 Uiso 1 1 calc R . .
C22 C 0.1627(6) 0.4543(7) 0.8449(5) 0.0571(15) Uani 1 1 d . . .
H22A H 0.1726 0.4813 0.7636 0.069 Uiso 1 1 calc R . .
H22B H 0.0743 0.5174 0.8653 0.069 Uiso 1 1 calc R . .
C23 C 0.5625(6) 0.2442(6) 0.4915(4) 0.0469(12) Uani 1 1 d . . .
H23 H 0.5089 0.3350 0.4864 0.056 Uiso 1 1 calc R . .
C24 C 0.5379(7) 0.1443(6) 0.5838(5) 0.0531(14) Uani 1 1 d . . .
H24 H 0.4662 0.1728 0.6350 0.064 Uiso 1 1 calc R . .
C25 C 0.6168(9) -0.0082(7) 0.6100(6) 0.073(2) Uani 1 1 d . . .
H25A H 0.5894 -0.0364 0.5625 0.087 Uiso 1 1 calc R . .
H25B H 0.5934 -0.0553 0.6875 0.087 Uiso 1 1 calc R . .
C26 C 0.7707(9) -0.0518(6) 0.5926(6) 0.070(2) Uani 1 1 d . . .
H26A H 0.8146 -0.1463 0.6408 0.084 Uiso 1 1 calc R . .
H26B H 0.7999 -0.0477 0.5153 0.084 Uiso 1 1 calc R . .
C27 C 0.8173(6) 0.0360(6) 0.6177(5) 0.0533(14) Uani 1 1 d . . .
H27 H 0.8334 0.0128 0.6916 0.064 Uiso 1 1 calc R . .
C28 C 0.8378(6) 0.1508(6) 0.5362(5) 0.0526(14) Uani 1 1 d . . .
H28 H 0.8735 0.1942 0.5589 0.063 Uiso 1 1 calc R . .
C29 C 0.8059(7) 0.2095(7) 0.4140(5) 0.0648(18) Uani 1 1 d . . .
H29A H 0.8782 0.1529 0.3740 0.078 Uiso 1 1 calc R . .
H29B H 0.8053 0.3007 0.3808 0.078 Uiso 1 1 calc R . .
C30 C 0.6701(7) 0.2180(7) 0.3976(5) 0.0604(16) Uani 1 1 d . . .
H30A H 0.6369 0.2910 0.3276 0.073 Uiso 1 1 calc R . .
H30B H 0.6848 0.1327 0.3912 0.073 Uiso 1 1 calc R . .
B1 B 0.4226(6) 0.3577(6) 0.8659(4) 0.0384(11) Uani 1 1 d . . .


_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 C28 2.120(6) . ?
Rh1 C27 2.123(5) . ?
Rh1 C24 2.226(6) . ?
Rh1 C23 2.246(5) . ?
Rh1 P1 2.2949(13) . ?
Rh1 Cl1 2.3936(13) . ?
Cl1 B1 2.188(5) . ?
P1 C3 1.824(5) . ?
P1 C1 1.833(5) . ?
P1 C9 1.844(5) . ?
C1 C2 1.530(8) . ?
C2 B1 1.605(8) . ?
C3 C4 1.389(7) . ?
C3 C8 1.394(7) . ?
C4 C5 1.395(8) . ?
C5 C6 1.360(9) . ?
C6 C7 1.396(9) . ?
C7 C8 1.385(8) . ?
C9 C10 1.380(7) . ?
C9 C14 1.395(7) . ?
C10 C11 1.389(8) . ?
C11 C12 1.387(9) . ?
C12 C13 1.368(9) . ?
C13 C14 1.393(8) . ?
C15 C20 1.524(8) . ?
C15 C16 1.548(8) . ?
C15 B1 1.608(7) . ?
C16 C17 1.542(9) . ?
C17 C18 1.531(8) . ?
C18 C19 1.552(7) . ?
C19 C22 1.517(8) . ?
C19 B1 1.607(8) . ?
C20 C21 1.534(9) . ?
C21 C22 1.551(10) . ?
C23 C24 1.367(8) . ?
C23 C30 1.506(8) . ?
C24 C25 1.508(9) . ?
C25 C26 1.524(12) . ?
C26 C27 1.508(9) . ?
C27 C28 1.406(9) . ?
C28 C29 1.519(8) . ?
C29 C30 1.524(11) . ?

