 
data_IR-006_a
 
_audit_creation_method            'SHELXL-2018/3'
_shelx_SHELXL_version_number      '2018/3'
_chemical_name_systematic         ?
_chemical_name_common             ?
_chemical_melting_point           ?
_chemical_formula_moiety          ?
_chemical_formula_sum
 'C44 H68 P2' 
_chemical_formula_weight          658.92

loop_
 _atom_type_symbol
 _atom_type_description
 _atom_type_scat_dispersion_real
 _atom_type_scat_dispersion_imag
 _atom_type_scat_source
 'C'  'C'   0.0181   0.0091
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'H'  'H'   0.0000   0.0000
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 'P'  'P'   0.2955   0.4335
 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
 
_space_group_crystal_system       triclinic
_space_group_IT_number            2
_space_group_name_H-M_alt         'P -1'
_space_group_name_Hall            '-P 1'
 
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
 
loop_
 _space_group_symop_operation_xyz
 'x, y, z'
 '-x, -y, -z'
 
_cell_length_a                    9.3707(2)
_cell_length_b                    9.9337(2)
_cell_length_c                    10.0310(2)
_cell_angle_alpha                 90.2806(17)
_cell_angle_beta                  93.674(2)
_cell_angle_gamma                 93.3011(19)
_cell_volume                      930.25(4)
_cell_formula_units_Z             1
_cell_measurement_temperature   100.01(10) 
_cell_measurement_reflns_used   7929
_cell_measurement_theta_min     4.4240
_cell_measurement_theta_max     75.6390
 
_exptl_crystal_description        "plate"
_exptl_crystal_colour             "colourless"
_exptl_crystal_density_meas       ?
_exptl_crystal_density_method     ?
_exptl_crystal_density_diffrn     1.176          
_exptl_crystal_F_000              362
_exptl_transmission_factor_min    ?
_exptl_transmission_factor_max    ?
_exptl_crystal_size_max                             0.104
_exptl_crystal_size_mid                             0.085
_exptl_crystal_size_min                             0.065
_exptl_absorpt_coefficient_mu                       1.267
_exptl_absorpt_correction_T_min                     0.881
_exptl_absorpt_correction_T_max                     1.000
_exptl_absorpt_correction_type    gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.40.20a (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    ?
_diffrn_ambient_temperature       100.01(10) 
_diffrn_radiation_wavelength      1.54184
_diffrn_radiation_type            CuK\a
_diffrn_source 'micro-focus sealed X-ray tube'
_diffrn_source_type 'PhotonJet (Cu) X-ray Source'
_diffrn_measurement_device_type 'XtaLAB Synergy, Dualflex, HyPix'
_diffrn_measurement_method 'ω scans'
_diffrn_detector_area_resol_mean  ?
_diffrn_reflns_number             11228
_diffrn_reflns_av_unetI/netI      0.0244
_diffrn_reflns_av_R_equivalents   0.0250
_diffrn_reflns_limit_h_min        -11
_diffrn_reflns_limit_h_max        11
_diffrn_reflns_limit_k_min        -11
_diffrn_reflns_limit_k_max        11
_diffrn_reflns_limit_l_min        -11
_diffrn_reflns_limit_l_max        11
_diffrn_reflns_theta_min          4.417
_diffrn_reflns_theta_max          67.079
_diffrn_reflns_theta_full         67.079
_diffrn_measured_fraction_theta_max   1.000
_diffrn_measured_fraction_theta_full  1.000
_diffrn_reflns_Laue_measured_fraction_max    1.000
_diffrn_reflns_Laue_measured_fraction_full   1.000
_diffrn_reflns_point_group_measured_fraction_max   1.000
_diffrn_reflns_point_group_measured_fraction_full  1.000
_reflns_number_total              3314
_reflns_number_gt                 3117
_reflns_threshold_expression      'I > 2σ(I)'
_reflns_Friedel_coverage          0.000
_reflns_Friedel_fraction_max      .
_reflns_Friedel_fraction_full     .
 
