Synthesis of a Family of Spirocyclic Scaffolds: Building Blocks for the Exploration of Chemical Space
Sarvesh Kumar; Paul D. Thornton; Thomas O. Painter; Prashi Jain; Jared Downard; Justin T. Douglas; Conrad Santini; Journal of Organic Chemistry 78 (2013) 6529–6539; doi:10.1021/jo400738b

data_4028396
_publ_section_title
;
 Synthesis of a Family of Spirocyclic Scaffolds: Building Blocks for the
 Exploration of Chemical Space
;
_journal_name_full               'Journal of Organic Chemistry'
_journal_page_first              6529
_journal_page_last               6539
_journal_paper_doi               10.1021/jo400738b
_journal_volume                  78
_journal_year                    2013
_chemical_formula_sum            'C16 H22 Cl N O4'
_chemical_formula_weight         327.80
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXTL
_cell_angle_alpha                103.880(2)
_cell_angle_beta                 92.202(2)
_cell_angle_gamma                95.783(2)
_cell_formula_units_Z            2
_cell_length_a                   6.0662(2)
_cell_length_b                   8.1707(2)
_cell_length_c                   16.8920(5)
_cell_measurement_reflns_used    4936
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      69.70
_cell_measurement_theta_min      5.41
_cell_volume                     806.97(4)
_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  'Bruker SHELXTL'
_computing_structure_solution    'Bruker SHELXTL'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.96
_diffrn_measured_fraction_theta_max 0.925
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  'Helios multilayer optics'
_diffrn_radiation_source         'Bruker MicroStar microfocus rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0182
_diffrn_reflns_av_sigmaI/netI    0.0195
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            8871
_diffrn_reflns_theta_full        66.00
_diffrn_reflns_theta_max         69.69
_diffrn_reflns_theta_min         2.70
_exptl_absorpt_coefficient_mu    2.251
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.863
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       Thin
_exptl_crystal_F_000             348
_exptl_crystal_size_max          0.90
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.301
_refine_diff_density_min         -0.190
_refine_diff_density_rms         0.046
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     279
_refine_ls_number_reflns         2813
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0372
_refine_ls_R_factor_gt           0.0341
_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^)+(0.0547P)^2^+0.3043P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0890
_refine_ls_wR_factor_ref         0.0914
_reflns_number_gt                2592
_reflns_number_total             2813
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            jo400738b_si_003.cif
_cod_data_source_block           q59d
_cod_database_code               4028396