Synthesis of Endocyclic Cycloalkyne Amino Acids.
Rothman, Jeffrey H.; ACS omega 7 (2022) 9053–9060; doi:10.1021/acsomega.2c00270

data_4519398
_publ_section_title
;
 Synthesis of Endocyclic Cycloalkyne Amino Acids.
;
_journal_issue                   10
_journal_name_full               'ACS omega'
_journal_page_first              9053
_journal_page_last               9060
_journal_paper_doi               10.1021/acsomega.2c00270
_journal_volume                  7
_journal_year                    2022
_chemical_formula_sum            'C27 H20 Co2 N2 O12 S'
_chemical_formula_weight         714.37
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 90.851(9)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   44.87(2)
_cell_length_b                   8.909(4)
_cell_length_c                   14.807(7)
_cell_measurement_reflns_used    4194
_cell_measurement_temperature    210(2)
_cell_measurement_theta_max      23.04
_cell_measurement_theta_min      2.33
_cell_volume                     5918(5)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
_computing_data_reduction        'Bruker SAINT'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELXS-97 (Sheldrick 2008)'
_diffrn_ambient_temperature      210(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1139
_diffrn_reflns_av_unetI/netI     0.1027
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       56
_diffrn_reflns_limit_h_min       -56
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            26094
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         26.372
_diffrn_reflns_theta_min         1.816
_exptl_absorpt_coefficient_mu    1.258
_exptl_absorpt_correction_T_max  0.7437
_exptl_absorpt_correction_T_min  0.5152
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.603
_exptl_crystal_description       prism
_exptl_crystal_F_000             2896
_exptl_crystal_size_max          0.180
_exptl_crystal_size_mid          0.100
_exptl_crystal_size_min          0.100
_refine_diff_density_max         0.488
_refine_diff_density_min         -0.744
_refine_diff_density_rms         0.108
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         6062
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0824
_refine_ls_R_factor_gt           0.0567
_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^)+(0.0625P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1403
_refine_ls_wR_factor_ref         0.1608
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4304
_reflns_number_total             6062
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ao2c00270_si_003.cif
_cod_data_source_block           co_oct3
_cod_original_cell_volume        5919(5)
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               4519398
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.805
_shelx_estimated_absorpt_t_max   0.885
_shelx_res_checksum              81916
_shelx_hkl_checksum              66055