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
C28 Rh1 C27 38.7(2) . . ?
C28 Rh1 C24 96.9(3) . . ?
C27 Rh1 C24 81.1(3) . . ?
C28 Rh1 C23 81.5(2) . . ?
C27 Rh1 C23 88.6(2) . . ?
C24 Rh1 C23 35.6(2) . . ?
C28 Rh1 P1 90.77(18) . . ?
C27 Rh1 P1 96.09(18) . . ?
C24 Rh1 P1 163.22(15) . . ?
C23 Rh1 P1 161.17(16) . . ?
C28 Rh1 Cl1 153.93(17) . . ?
C27 Rh1 Cl1 166.65(19) . . ?
C24 Rh1 Cl1 90.45(18) . . ?
C23 Rh1 Cl1 90.47(15) . . ?
P1 Rh1 Cl1 89.07(5) . . ?
B1 Cl1 Rh1 112.55(16) . . ?
C3 P1 C1 104.1(3) . . ?
C3 P1 C9 104.2(2) . . ?
C1 P1 C9 100.6(2) . . ?
C3 P1 Rh1 110.74(16) . . ?
C1 P1 Rh1 119.14(18) . . ?
C9 P1 Rh1 116.37(18) . . ?
C2 C1 P1 116.1(4) . . ?
C1 C2 B1 117.9(4) . . ?
C4 C3 C8 118.7(5) . . ?
C4 C3 P1 119.6(4) . . ?
C8 C3 P1 121.7(4) . . ?
C3 C4 C5 120.5(5) . . ?
C6 C5 C4 120.2(5) . . ?
C5 C6 C7 120.4(5) . . ?
C8 C7 C6 119.5(6) . . ?
C7 C8 C3 120.6(5) . . ?
C10 C9 C14 118.8(5) . . ?
C10 C9 P1 123.4(4) . . ?
C14 C9 P1 117.8(4) . . ?
C9 C10 C11 120.9(5) . . ?
C12 C11 C10 119.7(6) . . ?
C13 C12 C11 120.0(6) . . ?
C12 C13 C14 120.4(6) . . ?
C13 C14 C9 120.2(6) . . ?
C20 C15 C16 112.9(5) . . ?
C20 C15 B1 113.2(4) . . ?
C16 C15 B1 104.7(4) . . ?
C17 C16 C15 115.4(5) . . ?
C18 C17 C16 115.5(5) . . ?
C17 C18 C19 115.8(5) . . ?
C22 C19 C18 112.6(5) . . ?
C22 C19 B1 112.9(5) . . ?
C18 C19 B1 105.3(4) . . ?
C15 C20 C21 115.3(5) . . ?
C20 C21 C22 114.1(5) . . ?
C19 C22 C21 114.9(5) . . ?
C24 C23 C30 124.8(6) . . ?
C24 C23 Rh1 71.4(3) . . ?
C30 C23 Rh1 110.2(4) . . ?
C23 C24 C25 125.8(6) . . ?
C23 C24 Rh1 73.0(3) . . ?
C25 C24 Rh1 107.4(4) . . ?
C24 C25 C26 113.3(6) . . ?
C27 C26 C25 113.3(6) . . ?
C28 C27 C26 124.0(6) . . ?
C28 C27 Rh1 70.6(3) . . ?
C26 C27 Rh1 113.9(5) . . ?
C27 C28 C29 124.9(6) . . ?
C27 C28 Rh1 70.8(3) . . ?
C29 C28 Rh1 109.9(4) . . ?
C28 C29 C30 114.0(5) . . ?
C23 C30 C29 113.7(5) . . ?
C2 B1 C19 117.5(5) . . ?
C2 B1 C15 118.6(5) . . ?
C19 B1 C15 107.4(4) . . ?
C2 B1 Cl1 101.1(3) . . ?
C19 B1 Cl1 104.4(3) . . ?
C15 B1 Cl1 106.0(3) . . ?

_diffrn_measured_fraction_theta_max 0.941
_diffrn_reflns_theta_full        27.59
_diffrn_measured_fraction_theta_full 0.941
_refine_diff_density_max         1.324
_refine_diff_density_min         -0.682
_refine_diff_density_rms         0.113

####################################################################### 
# 
# 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_bp5plt
_database_code_depnum_ccdc_archive 'CCDC 1833916'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;

_audit_creation_method           SHELXL-97
_chemical_name_systematic        
carbonylchlorobis[(2-(9-borabicyclo[3.3.1]non-9-yl)ethyl)diphenylphosphine]rhodium
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C49 H66 B2 Cl O2 P2 Rh'
_chemical_formula_weight         908.94

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'
B B 0.0013 0.0007 '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'
Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Rh Rh -1.1178 0.9187 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_H-M   P21/n

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

_cell_length_a                   10.851(1)
_cell_length_b                   18.685(2)
_cell_length_c                   23.362(2)
_cell_angle_alpha                90.00
_cell_angle_beta                 97.510(2)
_cell_angle_gamma                90.00
_cell_volume                     4696.1(8)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7499
_cell_measurement_theta_min      2.79
_cell_measurement_theta_max      27.50

_exptl_crystal_description       block
_exptl_crystal_colour            yellow
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.18
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             1912
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_type   multi-scans
_exptl_absorpt_correction_T_min  0.825
_exptl_absorpt_correction_T_max  0.911
_exptl_absorpt_process_details   SADABS

_exptl_special_details           
; 
 ? 
;

_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  Siemens
_diffrn_measurement_method       ?
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        none
_diffrn_reflns_number            33424
_diffrn_reflns_av_R_equivalents  0.0384
_diffrn_reflns_av_sigmaI/netI    0.0448
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_theta_min         2.07
_diffrn_reflns_theta_max         27.56
_reflns_number_total             10790
_reflns_number_gt                8081
_reflns_threshold_expression     >2sigma(I)

_computing_data_collection       ?
_computing_cell_refinement       ?
_computing_data_reduction        ?
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

_refine_special_details          
;Refinement of F² against ALL reflections.  The weighted R-factor wR and 
 goodness of fit S are based on F², conventional R-factors R are based 
 on F, with F set to zero for negative F². The threshold expression of 
 F² > 2sigma(F²) is used only for calculating R-factors(gt) etc. and is 
 not relevant to the choice of reflections for refinement.  R-factors based 
 on F² are statistically about twice as large as those based on F, and R- 
 factors based on ALL data will be even larger. The crystallographic
 asymmetric unit contains badly disordered molecules of diethyl ether, 
 which were treated as a diffuse electron density contribution
 with the aid of the SQUEEZE routine in the program PLATON.  Although
 specific positions for the independent carbon, hydrogen, and oxygen
 atoms of the disordered molecules of diethyl ether were not
 determined, the calculated density, absorption coefficient and empirical
 formula weight reflect their presence within the crystal lattice.,SQUEEZE
;

