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_1517389
_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            'C18 H26 O2'
_chemical_formula_weight         274.39
_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'
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 105.1645(12)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   5.9268(6)
_cell_length_b                   33.959(4)
_cell_length_c                   7.8335(8)
_cell_measurement_reflns_used    8399
_cell_measurement_temperature    143(2)
_cell_measurement_theta_max      27.93
_cell_measurement_theta_min      2.40
_cell_volume                     1521.7(3)
_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-2012 (Sheldrick, 2012)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      143(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.947
_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  0.0253
_diffrn_reflns_av_unetI/netI     0.0195
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -7
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       -9
_diffrn_reflns_number            17594
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.500
_diffrn_reflns_theta_max         28.281
_diffrn_reflns_theta_min         2.399
_exptl_absorpt_coefficient_mu    0.076
_exptl_absorpt_correction_T_max  0.8621
_exptl_absorpt_correction_T_min  0.8088
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'Bruker SADABS'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.198
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    not_measured
_exptl_crystal_description       prism
_exptl_crystal_F_000             600
_exptl_crystal_size_max          0.284
_exptl_crystal_size_mid          0.265
_exptl_crystal_size_min          0.152
_refine_diff_density_max         0.400
_refine_diff_density_min         -0.180
_refine_diff_density_rms         0.039
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     285
_refine_ls_number_reflns         3575
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.040
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_gt           0.0390
_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^)+(0.0569P)^2^+0.4141P] 
 where P=(Fo^2^+2Fc^2^)/3 
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1012
_refine_ls_wR_factor_ref         0.1064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3045
_reflns_number_total             3575
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ol502205m_si_004.cif
_cod_data_source_block           cdv24
_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               1517389
_shelx_estimated_absorpt_t_min   0.979
_shelx_estimated_absorpt_t_max   0.989
_shelxl_version_number           2012-9
_shelx_res_checksum              31140
_shelx_hkl_checksum              21355