_reflns_special_details
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences.
;
 
_computing_data_collection     'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_cell_refinement     'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_data_reduction      'CrysAlisPro 1.171.40.20a (Rigaku OD, 2018)'
_computing_structure_solution   'SHELXT-2018/2 (Sheldrick, 2018)'  
_computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_molecular_graphics     ?
_computing_publication_material   ?
_refine_special_details           ?
_refine_ls_structure_factor_coef  Fsqd
_refine_ls_matrix_type            full
_refine_ls_weighting_scheme       calc
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.0359P)²+0.4679P] where P=(Fo²+2Fc²)/3'
_atom_sites_solution_primary      ?
_atom_sites_solution_secondary    ?
_atom_sites_solution_hydrogens    geom
_refine_ls_hydrogen_treatment     constr
_refine_ls_extinction_method      none
_refine_ls_extinction_coef        .
_refine_ls_number_reflns          3314
_refine_ls_number_parameters      211
_refine_ls_number_restraints      0
_refine_ls_R_factor_all           0.0343
_refine_ls_R_factor_gt            0.0327
_refine_ls_wR_factor_ref          0.0839
_refine_ls_wR_factor_gt           0.0827
_refine_ls_goodness_of_fit_ref    1.062
_refine_ls_restrained_S_all       1.062
_refine_ls_shift/su_max           0.001
_refine_ls_shift/su_mean          0.000
 
