Temperature-Dependent Double Isocyanide Insertion Reaction To Construct a Polycyclic Skeleton.
Tian, Yaming; Tian, Lumin; Li, Chunju; Jia, Xueshun; Li, Jian; Organic letters 18 (2016) 840–843; doi:10.1021/acs.orglett.6b00131

data_1542635
_publ_section_title
;
 Temperature-Dependent Double Isocyanide Insertion Reaction To Construct a
 Polycyclic Skeleton.
;
_journal_issue                   4
_journal_name_full               'Organic letters'
_journal_page_first              840
_journal_page_last               843
_journal_paper_doi               10.1021/acs.orglett.6b00131
_journal_volume                  18
_journal_year                    2016
_chemical_formula_sum            'C31 H31 N3 O3'
_chemical_formula_weight         493.59
_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   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                92.640(5)
_cell_angle_beta                 97.053(5)
_cell_angle_gamma                92.437(5)
_cell_formula_units_Z            2
_cell_length_a                   10.139(4)
_cell_length_b                   11.268(5)
_cell_length_c                   11.710(5)
_cell_measurement_reflns_used    1882
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      22.87
_cell_measurement_theta_min      2.51
_cell_volume                     1324.7(10)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      296(2)
_diffrn_measured_fraction_theta_full 0.982
_diffrn_measured_fraction_theta_max 0.982
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0178
_diffrn_reflns_av_sigmaI/netI    0.0340
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       7
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            6925
_diffrn_reflns_theta_full        25.05
_diffrn_reflns_theta_max         25.05
_diffrn_reflns_theta_min         2.03
_exptl_absorpt_coefficient_mu    0.080
_exptl_absorpt_correction_T_max  0.9888
_exptl_absorpt_correction_T_min  0.9747
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             524
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.229
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.033
_refine_ls_extinction_coef       0.0087(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
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_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     341
_refine_ls_number_reflns         4603
_refine_ls_number_restraints     0
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_refine_ls_R_factor_all          0.0708
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0622P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1265
_refine_ls_wR_factor_ref         0.1402
_reflns_number_gt                3243
_reflns_number_total             4603
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ol6b00131_si_001.cif
_cod_data_source_block           d
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to
/usr/data/users/saulius/crontab/automatic-downloads/current/ACS/lib/dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 4268 2015-11-12 08:31:59Z antanas 
;
_cod_original_cell_volume        1324.8(9)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               1542635