Stereocontrolled Preparation of Diversely Trifunctionalized Cyclobutanes.
Chang, Zong; Guillot, Régis; Boddaert, Thomas; Aitken, David J.; The Journal of organic chemistry 84 (2019) 10518–10525; doi:10.1021/acs.joc.9b01463

data_4034030
_publ_section_title
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 Stereocontrolled Preparation of Diversely Trifunctionalized Cyclobutanes.
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_journal_issue                   16
_journal_name_full               'The Journal of organic chemistry'
_journal_page_first              10518
_journal_page_last               10525
_journal_paper_doi               10.1021/acs.joc.9b01463
_journal_volume                  84
_journal_year                    2019
_chemical_formula_moiety         '	3(C18 H22 N2 O8), C4 H8 O2, 0.5(C4 O2) '
_chemical_formula_sum            'C60 H74 N6 O27'
_chemical_formula_weight         1311.25
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 92.113(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.6074(6)
_cell_length_b                   15.3263(6)
_cell_length_c                   32.0745(13)
_cell_measurement_reflns_used    9878
_cell_measurement_temperature    100(1)
_cell_measurement_theta_max      70.22
_cell_measurement_theta_min      2.76
_cell_volume                     6684.6(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX3'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      100(1)
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker VENTURE PHOTON100 CMOS'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0745
_diffrn_reflns_av_unetI/netI     0.0379
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       39
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_number            116009
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        70.240
_diffrn_reflns_theta_max         70.240
_diffrn_reflns_theta_min         2.757
_exptl_absorpt_coefficient_mu    0.879
_exptl_absorpt_correction_T_max  0.9712
_exptl_absorpt_correction_T_min  0.9359
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Apex3 Bruker'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.303
_exptl_crystal_description       needle
_exptl_crystal_F_000             2768
_exptl_crystal_size_max          0.230
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.730
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     849
_refine_ls_number_reflns         12688
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.0771
_refine_ls_R_factor_gt           0.0547
_refine_ls_shift/su_max          0.014
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0659P)^2^+5.7162P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1359
_refine_ls_wR_factor_ref         0.1495
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9463
_reflns_number_total             12688
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo9b01463_si_003.cif
_cod_data_source_block           XRay2
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4034030
_shelx_estimated_absorpt_t_min   0.829
_shelx_estimated_absorpt_t_max   0.979
_shelx_res_checksum              84507
_shelx_hkl_checksum              96015