loop_
 _atom_site_label
 _atom_site_type_symbol
 _atom_site_fract_x
 _atom_site_fract_y
 _atom_site_fract_z
 _atom_site_U_iso_or_equiv
 _atom_site_adp_type
 _atom_site_occupancy
 _atom_site_site_symmetry_order  
 _atom_site_calc_flag
 _atom_site_refinement_flags_posn
 _atom_site_refinement_flags_adp
 _atom_site_refinement_flags_occupancy
 _atom_site_disorder_assembly
 _atom_site_disorder_group
P1 P 0.59703(3) 0.30839(3) 0.42105(3) 0.01444(11) Uani 1 1 d . . . . .
C1 C 0.57113(13) 0.49315(12) 0.46285(13) 0.0144(3) Uani 1 1 d . . . . .
H1 H 0.650818 0.523304 0.526000 0.017 Uiso 1 1 calc R U . . .
C2 C 0.57832(14) 0.58498(13) 0.34149(13) 0.0148(3) Uani 1 1 d . . . . .
C3 C 0.67539(14) 0.69943(13) 0.34792(13) 0.0162(3) Uani 1 1 d . . . . .
C4 C 0.68515(14) 0.78382(13) 0.23791(14) 0.0181(3) Uani 1 1 d . . . . .
H4 H 0.749295 0.858931 0.243848 0.022 Uiso 1 1 calc R U . . .
C5 C 0.60192(15) 0.75923(13) 0.11947(14) 0.0192(3) Uani 1 1 d . . . . .
C6 C 0.50416(15) 0.64863(13) 0.11535(13) 0.0180(3) Uani 1 1 d . . . . .
H6 H 0.446199 0.631634 0.037646 0.022 Uiso 1 1 calc R U . . .
C7 C 0.48951(14) 0.56196(13) 0.22332(13) 0.0157(3) Uani 1 1 d . . . . .
C8 C 0.77137(14) 0.73514(13) 0.47176(14) 0.0188(3) Uani 1 1 d . . . . .
H8A H 0.831667 0.662207 0.492663 0.028 Uiso 1 1 calc R U . . .
H8B H 0.713492 0.750548 0.545309 0.028 Uiso 1 1 calc R U . . .
H8C H 0.829778 0.815301 0.455803 0.028 Uiso 1 1 calc R U . . .
C9 C 0.61885(18) 0.84931(15) 0.00020(15) 0.0266(3) Uani 1 1 d . . . . .
H9A H 0.708453 0.834847 -0.037375 0.040 Uiso 1 1 calc R U . . .
H9B H 0.617175 0.941870 0.027711 0.040 Uiso 1 1 calc R U . . .
H9C H 0.541705 0.828523 -0.065624 0.040 Uiso 1 1 calc R U . . .
C10 C 0.36953(14) 0.45308(13) 0.20862(13) 0.0181(3) Uani 1 1 d . . . . .
H10A H 0.346315 0.434249 0.115546 0.027 Uiso 1 1 calc R U . . .
H10B H 0.286642 0.483268 0.248813 0.027 Uiso 1 1 calc R U . . .
H10C H 0.399582 0.372683 0.252189 0.027 Uiso 1 1 calc R U . . .
C11 C 0.69769(14) 0.24819(13) 0.57452(13) 0.0159(3) Uani 1 1 d . . . . .
H11 H 0.648575 0.283747 0.649351 0.019 Uiso 1 1 calc R U . . .
C12 C 0.85517(14) 0.29242(14) 0.60374(13) 0.0188(3) Uani 1 1 d . . . . .
H12A H 0.867031 0.389964 0.600208 0.023 Uiso 1 1 calc R U . . .
H12B H 0.911616 0.255349 0.536159 0.023 Uiso 1 1 calc R U . . .
C13 C 0.90887(15) 0.24433(15) 0.74191(14) 0.0225(3) Uani 1 1 d . . . . .
H13A H 1.009608 0.271643 0.757831 0.027 Uiso 1 1 calc R U . . .
H13B H 0.856772 0.286361 0.809881 0.027 Uiso 1 1 calc R U . . .
C14 C 0.88864(16) 0.09136(15) 0.75232(14) 0.0244(3) Uani 1 1 d . . . . .
H14A H 0.918510 0.063893 0.841999 0.029 Uiso 1 1 calc R U . . .
H14B H 0.948358 0.049290 0.690531 0.029 Uiso 1 1 calc R U . . .
C15 C 0.73209(17) 0.04384(14) 0.72035(14) 0.0238(3) Uani 1 1 d . . . . .
H15A H 0.674242 0.076593 0.789070 0.029 Uiso 1 1 calc R U . . .
H15B H 0.723413 -0.053934 0.720927 0.029 Uiso 1 1 calc R U . . .
C16 C 0.67542(16) 0.09400(13) 0.58418(14) 0.0214(3) Uani 1 1 d . . . . .
H16A H 0.574120 0.068094 0.570558 0.026 Uiso 1 1 calc R U . . .
H16B H 0.724730 0.051855 0.514311 0.026 Uiso 1 1 calc R U . . .
C17 C 0.72365(14) 0.31676(13) 0.28358(13) 0.0167(3) Uani 1 1 d . . . . .
H17 H 0.666618 0.347279 0.205362 0.020 Uiso 1 1 calc R U . . .
C18 C 0.86070(14) 0.41077(13) 0.29117(13) 0.0182(3) Uani 1 1 d . . . . .
H18A H 0.836700 0.501991 0.311506 0.022 Uiso 1 1 calc R U . . .
H18B H 0.926666 0.381615 0.362277 0.022 Uiso 1 1 calc R U . . .
C19 C 0.93246(15) 0.40883(14) 0.15815(14) 0.0208(3) Uani 1 1 d . . . . .
H19A H 0.868562 0.443372 0.088190 0.025 Uiso 1 1 calc R U . . .
H19B H 1.019308 0.467157 0.164920 0.025 Uiso 1 1 calc R U . . .
C20 C 0.96913(15) 0.26621(15) 0.12145(14) 0.0229(3) Uani 1 1 d . . . . .
H20A H 1.009992 0.267059 0.035006 0.027 Uiso 1 1 calc R U . . .
H20B H 1.040200 0.234997 0.186936 0.027 Uiso 1 1 calc R U . . .
C21 C 0.83654(15) 0.16975(14) 0.11651(14) 0.0217(3) Uani 1 1 d . . . . .
H21A H 0.864107 0.078877 0.099722 0.026 Uiso 1 1 calc R U . . .
H21B H 0.770666 0.194397 0.043330 0.026 Uiso 1 1 calc R U . . .
C22 C 0.76105(15) 0.17273(13) 0.24733(14) 0.0191(3) Uani 1 1 d . . . . .
H22A H 0.822803 0.137850 0.318773 0.023 Uiso 1 1 calc R U . . .
H22B H 0.673950 0.114832 0.238594 0.023 Uiso 1 1 calc R U . . .
 
