;   () –; doi:10.1039/D3DT00612C

data_1569095
_journal_paper_doi               10.1039/D3DT00612C
_chemical_formula_moiety         'C58 H61 O4 P, C H Cl3'
_chemical_formula_sum            'C59 H62 Cl3 O4 P'
_chemical_formula_weight         972.40
_space_group_crystal_system      orthorhombic
_space_group_IT_number           61
_space_group_name_Hall           '-P 2ac 2ab'
_space_group_name_H-M_alt        'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-18
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6257)
;
_audit_update_record
;
2022-12-16 deposited with the CCDC.	2023-05-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   16.8473(19)
_cell_length_b                   16.4750(19)
_cell_length_c                   37.556(4)
_cell_measurement_reflns_used    6548
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      23.2988
_cell_measurement_theta_min      2.8054
_cell_volume                     10424(2)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Kappa APEX II'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0616
_diffrn_reflns_av_unetI/netI     0.0541
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       45
_diffrn_reflns_limit_l_min       -45
_diffrn_reflns_number            40548
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         25.680
_diffrn_reflns_theta_min         1.624
_diffrn_source                   tube
_diffrn_source_current           31.0
_diffrn_source_power             1.705
_diffrn_source_voltage           55.0
_exptl_absorpt_coefficient_mu    0.253
_exptl_absorpt_correction_T_max  0.7458
_exptl_absorpt_correction_T_min  0.6367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014) was used for absorption correction.
wR2(int) was 0.0756 before and 0.0614 after correction.
The Ratio of minimum to maximum transmission is 0.8537.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.239
_exptl_crystal_description       plate
_exptl_crystal_F_000             4112
_exptl_crystal_size_max          0.03
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.015
_refine_diff_density_max         1.106
_refine_diff_density_min         -1.391
_refine_diff_density_rms         0.113
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.076
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     628
_refine_ls_number_reflns         9873
_refine_ls_number_restraints     12
_refine_ls_restrained_S_all      1.076
_refine_ls_R_factor_all          0.1228
_refine_ls_R_factor_gt           0.0967
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1529P)^2^+36.7837P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2774
_refine_ls_wR_factor_ref         0.2991
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7373
_reflns_number_total             9873
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3dt00612c3.cif
_cod_data_source_block           fea110_1_a
_cod_database_code               1569095
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.996
_shelx_estimated_absorpt_t_min   0.992
_exptl_absorpt_special_details   SADABS
_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
C45 \\sim C45A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
C46 \\sim C46A: within 2A with sigma of 0.004 and sigma for terminal atoms of
0.008 within 2A
3. Others
 Sof(H44C)=Sof(H44D)=Sof(C45A)=Sof(H45C)=Sof(H45D)=Sof(C46A)=Sof(H46D)=
 Sof(H46E)=Sof(H46F)=1-FVAR(1)
 Sof(H44A)=Sof(H44B)=Sof(C45)=Sof(H45A)=Sof(H45B)=Sof(C46)=Sof(H46A)=Sof(H46B)=
 Sof(H46C)=FVAR(1)
4.a Ternary CH refined with riding coordinates:
 C50(H50)
4.b Secondary CH2 refined with riding coordinates:
 C13(H13A,H13B), C20(H20A,H20B), C27(H27A,H27B), C34(H34A,H34B), C35(H35A,
 H35B), C36(H36A,H36B), C38(H38A,H38B), C39(H39A,H39B), C41(H41A,H41B),
 C42(H42A,H42B), C44(H44A,H44B), C44(H44C,H44D), C45(H45A,H45B), C45A(H45C,H45D)
4.c Aromatic/amide H refined with riding coordinates:
 C2(H2), C3(H3), C4(H4), C5(H5), C8(H8), C12(H12), C15(H15), C16(H16),
 C17(H17), C22(H22), C23(H23), C24(H24), C29(H29), C30(H30), C31(H31), C48(H48),
  C49(H49), C51(H51), C52(H52), C54(H54), C55(H55), C56(H56), C57(H57),
 C58(H58), C999(H999)
4.d Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C40(H40A,H40B,H40C), C43(H43A,H43B,H43C), C46(H46A,H46B,
 H46C), C46A(H46D,H46E,H46F)
;
_shelx_res_checksum              5603
_olex2_submission_special_instructions 'No special instructions were received'