Diversity-Oriented Approach to Macrocyclic Cyclophane Derivatives by Suzuki-Miyaura Cross-Coupling and Olefin Metathesis as Key Steps
Sambasivarao Kotha; Arjun S. Chavan; Mobin Shaikh; Journal of Organic Chemistry 77 (2012) 482–489; doi:10.1021/jo2020714

data_4026861
_publ_section_title
;
 Diversity-Oriented Approach to Macrocyclic Cyclophane Derivatives by
 Suzuki-Miyaura Cross-Coupling and Olefin Metathesis as Key Steps
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              482
_journal_page_last               489
_journal_paper_doi               10.1021/jo2020714
_journal_volume                  77
_journal_year                    2012
_chemical_formula_sum            'C54 H44 O4'
_chemical_formula_weight         756.89
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_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 97.203(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.4276(2)
_cell_length_b                   17.4034(4)
_cell_length_c                   24.8191(7)
_cell_measurement_reflns_used    10196
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.7785
_cell_measurement_theta_min      3.3652
_cell_volume                     4039.99(17)
_computing_cell_refinement       'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_data_collection       'CrysAlis CCD, Oxford Diffraction Ltd.,'
_computing_data_reduction        'CrysAlis RED, Oxford Diffraction Ltd.,'
_computing_molecular_graphics    Ortep3
_computing_publication_material  Shelx97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      120(2)
_diffrn_detector_area_resol_mean 15.9948
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device_type  'OXFORD DIFFRACTION XCALIBUR-S'
_diffrn_measurement_method       \w/q-scan
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Enhance (Mo) x-ray Source'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0350
_diffrn_reflns_av_sigmaI/netI    0.0472
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            26251
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         3.37
_exptl_absorpt_coefficient_mu    0.077
_exptl_absorpt_correction_T_max  0.9893
_exptl_absorpt_correction_T_min  0.9825
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlis RED, Oxford Diffraction Ltd.,
Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET)
(compiled Oct 18 2006,16:28:17)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
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_exptl_crystal_description       block
_exptl_crystal_F_000             1600
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
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_refine_diff_density_max         0.168
_refine_diff_density_min         -0.138
_refine_diff_density_rms         0.031
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.875
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     523
_refine_ls_number_reflns         7065
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.875
_refine_ls_R_factor_all          0.0577
_refine_ls_R_factor_gt           0.0336
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0383P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0719
_reflns_number_gt                4749
_reflns_number_total             7065
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo2020714_srk23b.cif
_cod_data_source_block           srk028
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4026861