 
_geom_special_details
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
 
loop_
 _geom_bond_atom_site_label_1
 _geom_bond_atom_site_label_2
 _geom_bond_distance
 _geom_bond_site_symmetry_2
 _geom_bond_publ_flag
P1 C11 1.8722(13) . ?
P1 C17 1.8750(13) . ?
P1 C1 1.9131(13) . ?
C1 C2 1.5274(17) . ?
C1 C1 1.581(2) 2_666 ?
C2 C3 1.4130(19) . ?
C2 C7 1.4139(19) . ?
C3 C4 1.3936(19) . ?
C3 C8 1.5145(19) . ?
C4 C5 1.391(2) . ?
C5 C6 1.388(2) . ?
C5 C9 1.5085(18) . ?
C6 C7 1.3956(18) . ?
C7 C10 1.5142(18) . ?
C11 C12 1.5249(19) . ?
C11 C16 1.5382(18) . ?
C12 C13 1.5321(18) . ?
C13 C14 1.525(2) . ?
C14 C15 1.528(2) . ?
C15 C16 1.5299(19) . ?
C17 C22 1.5398(18) . ?
C17 C18 1.5413(18) . ?
C18 C19 1.5327(18) . ?
C19 C20 1.526(2) . ?
C20 C21 1.523(2) . ?
C21 C22 1.5312(19) . ?
 
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
C11 P1 C17 107.50(6) . . ?
C11 P1 C1 102.95(6) . . ?
C17 P1 C1 104.18(6) . . ?
C2 C1 C1 112.23(12) . 2_666 ?
C2 C1 P1 112.99(9) . . ?
C1 C1 P1 110.70(11) 2_666 . ?
C3 C2 C7 118.32(12) . . ?
C3 C2 C1 118.96(11) . . ?
C7 C2 C1 122.71(11) . . ?
C4 C3 C2 120.02(12) . . ?
C4 C3 C8 117.77(12) . . ?
C2 C3 C8 122.22(12) . . ?
C5 C4 C3 122.06(13) . . ?
C6 C5 C4 117.49(12) . . ?
C6 C5 C9 121.61(13) . . ?
C4 C5 C9 120.89(13) . . ?
C5 C6 C7 122.52(13) . . ?
C6 C7 C2 119.52(12) . . ?
C6 C7 C10 116.52(12) . . ?
C2 C7 C10 123.81(11) . . ?
C12 C11 C16 110.47(11) . . ?
C12 C11 P1 120.33(9) . . ?
C16 C11 P1 109.70(9) . . ?
C11 C12 C13 110.66(11) . . ?
C14 C13 C12 111.01(12) . . ?
C13 C14 C15 110.92(11) . . ?
C14 C15 C16 111.79(12) . . ?
C15 C16 C11 111.21(11) . . ?
C22 C17 C18 109.60(11) . . ?
C22 C17 P1 109.07(9) . . ?
C18 C17 P1 122.21(9) . . ?
C19 C18 C17 110.36(11) . . ?
C20 C19 C18 111.07(11) . . ?
C21 C20 C19 111.09(11) . . ?
C20 C21 C22 111.56(12) . . ?
C21 C22 C17 111.47(11) . . ?
 
_refine_diff_density_max    0.350
_refine_diff_density_min   -0.267
_refine_diff_density_rms    0.040



