Quantifying macrocyclization-induced strain utilizing <i>N</i>-phenylimides as conformational reporters.
Emenike, Bright U.; Shinn, David W.; Spinelle, Ronald A.; Yoo, Barney; Rosario, Ambar M.; Chemical communications (Cambridge, England) 60 (2024) 4040–4043; doi:10.1039/d3cc06296a

data_7132765
_publ_section_title
;
 Quantifying macrocyclization-induced strain utilizing
 <i>N</i>-phenylimides as conformational reporters.
;
_journal_issue                   30
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              4040
_journal_page_last               4043
_journal_paper_doi               10.1039/d3cc06296a
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety         'C35 H36 N2 O9'
_chemical_formula_sum            'C35 H36 N2 O9'
_chemical_formula_weight         628.66
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_audit_update_record
;
2023-12-26 deposited with the CCDC.	2024-02-22 downloaded from the CCDC.
;
_cell_angle_alpha                110.478(3)
_cell_angle_beta                 90.035(2)
_cell_angle_gamma                90.542(2)
_cell_formula_units_Z            4
_cell_length_a                   10.6256(6)
_cell_length_b                   14.6830(8)
_cell_length_c                   20.9217(10)
_cell_measurement_reflns_used    9655
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      79.5869
_cell_measurement_theta_min      3.2130
_cell_volume                     3057.7(3)
_computing_cell_refinement       'SAINT V8.37A (Bruker, 2016)'
_computing_data_collection       'Apex3 v2016.9-0 (Bruker, 2016)'
_computing_data_reduction        'SAINT V8.37A (Bruker, 2016)'
_computing_structure_refinement
;  
SHELXL-2016/6 (Sheldrick, 2015, 2016), 
SHELXLE Rev714 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      150(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker AXS D8 Quest CMOS diffractometer'
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_monochromator  'laterally graded multilayer (Goebel) mirror'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0729
_diffrn_reflns_av_unetI/netI     0.0776
_diffrn_reflns_Laue_measured_fraction_full 0.982
_diffrn_reflns_Laue_measured_fraction_max 0.925
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            36423
_diffrn_reflns_point_group_measured_fraction_full 0.982
_diffrn_reflns_point_group_measured_fraction_max 0.925
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         80.121
_diffrn_reflns_theta_min         3.213
_diffrn_source                   'I-mu-S microsource X-ray tube'
_exptl_absorpt_coefficient_mu    0.818
_exptl_absorpt_correction_T_max  0.7543
_exptl_absorpt_correction_T_min  0.6094
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
 SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D.,
 J. Appl. Cryst. 48 (2015) 3-10
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.366
_exptl_crystal_description       block
_exptl_crystal_F_000             1328
_exptl_crystal_size_max          0.170
_exptl_crystal_size_mid          0.140
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.269
_refine_diff_density_min         -0.225
_refine_diff_density_rms         0.047
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.047
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         12348
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.047
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_gt           0.0497
_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/[\s^2^(Fo^2^)+(0.0470P)^2^+0.5235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1237
_refine_ls_wR_factor_ref         0.1311
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9787
_reflns_number_total             12348
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc06296a2.cif
_cod_data_source_block           BUE_1ether_0m
_cod_depositor_comments
'Adding full bibliography for 7132765--7132767.cif.'
_cod_database_code               7132765
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_min   0.873
_shelx_estimated_absorpt_t_max   0.923
_shelx_res_checksum              45492
_shelx_hkl_checksum              19292