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[σ²(Fo²)+(0.0629P)²+0.0000P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    riding
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10790
_refine_ls_number_parameters     469
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0527
_refine_ls_R_factor_gt           0.0367
_refine_ls_wR_factor_ref         0.1085
_refine_ls_wR_factor_gt          0.1025
_refine_ls_goodness_of_fit_ref   1.031
_refine_ls_restrained_S_all      1.031
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
# SQUEEZE RESULTS (APPEND TO CIF)
# Note: Data are Listed for all Voids in the P1 Unit Cell
# i.e. Centre of Gravity, Solvent Accessible Volume,
# Recovered number of Electrons in the Void and
# Details about the Squeezed Material
loop_
_platon_squeeze_void_nr
_platon_squeeze_void_average_x
_platon_squeeze_void_average_y
_platon_squeeze_void_average_z
_platon_squeeze_void_volume
_platon_squeeze_void_count_electrons
_platon_squeeze_void_content
1 0.000 0.000 0.000 403 121 ' '
2 0.500 0.500 0.500 403 121 ' '
_platon_squeeze_details          
;
;
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_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Rh1 Rh 0.770419(14) 0.523836(9) 0.189290(8) 0.03540(7) Uani 1 1 d . . .
Cl1 Cl 0.93947(6) 0.47715(4) 0.25347(3) 0.05454(17) Uani 1 1 d . . .
P1 P 0.90703(5) 0.61331(3) 0.17130(3) 0.03835(14) Uani 1 1 d . . .
P2 P 0.65254(5) 0.42046(3) 0.19475(3) 0.03693(14) Uani 1 1 d . . .
O1 O 0.55620(17) 0.59408(11) 0.12203(10) 0.0671(6) Uani 1 1 d . . .
C1 C 0.6406(2) 0.56637(14) 0.14741(11) 0.0447(5) Uani 1 1 d . . .
C2 C 0.9791(2) 0.66521(14) 0.23315(11) 0.0494(6) Uani 1 1 d . . .
H2A H 1.0341 0.7003 0.2193 0.059 Uiso 1 1 calc R . .
H2B H 0.9141 0.6913 0.2491 0.059 Uiso 1 1 calc R . .
C3 C 1.0534(2) 0.62251(16) 0.28200(11) 0.0513(6) Uani 1 1 d . . .
H3A H 1.1000 0.6565 0.3077 0.062 Uiso 1 1 calc R . .
H3B H 1.1135 0.5937 0.2650 0.062 Uiso 1 1 calc R . .
C4 C 0.7482(2) 0.34129(13) 0.21240(11) 0.0445(5) Uani 1 1 d . . .
H4A H 0.7965 0.3476 0.2500 0.053 Uiso 1 1 calc R . .
H4B H 0.6949 0.2999 0.2143 0.053 Uiso 1 1 calc R . .
C5 C 0.8369(2) 0.32776(14) 0.16709(12) 0.0487(6) Uani 1 1 d . . .
H5A H 0.8748 0.3731 0.1593 0.058 Uiso 1 1 calc R . .
H5B H 0.7869 0.3129 0.1316 0.058 Uiso 1 1 calc R . .
C6 C 0.8490(2) 0.68433(13) 0.12195(10) 0.0427(5) Uani 1 1 d . . .
C7 C 0.7487(3) 0.72527(14) 0.13444(13) 0.0537(6) Uani 1 1 d . . .
H7 H 0.7114 0.7151 0.1671 0.064 Uiso 1 1 calc R . .
C8 C 0.7042(3) 0.78081(16) 0.09872(15) 0.0674(8) Uani 1 1 d . . .
H8 H 0.6381 0.8083 0.1079 0.081 Uiso 1 1 calc R . .
C9 C 0.7560(3) 0.79579(17) 0.05016(15) 0.0721(9) Uani 1 1 d . . .
H9 H 0.7248 0.8330 0.0261 0.086 Uiso 1 1 calc R . .
C10 C 0.8537(3) 0.7562(2) 0.03673(14) 0.0754(9) Uani 1 1 d . . .
H10 H 0.8896 0.7668 0.0037 0.090 Uiso 1 1 calc R . .
C11 C 0.8999(3) 0.70000(17) 0.07202(12) 0.0612(7) Uani 1 1 d . . .
H11 H 0.9655 0.6727 0.0621 0.073 Uiso 1 1 calc R . .
C12 C 1.0342(2) 0.57464(16) 0.13827(12) 0.0514(6) Uani 1 1 d . . .
C13 C 1.0125(4) 0.51441(18) 0.10532(18) 0.0804(11) Uani 1 1 d . . .
H13 H 0.9340 0.4936 0.1004 0.096 Uiso 1 1 calc R . .
C14 C 1.1096(5) 0.4838(2) 0.0788(2) 0.1129(17) Uani 1 1 d . . .
H14 H 1.0954 0.4428 0.0564 0.135 Uiso 1 1 calc R . .
C15 C 1.2234(4) 0.5146(3) 0.0861(2) 0.1128(19) Uani 1 1 d . . .
H15 H 1.2875 0.4944 0.0688 0.135 Uiso 1 1 calc R . .
C16 C 1.2448(3) 0.5742(3) 0.1183(2) 0.0984(14) Uani 1 1 d . . .
H16 H 1.3234 0.5949 0.1230 0.118 Uiso 1 1 calc R . .
C17 C 1.1514(2) 0.6046(2) 0.14427(15) 0.0730(9) Uani 1 1 d . . .
H17 H 1.1672 0.6459 0.1662 0.088 Uiso 1 1 calc R . .
C18 C 1.0600(3) 0.53296(16) 0.37356(13) 0.0606(7) Uani 1 1 d . . .
H18 H 1.1386 0.5161 0.3619 0.073 Uiso 1 1 calc R . .
C19 C 1.0876(3) 0.59307(19) 0.41929(13) 0.0730(9) Uani 1 1 d . . .
