Investigations into an Anionic Oxy-Cope/Transannular Conjugate Addition Approach to 7,20-Diisocyanoadociane.
Roosen, Philipp C.; Vanderwal, Christopher D.; Organic letters 16 (2014) 4368–; doi:10.1021/ol502205m

data_1517387
_publ_section_title
;
 Investigations into an Anionic Oxy-Cope/Transannular Conjugate Addition
 Approach to 7,20-Diisocyanoadociane.
;
_journal_issue                   17
_journal_name_full               'Organic letters'
_journal_page_first              4368
_journal_paper_doi               10.1021/ol502205m
_journal_volume                  16
_journal_year                    2014
_chemical_formula_sum            'C13 H18 O2'
_chemical_formula_weight         206.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_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
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_cell_angle_alpha                104.2514(8)
_cell_angle_beta                 98.7965(8)
_cell_angle_gamma                110.1474(7)
_cell_formula_units_Z            2
_cell_length_a                   7.4167(5)
_cell_length_b                   8.7830(6)
_cell_length_c                   9.1296(7)
_cell_measurement_reflns_used    5050
_cell_measurement_temperature    83(2)
_cell_measurement_theta_max      28.63
_cell_measurement_theta_min      2.38
_cell_volume                     522.34(6)
_computing_cell_refinement       'Bruker SAINT'
_computing_data_collection       'Bruker APEX2'
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_computing_publication_material  'Bruker SHELXTL'
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_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
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_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.908
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
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_diffrn_reflns_av_R_equivalents  0.0111
_diffrn_reflns_av_unetI/netI     0.0120
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.908
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            6268
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.908
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.865
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_exptl_absorpt_coefficient_mu    0.086
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_exptl_absorpt_correction_T_min  0.8158
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_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       irregular
_exptl_crystal_F_000             224
_exptl_crystal_size_max          0.405
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_refine_diff_density_rms         0.052
_refine_ls_extinction_method     none
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_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
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_refine_ls_number_reflns         2486
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.084
_refine_ls_R_factor_all          0.0411
_refine_ls_R_factor_gt           0.0391
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; 
 w=1/[\s^2^(Fo^2^)+(0.0581P)^2^+0.2499P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1147
_refine_ls_wR_factor_ref         0.1168
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2311
_reflns_number_total             2486
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol502205m_si_003.cif
_cod_data_source_block           cdv25
_cod_depositor_comments
;Adding full bibliography for 1517387--1517389.cif.

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not_measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_database_code               1517387
_shelx_estimated_absorpt_t_min   0.966
_shelx_estimated_absorpt_t_max   0.974
_shelxl_version_number           2012-9
_shelx_res_checksum              47982
_shelx_hkl_checksum              47816