Diversity-oriented synthesis and cytotoxic activity evaluation of biaryl-containing macrocycles.
Pérez-Labrada, Karell; Cruz-Mendoza, Marco A; Chávez-Riveros, Alejandra; Hernández-Vázquez, Eduardo; Torroba, Tomás; Miranda, Luis D.; Organic & biomolecular chemistry 15 (2017) 2450–2458; doi:10.1039/c6ob02726a

data_7155514
_publ_section_title
;
 Diversity-oriented synthesis and cytotoxic activity evaluation of
 biaryl-containing macrocycles.
;
_journal_issue                   11
_journal_name_full               'Organic &amp; biomolecular chemistry'
_journal_page_first              2450
_journal_page_last               2458
_journal_paper_doi               10.1039/c6ob02726a
_journal_volume                  15
_journal_year                    2017
_chemical_formula_sum            'C63 H80 N8 O9'
_chemical_formula_weight         1093.35
_chemical_name_systematic
'N-(tert-butyl)-2-(9-(2-(cyclopentylamino)-2-oxoethyl)-3,10-dioxo-4,9-diaza-1,2(1,3)-dibenzenacyclodecaphane-4-yl)acetamide '
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_audit_update_record
;
2017-02-03 deposited with the CCDC.
2017-02-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 97.9726(15)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   7.5086(2)
_cell_length_b                   20.5310(5)
_cell_length_c                   20.0462(5)
_cell_measurement_reflns_used    9954
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      68.36
_cell_measurement_theta_min      2.23
_cell_volume                     3060.43(13)
_computing_cell_refinement       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_collection       'APEX3 v2016.1 (Bruker, 2014)'
_computing_data_reduction        'SAINT V8.37A  (Bruker, 2014)'
_computing_molecular_graphics    'XP V 5.1 (Bruker, 1998)'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-2014 (Bruker, 2014)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 52.0833
_diffrn_measured_fraction_theta_full 0.968
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type
'Bruker D8 Venture \k-geometry diffractometer 208039-01'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0342
_diffrn_reflns_av_unetI/netI     0.0433
_diffrn_reflns_Laue_measured_fraction_full 0.968
_diffrn_reflns_Laue_measured_fraction_max 0.965
_diffrn_reflns_limit_h_max       6
_diffrn_reflns_limit_h_min       -8
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            13187
_diffrn_reflns_point_group_measured_fraction_full 0.968
_diffrn_reflns_point_group_measured_fraction_max 0.965
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.396
_diffrn_reflns_theta_min         3.096
_diffrn_source                   'micro-focus X-ray source'
_exptl_absorpt_coefficient_mu    0.643
_exptl_absorpt_correction_T_max  0.7531
_exptl_absorpt_correction_T_min  0.6386
_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    1.186
_exptl_crystal_description       prism
_exptl_crystal_F_000             1172
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: MeOH'
_exptl_crystal_size_max          0.294
_exptl_crystal_size_mid          0.260
_exptl_crystal_size_min          0.142
_refine_diff_density_max         0.715
_refine_diff_density_min         -0.405
_refine_diff_density_rms         0.069
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.197
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     410
_refine_ls_number_reflns         5417
_refine_ls_number_restraints     93
_refine_ls_restrained_S_all      1.195
_refine_ls_R_factor_all          0.1764
_refine_ls_R_factor_gt           0.1513
_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^)+(0.1071P)^2^+7.7519P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3364
_refine_ls_wR_factor_ref         0.3543
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4068
_reflns_number_total             5417
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c6ob02726a2.cif
_cod_data_source_block           036MGL17
_cod_depositor_comments          'Adding full bibliography for 7155514.cif.'
_cod_database_code               7155514
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.834
_shelx_estimated_absorpt_t_max   0.914
_shelx_res_checksum              77247