H19A H 1.1290 0.5719 0.4546 0.088 Uiso 1 1 calc R . .
H19B H 1.1451 0.6267 0.4055 0.088 Uiso 1 1 calc R . .
C20 C 0.9754(3) 0.63421(19) 0.43365(14) 0.0735(9) Uani 1 1 d . . .
H20A H 1.0039 0.6779 0.4536 0.088 Uiso 1 1 calc R . .
H20B H 0.9337 0.6058 0.4600 0.088 Uiso 1 1 calc R . .
C21 C 0.8810(3) 0.65396(17) 0.38154(14) 0.0678(8) Uani 1 1 d . . .
H21A H 0.9127 0.6945 0.3620 0.081 Uiso 1 1 calc R . .
H21B H 0.8044 0.6689 0.3953 0.081 Uiso 1 1 calc R . .
C22 C 0.8512(2) 0.59271(14) 0.33736(12) 0.0509(6) Uani 1 1 d . . .
H22 H 0.8004 0.6121 0.3031 0.061 Uiso 1 1 calc R . .
C23 C 0.7812(3) 0.53058(17) 0.36056(16) 0.0688(8) Uani 1 1 d . . .
H23A H 0.7504 0.4996 0.3286 0.083 Uiso 1 1 calc R . .
H23B H 0.7098 0.5496 0.3765 0.083 Uiso 1 1 calc R . .
C24 C 0.8583(4) 0.48540(18) 0.40708(17) 0.0821(11) Uani 1 1 d . . .
H24A H 0.8621 0.5103 0.4437 0.099 Uiso 1 1 calc R . .
H24B H 0.8154 0.4404 0.4108 0.099 Uiso 1 1 calc R . .
C25 C 0.9903(4) 0.46911(17) 0.39587(15) 0.0764(10) Uani 1 1 d . . .
H25A H 0.9875 0.4306 0.3678 0.092 Uiso 1 1 calc R . .
H25B H 1.0372 0.4521 0.4314 0.092 Uiso 1 1 calc R . .
C26 C 0.5610(2) 0.39515(13) 0.12681(10) 0.0398(5) Uani 1 1 d . . .
C27 C 0.4642(3) 0.34659(15) 0.12583(13) 0.0558(7) Uani 1 1 d . . .
H27 H 0.4440 0.3275 0.1602 0.067 Uiso 1 1 calc R . .
C28 C 0.3973(3) 0.32645(18) 0.07357(15) 0.0699(9) Uani 1 1 d . . .
H28 H 0.3325 0.2938 0.0732 0.084 Uiso 1 1 calc R . .
C29 C 0.4255(3) 0.35400(18) 0.02271(15) 0.0728(9) Uani 1 1 d . . .
H29 H 0.3797 0.3407 -0.0121 0.087 Uiso 1 1 calc R . .
C30 C 0.5225(3) 0.40169(19) 0.02349(13) 0.0697(9) Uani 1 1 d . . .
H30 H 0.5426 0.4204 -0.0110 0.084 Uiso 1 1 calc R . .
C31 C 0.5900(3) 0.42191(16) 0.07518(12) 0.0558(7) Uani 1 1 d . . .
H31 H 0.6556 0.4539 0.0752 0.067 Uiso 1 1 calc R . .
C32 C 0.5396(2) 0.42045(13) 0.24579(11) 0.0410(5) Uani 1 1 d . . .
C33 C 0.5608(3) 0.38510(17) 0.29759(13) 0.0612(7) Uani 1 1 d . . .
H33 H 0.6339 0.3592 0.3068 0.073 Uiso 1 1 calc R . .
C34 C 0.4747(3) 0.3876(2) 0.33635(15) 0.0824(11) Uani 1 1 d . . .
H34 H 0.4906 0.3638 0.3715 0.099 Uiso 1 1 calc R . .
C35 C 0.3673(3) 0.4245(2) 0.32324(16) 0.0764(10) Uani 1 1 d . . .
H35 H 0.3090 0.4252 0.3491 0.092 Uiso 1 1 calc R . .
C36 C 0.3441(3) 0.46092(18) 0.27201(17) 0.0701(9) Uani 1 1 d . . .
H36 H 0.2709 0.4869 0.2633 0.084 Uiso 1 1 calc R . .
C37 C 0.4304(3) 0.45879(15) 0.23331(14) 0.0561(7) Uani 1 1 d . . .
H37 H 0.4147 0.4834 0.1985 0.067 Uiso 1 1 calc R . .
C38 C 1.0606(3) 0.2735(2) 0.15069(16) 0.0771(10) Uani 1 1 d . . .
H38 H 1.0475 0.3036 0.1161 0.092 Uiso 1 1 calc R . .
C39 C 1.1050(4) 0.2001(3) 0.1356(2) 0.1085(15) Uani 1 1 d . . .
H39A H 1.0985 0.1963 0.0939 0.130 Uiso 1 1 calc R . .
H39B H 1.1922 0.1957 0.1508 0.130 Uiso 1 1 calc R . .
C40 C 1.0389(5) 0.1417(3) 0.1568(2) 0.1204(17) Uani 1 1 d . . .
H40A H 1.0902 0.0994 0.1553 0.144 Uiso 1 1 calc R . .
H40B H 0.9648 0.1341 0.1294 0.144 Uiso 1 1 calc R . .
C41 C 0.9996(4) 0.14402(19) 0.21435(18) 0.0863(11) Uani 1 1 d . . .
H41A H 1.0691 0.1298 0.2425 0.104 Uiso 1 1 calc R . .
H41B H 0.9337 0.1093 0.2160 0.104 Uiso 1 1 calc R . .
C42 C 0.9538(3) 0.21692(18) 0.23119(15) 0.0685(9) Uani 1 1 d . . .
H42 H 0.8732 0.2117 0.2455 0.082 Uiso 1 1 calc R . .
C43 C 1.0426(4) 0.2534(3) 0.27546(18) 0.0940(12) Uani 1 1 d . . .
H43A H 1.0051 0.2975 0.2866 0.113 Uiso 1 1 calc R . .
H43B H 1.0565 0.2231 0.3094 0.113 Uiso 1 1 calc R . .
C44 C 1.1637(4) 0.2703(3) 0.2566(2) 0.1174(17) Uani 1 1 d . . .
H44A H 1.2094 0.2260 0.2539 0.141 Uiso 1 1 calc R . .
H44B H 1.2109 0.2997 0.2859 0.141 Uiso 1 1 calc R . .
C45 C 1.1557(4) 0.3097(3) 0.1981(3) 0.1199(17) Uani 1 1 d . . .
H45A H 1.2372 0.3101 0.1853 0.144 Uiso 1 1 calc R . .
H45B H 1.1309 0.3589 0.2031 0.144 Uiso 1 1 calc R . .
B1 B 0.9811(3) 0.57098(17) 0.32040(13) 0.0479(7) Uani 1 1 d . . .
B2 B 0.9424(3) 0.27235(18) 0.18103(14) 0.0510(7) Uani 1 1 d . . .


_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 C1 1.793(3) . ?
Rh1 P1 2.3091(6) . ?
Rh1 P2 2.3293(6) . ?
Rh1 Cl1 2.3781(7) . ?
P1 C6 1.816(2) . ?
P1 C12 1.816(3) . ?
P1 C2 1.829(3) . ?
P2 C32 1.818(2) . ?
P2 C26 1.821(2) . ?
P2 C4 1.823(2) . ?
O1 C1 1.147(3) . ?
C2 C3 1.532(4) . ?
C3 B1 1.591(4) . ?
C4 C5 1.541(3) . ?
C5 B2 1.546(4) . ?
C6 C11 1.385(4) . ?
C6 C7 1.392(4) . ?
C7 C8 1.379(4) . ?
C8 C9 1.359(5) . ?
C9 C10 1.363(5) . ?
C10 C11 1.387(4) . ?
C12 C13 1.366(5) . ?
C12 C17 1.380(4) . ?
C13 C14 1.411(5) . ?
C14 C15 1.353(7) . ?
C15 C16 1.348(7) . ?
C16 C17 1.370(5) . ?
C18 C25 1.540(5) . ?
C18 C19 1.552(4) . ?
C18 B1 1.582(4) . ?
C19 C20 1.514(5) . ?
C20 C21 1.530(4) . ?
C21 C22 1.547(4) . ?
C22 C23 1.525(4) . ?
C22 B1 1.567(4) . ?
C23 C24 1.535(5) . ?
C24 C25 1.519(5) . ?
C26 C31 1.379(4) . ?
C26 C27 1.387(3) . ?
C27 C28 1.388(4) . ?
C28 C29 1.366(5) . ?
C29 C30 1.377(5) . ?
C30 C31 1.380(4) . ?
C32 C33 1.371(4) . ?
C32 C37 1.383(4) . ?
C33 C34 1.385(4) . ?
C34 C35 1.355(5) . ?
C35 C36 1.371(5) . ?
C36 C37 1.384(4) . ?
C38 C39 1.509(5) . ?
C38 B2 1.545(4) . ?
C38 C45 1.565(6) . ?
C39 C40 1.429(6) . ?
C40 C41 1.464(6) . ?
C41 C42 1.520(5) . ?
C42 C43 1.484(5) . ?
C42 B2 1.557(4) . ?
C43 C44 1.474(6) . ?
C44 C45 1.546(7) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
C1 Rh1 P1 93.28(8) . . ?
C1 Rh1 P2 89.97(8) . . ?
P1 Rh1 P2 168.67(2) . . ?
C1 Rh1 Cl1 173.32(8) . . ?
P1 Rh1 Cl1 85.40(2) . . ?
P2 Rh1 Cl1 92.59(2) . . ?
C6 P1 C12 103.92(12) . . ?
C6 P1 C2 101.02(12) . . ?
C12 P1 C2 106.07(13) . . ?
C6 P1 Rh1 117.85(8) . . ?
C12 P1 Rh1 109.30(10) . . ?
C2 P1 Rh1 117.28(9) . . ?
C32 P2 C26 103.54(11) . . ?
C32 P2 C4 105.32(11) . . ?
C26 P2 C4 102.47(12) . . ?
C32 P2 Rh1 117.26(8) . . ?
C26 P2 Rh1 114.10(8) . . ?
C4 P2 Rh1 112.62(8) . . ?
O1 C1 Rh1 178.1(2) . . ?
C3 C2 P1 116.19(19) . . ?
C2 C3 B1 119.0(2) . . ?
C5 C4 P2 111.45(17) . . ?
C4 C5 B2 118.4(2) . . ?
C11 C6 C7 117.9(3) . . ?
C11 C6 P1 123.1(2) . . ?
C7 C6 P1 118.96(19) . . ?
C8 C7 C6 120.5(3) . . ?
C9 C8 C7 120.7(3) . . ?
C8 C9 C10 119.9(3) . . ?
C9 C10 C11 120.4(3) . . ?
C6 C11 C10 120.5(3) . . ?
C13 C12 C17 118.7(3) . . ?
C13 C12 P1 118.9(2) . . ?
C17 C12 P1 122.5(3) . . ?
C12 C13 C14 119.9(4) . . ?
C15 C14 C13 119.6(4) . . ?
C16 C15 C14 120.7(4) . . ?
C15 C16 C17 120.4(4) . . ?
C16 C17 C12 120.8(4) . . ?
C25 C18 C19 112.8(3) . . ?
C25 C18 B1 112.0(3) . . ?
C19 C18 B1 104.5(2) . . ?
C20 C19 C18 115.6(3) . . ?
C19 C20 C21 114.9(3) . . ?
C20 C21 C22 114.3(3) . . ?
C23 C22 C21 113.4(2) . . ?
C23 C22 B1 113.5(2) . . ?
C21 C22 B1 104.1(2) . . ?
C22 C23 C24 114.8(3) . . ?
C25 C24 C23 115.3(3) . . ?
C24 C25 C18 114.8(3) . . ?
C31 C26 C27 118.8(2) . . ?
C31 C26 P2 120.50(19) . . ?
C27 C26 P2 120.7(2) . . ?
C26 C27 C28 120.0(3) . . ?
C29 C28 C27 120.8(3) . . ?
C28 C29 C30 119.4(3) . . ?
C29 C30 C31 120.4(3) . . ?
C26 C31 C30 120.7(3) . . ?
C33 C32 C37 118.4(2) . . ?
C33 C32 P2 121.94(19) . . ?
C37 C32 P2 119.6(2) . . ?
C32 C33 C34 120.8(3) . . ?
C35 C34 C33 120.2(3) . . ?
C34 C35 C36 120.3(3) . . ?
C35 C36 C37 119.5(3) . . ?
C32 C37 C36 120.8(3) . . ?
C39 C38 B2 113.8(3) . . ?
C39 C38 C45 110.9(3) . . ?
B2 C38 C45 101.0(3) . . ?
C40 C39 C38 115.0(3) . . ?
C39 C40 C41 121.0(4) . . ?
C40 C41 C42 114.1(3) . . ?
C43 C42 C41 112.8(3) . . ?
C43 C42 B2 101.5(3) . . ?
C41 C42 B2 113.5(3) . . ?
C44 C43 C42 114.4(4) . . ?
C43 C44 C45 114.6(4) . . ?
C44 C45 C38 112.1(3) . . ?
C22 B1 C18 109.3(2) . . ?
C22 B1 C3 120.8(2) . . ?
C18 B1 C3 117.3(2) . . ?
C38 B2 C5 122.0(3) . . ?
C38 B2 C42 111.4(3) . . ?
C5 B2 C42 126.0(2) . . ?

_diffrn_measured_fraction_theta_max 0.994
_diffrn_reflns_theta_full        27.56
_diffrn_measured_fraction_theta_full 0.994
_refine_diff_density_max         0.431
_refine_diff_density_min         -0.318
_refine_diff_density_rms         0.063

####################################################################### 
# 
# 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_bp46cms
_database_code_depnum_ccdc_archive 'CCDC 1833917'
_audit_update_record             
;
2018-03-30 deposited with the CCDC.
2018-06-04 downloaded from the CCDC.
;
_chemical_name_systematic        
Potassium[[2-(trifluoroborate)ethyl]diphenylphosphine]trihydroboron
_chemical_name_common            ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C17 H23 B2 F3 K O P'
_chemical_formula_iupac          ?
_chemical_formula_weight         392.04

_chemical_melting_point          ?

_space_group_crystal_system      monoclinic
_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                   16.5781(6)
_cell_length_b                   6.9492(3)
_cell_length_c                   17.6391(7)
_cell_angle_alpha                90
_cell_angle_beta                 96.3164(10)
_cell_angle_gamma                90
_cell_volume                     2019.77(14)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    9966
_cell_measurement_theta_min      3.1817
_cell_measurement_theta_max      32.7103
_cell_measurement_temperature    100.(2)

_exptl_crystal_description       block
_exptl_crystal_colour            colourless
_exptl_crystal_size_max          0.509
_exptl_crystal_size_mid          0.489
_exptl_crystal_size_min          0.188
_exptl_crystal_density_diffrn    1.289
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             816

_exptl_absorpt_coefficient_mu    0.370
_exptl_absorpt_correction_type   Multi-Scan
_exptl_absorpt_process_details   
;
SADABS-2016/2 - Bruker AXS area detector scaling and absorption correction
;
_exptl_absorpt_correction_T_min  0.83
_exptl_absorpt_correction_T_max  0.93

_exptl_special_details           
;
;

_diffrn_ambient_temperature      100.(2)

_diffrn_source                   ?
_diffrn_source_type              'fine-focus sealed tube'

_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_monochromator  Triumph

_diffrn_measurement_device_type  'Bruker AXS D8 Venture fixed chi'
_diffrn_measurement_method       'omega scan, PHOTON 100 CMOS'

_diffrn_detector_area_resol_mean 10.4167

_diffrn_reflns_number            41036
_diffrn_reflns_av_R_equivalents  0.0312
_diffrn_reflns_av_unetI/netI     0.0197
_diffrn_reflns_theta_min         3.15
_diffrn_reflns_theta_max         30.00
_diffrn_reflns_theta_full        30.00
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measured_fraction_theta_full 0.998
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_limit_l_max       24

_refine_special_details          
;
;

_reflns_number_total             5892
_reflns_number_gt                5176
_reflns_threshold_expression     'I > 2σ(I)'

_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_R_factor_all          0.0431
_refine_ls_R_factor_gt           0.0360
_refine_ls_wR_factor_gt          0.0862
_refine_ls_wR_factor_ref         0.0906
_refine_ls_goodness_of_fit_ref   1.073
_refine_ls_restrained_S_all      1.073
_refine_ls_number_reflns         5892
_refine_ls_number_parameters     241
_refine_ls_number_restraints     0
_refine_ls_number_constraints    ?
_refine_ls_hydrogen_treatment    mixed
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'w=1/[σ²(Fo²)+(0.0352P)²+1.4010P] where P=(Fo²+2Fc²)/3'

_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     ?
_atom_sites_solution_secondary   ?

_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.442
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?

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'
B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
F F 0.0171 0.0103 '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'
K K 0.2009 0.2494 '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'

_computing_data_collection       ?
_computing_cell_refinement       'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_data_reduction        'SAINT V8.37A (Bruker AXS Inc., 2015)'
_computing_structure_solution    ?
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_molecular_graphics    ?
_computing_publication_material  ?

loop_
_atom_site_type_symbol
_atom_site_label
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_calc_flag
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_refinement_flags_posn
_atom_site_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
K K1 0.54210(2) 0.81994(4) 0.18186(2) 0.01921(7) Uani d . . . 1 . .
P P1 0.23045(2) 0.99184(4) 0.25973(2) 0.01324(7) Uani d . . . 1 . .
F F1 0.38554(6) 0.71123(17) 0.20280(7) 0.0442(3) Uani d . . . 1 . .
F F2 0.44094(6) 0.68579(14) 0.32480(7) 0.0414(3) Uani d . . . 1 . .
F F3 0.42767(5) 0.97753(11) 0.26915(5) 0.02178(17) Uani d . . . 1 . .
O O1 0.55611(8) 0.77334(19) 0.03559(6) 0.0355(3) Uani d . . . 1 . .
C C1 0.20214(8) 0.9173(2) 0.16172(7) 0.0192(2) Uani d . . . 1 . .
C C2 0.20928(9) 0.7283(2) 0.13661(8) 0.0244(3) Uani d . . . 1 . .
H H2 0.2323 0.6324 0.1708 0.029 Uiso calc U . R 1 . .
C C3 0.18271(10) 0.6802(3) 0.06143(9) 0.0338(4) Uani d . . . 1 . .
H H3 0.188 0.5517 0.0444 0.041 Uiso calc U . R 1 . .
C C4 0.14868(10) 0.8184(4) 0.01151(9) 0.0436(5) Uani d . . . 1 . .
H H4 0.13 0.7846 -0.0396 0.052 Uiso calc U . R 1 . .
C C5 0.14188(12) 1.0055(4) 0.03594(10) 0.0474(5) Uani d . . . 1 . .
H H5 0.1185 1.1002 0.0014 0.057 Uiso calc U . R 1 . .
C C6 0.16897(10) 1.0569(3) 0.11078(9) 0.0332(4) Uani d . . . 1 . .
H H6 0.1649 1.1865 0.127 0.04 Uiso calc U . R 1 . .
C C7 0.13644(7) 0.96137(18) 0.30323(7) 0.0150(2) Uani d . . . 1 . .
C C8 0.10910(8) 1.1084(2) 0.34776(8) 0.0213(3) Uani d . . . 1 . .
H H8 0.1397 1.2236 0.3558 0.026 Uiso calc U . R 1 . .
C C9 0.03675(9) 1.0863(2) 0.38064(9) 0.0278(3) Uani d . . . 1 . .
H H9 0.0182 1.1866 0.411 0.033 Uiso calc U . R 1 . .
C C10 -0.00790(8) 0.9187(3) 0.36903(9) 0.0280(3) Uani d . . . 1 . .
H H10 -0.057 0.9041 0.3915 0.034 Uiso calc U . R 1 . .
C C11 0.01869(8) 0.7718(2) 0.32477(8) 0.0257(3) Uani d . . . 1 . .
H H11 -0.0123 0.6571 0.3167 0.031 Uiso calc U . R 1 . .
C C12 0.09099(8) 0.7926(2) 0.29206(7) 0.0200(3) Uani d . . . 1 . .
H H12 0.1094 0.6915 0.262 0.024 Uiso calc U . R 1 . .
C C13 0.30023(7) 0.81635(17) 0.30671(7) 0.0149(2) Uani d . . . 1 . .
H H13 0.2734 0.6875 0.3009 0.018 Uiso calc U . R 1 . .
C C14 0.31218(8) 0.8643(2) 0.39262(8) 0.0229(3) Uani d . . . 1 . .
H H14A 0.3421 0.7597 0.4203 0.034 Uiso calc U . R 1 . .
H H14B 0.2591 0.8791 0.4115 0.034 Uiso calc U . R 1 . .
H H14C 0.3429 0.9844 0.4006 0.034 Uiso calc U . R 1 . .
C C15 0.58675(9) 0.7716(2) -0.02379(8) 0.0232(3) Uani d . . . 1 . .
C C16 0.61850(10) 0.9530(3) -0.05585(10) 0.0338(3) Uani d . . . 1 . .
H H16A 0.5886 1.0637 -0.0388 0.051 Uiso calc U . R 1 . .
H H16B 0.6113 0.9469 -0.1117 0.051 Uiso calc U . R 1 . .
H H16C 0.6763 0.9669 -0.038 0.051 Uiso calc U . R 1 . .
C C17 0.59368(12) 0.5904(2) -0.06823(9) 0.0341(4) Uani d . . . 1 . .
H H17A 0.5773 0.4807 -0.0386 0.051 Uiso calc U . R 1 . .
H H17B 0.65 0.5732 -0.0789 0.051 Uiso calc U . R 1 . .
H H17C 0.5583 0.5985 -0.1164 0.051 Uiso calc U . R 1 . .
B B1 0.38779(9) 0.7985(2) 0.27421(9) 0.0194(3) Uani d . . . 1 . .
B B2 0.26397(10) 1.2583(2) 0.26557(10) 0.0230(3) Uani d . . . 1 . .
H H1B2 0.2880(11) 1.289(3) 0.3271(11) 0.030(5) Uiso d . . . 1 . .
H H2B2 0.3124(12) 1.274(3) 0.2274(11) 0.034(5) Uiso d . . . 1 . .
H H3B2 0.2058(13) 1.344(3) 0.2480(12) 0.045(6) Uiso d . . . 1 . .


_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_site_symmetry_2
_geom_bond_distance
_geom_bond_publ_flag
K1 F2 2_655 2.5620(10) ?
K1 F3 2_645 2.5621(8) ?
K1 O1 . 2.6358(11) ?
K1 F1 . 2.7666(10) ?
K1 F3 . 2.7949(8) ?
K1 B1 . 3.1838(15) ?
K1 B2 2_645 3.2746(16) ?
K1 F2 . 3.3120(12) ?
K1 B1 2_655 3.5795(15) ?
P1 C1 . 1.8163(13) ?
P1 C13 . 1.8170(12) ?
P1 C7 . 1.8235(12) ?
P1 B2 . 1.9328(16) ?
F1 B1 . 1.3947(18) ?
F2 B1 . 1.4189(19) ?
F2 K1 2_645 2.5620(10) ?
F3 B1 . 1.4163(16) ?
F3 K1 2_655 2.5621(8) ?
O1 C15 . 1.2133(17) ?
C1 C6 . 1.394(2) ?
C1 C2 . 1.395(2) ?
C2 C3 . 1.391(2) ?
C3 C4 . 1.381(3) ?
C4 C5 . 1.378(3) ?
C5 C6 . 1.394(2) ?
C7 C8 . 1.3944(17) ?
C7 C12 . 1.3964(18) ?
C8 C9 . 1.3970(18) ?
C9 C10 . 1.384(2) ?
C10 C11 . 1.386(2) ?
C11 C12 . 1.3937(18) ?
C13 C14 . 1.5427(18) ?
C13 B1 . 1.6232(18) ?
C15 C17 . 1.494(2) ?
C15 C16 . 1.500(2) ?
B1 K1 2_645 3.5796(15) ?
B2 K1 2_655 3.2746(16) ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle
_geom_angle_publ_flag
C1 P1 C13 . . 109.11(6) ?
C1 P1 C7 . . 102.95(6) ?
C13 P1 C7 . . 105.12(6) ?
C1 P1 B2 . . 111.52(7) ?
C13 P1 B2 . . 116.99(6) ?
C7 P1 B2 . . 110.05(6) ?
C15 O1 K1 . . 159.47(12) ?
C6 C1 C2 . . 119.47(14) ?
C6 C1 P1 . . 117.21(12) ?
C2 C1 P1 . . 123.28(10) ?
C3 C2 C1 . . 119.96(15) ?
C4 C3 C2 . . 120.36(17) ?
C5 C4 C3 . . 119.89(15) ?
C4 C5 C6 . . 120.62(17) ?
C5 C6 C1 . . 119.69(17) ?
C8 C7 C12 . . 119.40(11) ?
C8 C7 P1 . . 119.86(10) ?
C12 C7 P1 . . 120.74(9) ?
C7 C8 C9 . . 120.05(13) ?
C10 C9 C8 . . 120.04(13) ?
C9 C10 C11 . . 120.36(13) ?
C10 C11 C12 . . 119.86(13) ?
C11 C12 C7 . . 120.28(12) ?
C14 C13 B1 . . 109.89(11) ?
C14 C13 P1 . . 108.04(9) ?
B1 C13 P1 . . 116.07(9) ?
O1 C15 C17 . . 121.65(15) ?
O1 C15 C16 . . 120.98(14) ?
C17 C15 C16 . . 117.37(13) ?
F1 B1 F3 . . 106.94(12) ?
F1 B1 F2 . . 106.32(12) ?
F3 B1 F2 . . 105.23(11) ?
F1 B1 C13 . . 114.59(11) ?
F3 B1 C13 . . 113.39(10) ?
F2 B1 C13 . . 109.73(12) ?

